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  • 1995-1999  (1,712)
  • 1955-1959
  • 1820-1829
  • 1995  (1,712)
  • 1824
  • Analytical Chemistry and Spectroscopy  (1,554)
  • crystal structure  (158)
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  • 1995-1999  (1,712)
  • 1955-1959
  • 1820-1829
Year
Keywords
  • 1
    Electronic Resource
    Electronic Resource
    α-Iminohydroxylamine-α-aminonitrone tautomerism: a 1∶1 mixture of two tautomeric forms in crystals of N-(4,5-dihydro-1H-imidazol-2-yl)-N-phenyl-hydroxylamine (1995)
    Springer
    Journal of chemical crystallography 25 (1995), S. 813-821 
    Details
    ISSN: 1572-8854
    Keywords: Tautomerism ; hydrogen bonding ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract Crystals consisting of two distinct chemical entities, tautomers of each other, in exact 1∶1 ratio, have been obtained and their structure determined by X-ray analysis. The crystals of C9H11N3·C9H11N3 are monoclinic,P21/c,a=15.674(3),b=17.085(3),c=13.758(3)Å, β=90.78(2)°,Z=8. There are two hydroxylamine and two aminonitrone molecules in the asymmetric unit. Hydrogen bonds connect those molecules into chiral layers. Layers of opposite chirality alternate andthe crystal is centrosymmetric as a whole. Within those layers chains of tautomers joined by very strong O−H... O and strong N−H... N bonds can be recognized. Proton transfer along those chains with simultaneous rearrangement of π-bonds within the molecules would result in interconversion of tautomers and would affect chirality of the layer.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01671076
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  • 2
    Electronic Resource
    Electronic Resource
    Dialkylimidazolium-sodium chloroaluminate ternary salt system: phase diagram and crystal structure (1995)
    Springer
    Journal of chemical crystallography 25 (1995), S. 57-62 
    Details
    ISSN: 1572-8854
    Keywords: phase diagram ; buffered chloroaluminate ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract The phase diagram of the buffered neutral aluminum chloride + 1-ethyl-3-methyl-1H-imidazolium chloride + sodium chloride (AlCl3-EMIC-NaCl) ternary melt system can be represented by a binary phase diagram composed of (EMI)AlCl4 and NaAlCl4. In the binary phase diagram, the salts are liquid at, or near, room temperature for a wide range of compositions. At the 1∶1 composition, the congruently melting compound (EMI)(Na)(AlCl4)2 with m.p.=36.7°C is formed. Crystals of this mixed organic-inorganic salt were grown for single crystal x-ray diffraction analysis. The compound crystalizes in the space group $$P\bar 1$$ with lattice parametersa=10.321(1) Å,b=10.895(3) Å,c=9.284(4) Å, α=98.31(2)°, β=100.83(4)°, γ=101.95(3)°. Data collected at −120°C gave final residuals ofR=0.037 andR w=0.045 using 2713 observed reflections. The packing diagram reveals Na+ ion zig-zag chains running along thea-axis with each Na+ surrounded by four AlCl 4 − units, reminiscent of NaAlCl4. The AlCl 4 − ions form a distorted square planar coordination sphere around Na+ at an average Na−Al distance of 3.76(4) Å. Using a sodium ionic radius of 1.16 Å, a new AlCl 4 − ionic radius of 2.60 Å is calculated. This radius is 0.21 Å shorter than the reported thermodynamic radius.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01667037
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  • 3
    Electronic Resource
    Electronic Resource
    Antifungal copyrine alkaloids: crystal structure of 3-methylsampangine (1995)
    Springer
    Journal of chemical crystallography 25 (1995), S. 223-226 
    Details
    ISSN: 1572-8854
    Keywords: Antifungal alkaloids ; 3-methylsampangine ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract 3-Methylsampangine, C16H10N2O, crystallizes in the monoclinic space group P21/c witha=7.260(3),b=10.697(5),c=15.342(6) Å, and β=102.69(4). All nonhydrogen atoms of this potent antifungal agent are planar to within 0.082 Å. The title compound exhibits potentin vitro antifungal activity againstC. neoformans, C. albicans andA. fumigatus.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01665173
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  • 4
    Electronic Resource
    Electronic Resource
    Crystal structure of decacalcium tetrapotassium hexakis (pyrophosphate) nonahydrate (1995)
    Springer
    Journal of chemical crystallography 25 (1995), S. 219-222 
    Details
    ISSN: 1572-8854
    Keywords: Calcium phosphate ; calcium pyrophosphate ; calcium potassium pyrophosphate ; crystal structure ; layer-type structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract The crystal structure of Ca10K4(P2O7)6·9H2O has been determined by single crystal X-ray diffraction. Crystals are hexagonal, space group P63cm witha=11.761(1),c=9.770(1) Å, andZ=1. The structure was refined toR=0.028 andR w=0.037 for 468 reflections withI≥3σ(I). The structure consists of a compact assembly of Ca and P2O7 ions arranged in layers perpendicular to thec-axis in a hexagonal array with relatively large open channels along thec-axis. The K ions and the water molecules are located in these open channels and are disordered.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01665172
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  • 5
    Electronic Resource
    Electronic Resource
    Unusual occurrence of photooxidation of a cage diol (1995)
    Springer
    Journal of chemical crystallography 25 (1995), S. 295-298 
    Details
    ISSN: 1572-8854
    Keywords: Cage-diol ; crystal structure ; photooxidation
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract An unusual photooxidation was noted upon photolytic cage closure of a substituted tricyclo[6.2.1.02.7]undecane-exo, exo-diol. The resultant compound, which may be regarded as a mono-reduced pentacyclo[5.4.0.02,6.03,10.05,9]undecane-8,11-dione, was characterizedvia X-ray crystallography. This species could be reduced to the tricyclo[6.2.1.02,7]undecane-endo, exo-diol under conditions previously shown to be inert for the parent dione.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01796053
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  • 6
    Electronic Resource
    Electronic Resource
    Crystal and molecular structure of 6,7-benzo-3,4 (1,4-dimethoxy-2,3-naphtho)-1,5-dioxosuberane (1995)
    Springer
    Journal of chemical crystallography 25 (1995), S. 379-382 
    Details
    ISSN: 1572-8854
    Keywords: Benzonaphthodioxosuberane ; crystal structure ; radermachol
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract The crystal and molecular structure of the title compound (2) C21H16O4 has been determined by an X-ray analysis, by direct methods from diffractometer data and refined by full-matrix least squares. The compound (2) crystallizes in the space group P21/a, with cell parameters:a=36.432(5),b=5.512(3),c=8.269(5) Å, β=108.0(3)°,z=4,D c =1.397 g/cm−3,R=7.8 for 1136 observed reflections. The conformation of the tetracyclic ring system shows a folding of two planar parts of the carbon skeleton about an axis passing thorough C8 and C16 of the seven membered ring C.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01665273
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  • 7
    Electronic Resource
    Electronic Resource
    Synthesis and structural characterization of [Au2Pd14(μ3-CO)7(μ2-CO)2(PMe3)11](PF6)2—An icosahedrally-based high nuclearity mixed metal cluster (1995)
    Springer
    Journal of cluster science 6 (1995), S. 71-91 
    Details
    ISSN: 1572-8862
    Keywords: Palladium ; gold ; cluster ; phosphine ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Physics
    Notes: Abstract [Au2Pd14(μ3-CO)7(μ2-CO)2(PMe3)11](PF6)2 has been synthesized from [Pd8(CO)8(PMe3)7] and AuCl(PCy3) in the presence of TIPF6. It has been characterised on the basis of mass spectrometry, infrared and NMR spectroscopy, and a single crystal X-ray diffraction study. The structure is based on a palladium-centered Au2Pd11 icosahedron which shares an edge with a Pd5 trigonal bipyramid.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01175837
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  • 8
    Electronic Resource
    Electronic Resource
    The synthesis and reactivity of the heptanuclear dianion [Os7(CO)20]2− including the synthesis and structural characterizations of the compounds [Os7(CO)20(AuPEt)3 2] and [Os8(CO)20(η6-C6H6] (1995)
    Springer
    Journal of cluster science 6 (1995), S. 163-173 
    Details
    ISSN: 1572-8862
    Keywords: Cluster carbonyl ; osmium ; gold ; arene ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Physics
    Notes: Abstract Reduction of the heptaosmium cluster [Os7(CO)21] With [Et4N][NH4) gives the cluster dianion [Os7(CO)20]2−,1, in high yield. The reaction of the dianion with [AuPR 3Cl] (R=Et or Ph) in the presence of TlPF6 forms [Os7((CO)20(AuPR 3)2] [R=Et (2a);R = Ph(2b)] in 80% yield, while the corresponding reaction with (Os(C6H6)(CH3CN)3]2+ gives [Os8(CO)20 (η 6-C6H6)] (3) in reasonable yield (ca. 30%). The dianion,1, and the clusters2 and3 have been fully characterized by bout spectroscopic and crystallographic methods. The crystal structure of the [Ph4P]+ salt of1 shows that the metals in the anion adopt a capped octahedral geometry, with all twenty carbonyl ligands in terminal sites. The metal core geometry in2a is best described as a tricapped octahedron, and is based on the structure of the dianion1 with two adjacent octahedral faces capped by the Au atoms of the two AuPEt3 groups. In a similar fashion, the geometry of3 is related to that of1 with the addition of an Os(C6H6) unit capped to a triangular face, to give a bicapped octahedral framework.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01175843
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  • 9
    Electronic Resource
    Electronic Resource
    Synthesis and characterization of the undecaosmium carbido carbonyl cluster: Crystal and molecular structures of [N(PPh3)2][Os11C(CO)27(μ-Cl)] (1995)
    Springer
    Journal of cluster science 6 (1995), S. 343-346 
    Details
    ISSN: 1572-8862
    Keywords: Undecaosmium carbido cluster ; µ-bridged chlorol preparation ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Physics
    Notes: Abstract A chloro-derivative of undecaosmium carbido cluster [Os11C(CO)27(µ-Cl)]-1 anion has been prepared and fully characterized by spectroscopic and crystallographic methods. The structure1 is an important intermediate for the conversion of [Os11C(CO)27]2 2 dianion to [OS10C(CO)24]2-3 dianion.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01169700
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  • 10
    Electronic Resource
    Electronic Resource
    Synthesis, chemical, and electrochemical characterization of the [Ag13{μ3-Fe(CO)4}] n− (n = 3, 4, 5) cluster anions: X-Ray structural determination of [N(PPh3)2]3 [Ag12(μ12-Ag){μ3Fe(CO)4}8]1 (1995)
    Springer
    Journal of cluster science 6 (1995), S. 107-123 
    Details
    ISSN: 1572-8862
    Keywords: Silver ; iron ; carbonyl ; cluster ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Physics
    Notes: Abstract The oxidation of the [Fe(CO)4]2− dianion with Ag+ salts occurs through a particularinner-sphere mechanism, which involves an intermediate cascade of silver clusters stabilized by Fe(CO)4 ligands. The last detectable Ag-Fe cluster of the sequence is the [Ag13{μ-Fe(CO)4}8]3− trianion, which has been selectively obtained by using ca. 1.7 equivalents of Ag+ per mole of [Fe(CO)4]2−. The [Ag13{μ-Fe(CO)4}8]3−- trianion has been isolated in a crystalline state with several quaternary cations, and has been characterized by X-ray diffraction studies of its bis(triphenylphosphine)iminium salt. [N(PPh3)2]3 [Ag13{μ 3-Fe(CO)4}8]·2(CH3)2CO, monoclinic, space group P21 (No.4),a = 16.284(2) Å,b =18.767(5) Å,c = 25.905(4) Å,β = 90.46(1)°,V = 7916(3) Å3,Z = 2,R = 0.0324. The molecular structure of the anion consists of a centered cuboctahedron of silver atoms with the triangular faces capped by Fe(CO)4 units. Chemical reduction of ( Ag13{μ 3-Fe(CO)4}8]3− affords the corresponding [Ag13{μ 3-Fe(CO)4)8]4−, which in turn gives [Ag13{μ 3-Fe(CO)4)8]5− and [Ag6{μ 3-Fe(CO)4}4]– upon further reduction. Electrochemical investigations confirm the reversibility of the [Ag13{μ 3-Fe(CO)4}8]3−/4− redox change. Furthermore, in spite of some electrode poisoning effects, evidence of the existence of the [Ag13{μ 3-Fe(CO)4}8]5− pentaanion was obtained. The yet structurally uncharacterized [Ag6{μ 3-Fe(CO)4)4]2− dianion is quantitatively obtained by reaction of [Fe(CO)4]2− with ca. 1.5 equivalents of Ag+ or by addition of one equivalent of Ag+ to solutions of the [Ag5{Fe(CO)4}4]3− trianion. All attempts to isolate its quaternary salts as crystalline materials failed owing to formation of amorphous insoluble precipitates. The above series ofμ 3-Fe(CO)4 octa-capped cuboctahedral Ag13 clusters can be envisioned as the Ag+ . Ag and Ag− cryptates of the [Ag12{μ}3-Fe(CO)4}8]4− cryptand. respectively.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01175839
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  • 11
    Electronic Resource
    Electronic Resource
    The synthesis and structural characterization of Os3(CO)8[Si(OMe)3][μ-PMe2(C6H4](μ-H)2: An unusual unsaturated triosmium cluster complex (1995)
    Springer
    Journal of cluster science 6 (1995), S. 437-447 
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    ISSN: 1572-8862
    Keywords: Osmium ; unsaturated cluster ; ortho-metallation ; siloxyl ligand ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Physics
    Notes: Abstract The reaction of Os3(CO)10(NCMe)[Si(OMe)3](μ-H),1, with PMe2Ph yielded the new complex Os3(CO)10(PMe2Ph)[Si(OMe)3](μ-H),2 by substitution of the MeCn ligand with the phosphine ligand. When heated to 125°C compound2 was decarbonylated and transformed into the new unsaturated cluster complex Os3(CO)8[μ-PMe2(C6H4)][Si(OMe)3](μ-H)2,3 in 54% yield. Compound3 was characterized by a single crystal X-ray diffraction analysis, osmium bonds. The phenyl ring of the phosphine ligand has undergoneortho-metallation by a neighboring metal atom. A terminally coordinated Si(OMe)3 ligand is coordinated to the third osmium atom. The cluster is unsaturated by the amount of 2 electrons, and there is an open coordination site on the siloxyl substituted osmium atom that is partially filled by a weak interaction with one of the π-bonds of theortho-metalled phenyl ring. Complex3 reacts with CO at 1 atm to reform compound2 in 85% yield in 5 h at 40°C. Crystal Data: for3: space group = P21/n,a = 9.911(2) Å,b = 18.451(6) Å,c = 14.872(2) Å,β = 95.64(2)°,Z = 4, 1994 reflections,R = 0.028.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01165472
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  • 12
    Electronic Resource
    Electronic Resource
    Doubly-bridged binuclear complexes of oxomolybdenum(V) and oxotungsten(V) containing sexadentate ligands (1995)
    Springer
    Journal of cluster science 6 (1995), S. 549-566 
    Details
    ISSN: 1572-8862
    Keywords: Molybdenum ; tungsten ; di-μ-oxo bridge ; sexadentate ligands ; asymmetric distortion ; stereoselectivity ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Physics
    Notes: Abstract Binuclear oxomolybdenum(V) and oxotungsten(V) complexes of the type, [M 2(O)2(μ-X)(μ-X 1)]”, where M=Mo, W;X.X 1=O, S; L=edta, pdta (n=2-), tpen, tppn (n=2+) (edta4– =ethylenediaminetetraacetate(4–), pdta=R- orR,S-propylenediaminetetraacetate(4–), tpen=N,N,N 1,N1-tetrakis(2-pyridyhnethyl)-ethylenediamine, and tppn=R- orR,S-N,N,N 1,N1-tetrakis(2-pyridylmethyl)-propylenediami ne) are reviewed with respect to their preparation, structure, spectroscopic properties, reactivities, and in particular asymmetric distortion around the bicyclo [4.1.1 ] type core and stereoselectivity related to this distortion,
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01165773
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  • 13
    Electronic Resource
    Electronic Resource
    Comparison of the crystal structure and molecular models of N,N-diisobutyl-2-(octylphenylphosphinyl)acetamide (CMPO) (1995)
    Springer
    Journal of chemical crystallography 25 (1995), S. 43-49 
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    ISSN: 1572-8854
    Keywords: Molecular mechanics ; molecular dynamics ; MNDO ; CMPO ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract The crystal structure of N,N-diisobutyl-2-(octylphenylphosphinyl)acetamide, or CMPO was recently determined. The compound crystallizes in the space group P21/c witha=13.446(6),b=22.280(7),c=17.217(7) Å, β=92.07(4)°, andD calc=1.05 g/cm3 forZ=8 @20°C). Molecular mechanics, molecular dynamics, and MNDO calculations were also performed on CMPO utilizing the SYBYL1 suite of programs. The results from these calculations are compared to the crystal structure and to similar calculations performed on CMPO using ALCHEMY2,3. In general, the results from the calculations agree fairly well with the parameters from the crystal structure.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01666193
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  • 14
    Electronic Resource
    Electronic Resource
    Mercury(II) complex with terpyridine: structure of the 2∶1 solvate of [Hg(terpy)2](CF3SO3)2 with acetone (1995)
    Springer
    Journal of chemical crystallography 25 (1995), S. 453-458 
    Details
    ISSN: 1572-8854
    Keywords: Mercury(II) terpyridine complex ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract [Hg(terpy)2](CF3SO3)2·0.5(CH3)2CO crystallizes in the triclinic $$P\bar 1$$ space group witha=14.631(6),b=15.258(4),c=18.785(7) Å, α=69.66(2), β=70.72(1), γ=88.55(1)°. The crystal structure consists of two independent [Hg(terpy)2]2+ cations, four trifluoromethanesulfonate anions and an acetone molecule in the asymmetric unit. Each mercury atom is coordinated by two tridentate terpyridine ligands forming an irregular six-coordination polyhedron. The Hg−N bond lengths range from 2.27(2) to 2.53(2) Å.
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    URL: http://dx.doi.org/10.1007/BF01665700
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  • 15
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    Electronic Resource
    Crystal structures of twoN-substituted 2-thioxo-1,3-dithiole-4-carboxamides (1995)
    Springer
    Journal of chemical crystallography 25 (1995), S. 463-467 
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    ISSN: 1572-8854
    Keywords: 1,3-dithiole-4-carboxamides ; resonance effect ; short intramolecular S...O contact ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract The two closely related compoundsN,N-dimethyl 5-(methylthio)-2-thioxo-1,3-dithiole-4-carboxamide1 andN-(p-methoxy-phenyl)-N-methyl 5-(methylthio)-2-thioxo-1,3-dithiole-4-carboxamide2 have been characterized by X-ray crystal structure determination. Crystal data for1: triclinic, $$P\bar 1$$ ,a=6.767(1),b=12.594(2),c=6.648(1) Å, α=101.38(1), β=93.37(2), γ=79.62(1)°,V=546.2 Å3,Z=2. Crystal data for2: monoclinic, Cc,a=19.836(4),b=6.057(1),c=15.860(3) Å, β=127.61(3)°,V=1509.5Å3,Z=4. The molecular structures of1 and2 show remarkable differences concerning the conformational behavior. These differences are related to the nature of the substituents at the nitrogen atom. The presence of an aromatic system in2 leads to an almost planar arrangement of the α-oxoketene dithioacetal moiety. This effect is accompanied by a short intramolecular S...O contact of 2.648(2) Å. In the absence of an aromatic system, as is the case for compound1, neither a resonance effect along the α-oxoketene dithioacetal fragment nor a short S...O distance is observed.
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    URL: http://dx.doi.org/10.1007/BF01665702
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  • 16
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    Electronic Resource
    The crystal structure of a heterobimetallic crown ether complex: [Na(dibenzo-18-crown-6)][FeCl4] (1995)
    Springer
    Journal of chemical crystallography 25 (1995), S. 579-582 
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    ISSN: 1572-8854
    Keywords: Dibenzo-18-crown-6 ; hetero bimetallic ; crown ether ; crystal structure ; ferric chloride
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract Slow evaporation of a solution of ferric chloride and dibenzo-18-crown-6 in 3∶1 CH3CN∶CH3OH produced single crystals of the title complex. This heterobimetallic crown ether complex, [Na(dibenzo-18-crown-6)][FeCl4], crystallizes in the monoclinic space group P2t/n with cell parameters (at 22°C)a=14.608(6),b=10.466(9),c=17.276(9)Å, β=91.47(6)°, andD calc=1.46 g cm−3 for Z=4. The structure consists of discrete ions with the shortest Na ... Cl distance a lengthy contact of 3.56(1)Å. The average Na...O separation is 2.69(3)Å. The [FeCl4]− anion exhibits a distorted tetrahedral geometry with an average Fe−Cl bond length of 2.16(2)Å.
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    URL: http://dx.doi.org/10.1007/BF01667027
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  • 17
    Electronic Resource
    Electronic Resource
    Nucleophilic additions of primary and secondary amines to pentacyclo[5.4.0.02,6.03,10.05,9]undecane-8,11-dione (1995)
    Springer
    Journal of chemical crystallography 25 (1995), S. 633-640 
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    ISSN: 1572-8854
    Keywords: Amines ; crystal structure ; pentacycloundecane-8,11-dione
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract The crystal structures of three compounds formedvia nucleophilic attack of a heterocyclic secondary amine on PCU-8,11-dione, with the concomitant intramolecular attack of one keto oxygen on the carbon of the other ketone, are presented. In all three compounds, the bridging oxygen contains substantial p-character, and the bonds to the “attacking” nitrogen are significantly shorter than would be expected.
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    URL: http://dx.doi.org/10.1007/BF01665969
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  • 18
    Electronic Resource
    Electronic Resource
    X-ray structure of sesterterpene, 16β-acetoxy-24-methyl-12,24-dioxoscalaran-25-al (1995)
    Springer
    Journal of chemical crystallography 25 (1995), S. 765-768 
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    ISSN: 1572-8854
    Keywords: Sesterterpene ; scalaran ; crystal structure ; marine compound
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract The molecular geometry of a tetracyclic sesterterpene has been determined by X-ray diffraction. The conformation of the aldehyde group as observed in the crystal structure supports the rationalization for the absence of aldehyde proton coupling in the nmr spectra of the compound. Crystal data: C28H42O5, M.W.=458.6; orthorhombic, P212121;a=10.797(2),b=29.270(9),c=8.033(1)Å,V=2538.7Å3,Dx=1.199 g cm−3;R=0.045 for 2287 observed reflections.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01670333
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  • 19
    Electronic Resource
    Electronic Resource
    Synthesis of a chiral calixarene: 5,11,17,23-tetra (tert-butyl)-25,27-bis[((+)-camphor-10-sulfonyl)-oxy]-calix[4]arene-26,28-diol: crystal and molecular structure of its (1∶2) complex with toluene (1995)
    Springer
    Journal of chemical crystallography 25 (1995), S. 401-406 
    Details
    ISSN: 1572-8854
    Keywords: Calixarene ; complex ; crystal structure ; chirality
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract The title compound was obtained by treatment ofp-tert-butylcalix[4]arene with (+) camphorsulfonyl chloride in triethylamine and toluene. A (1∶2) complex with toluene has been found. Its structure has been determined by X-ray crystallography. Crystals are triclinic with space group P1,a=16.426(3),b=18.553(3),c=13.661(2) Å, α=94.78(2), β=110.76(2), γ=72.83(2)°,V=3720(2) Å3,d c =1.127 g/cm3 Z=2. Refinement based on 10495 observed reflections led to a finalR value of 0.100. The two independent molecules of calixarene in the asymmetric unit are in the cone conformation and the calixarene cavities are empty. The guest molecule occupies the interhost space. The norborane skelton of (+) camphorsulfonyl group is the same as ones found in literature. Only van der Waals interactions exist between the host and the guest molecules.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01665277
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  • 20
    Electronic Resource
    Electronic Resource
    Synthesis and structure of a seven electron triangular cluster complex [Mo3S4Cl3(dppe)2(PEt3] (1995)
    Springer
    Journal of cluster science 6 (1995), S. 523-532 
    Details
    ISSN: 1572-8862
    Keywords: Molybdenum ; reduction ; seven-electron triangular cluster ; bridging sulfide ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Physics
    Notes: Abstract The triangular six-electron cluster complex [Mo3S4Cl4(PEt3) x (thf)5] produced by the excision reaction of Mo3S7Cl4 with triethypholsphine is reduced by magnesium at − 20°C. Subsequent addition of dppe (=1,2-his(diphenylphosphino)ethane) to the reduced species affords a seven-electron triangular cluster complex [Mo3S4Cl3(dppe)2(PEt3)]. The complex crystallizes in the space groupCm witha=17.170(6),b-19.878(6),c = 13.289(5)β = 121.73(2)°,V = 3858(2) A3, andZ = 2. The structure shows an almost equilateral triangle of three molybdenum atoms capped by a Sulfur atom and bridged by three sulfur atoms. The Mo Mo distances, ranging from 2.804(1) to 2.809(1) A are elongated ca. 0.04 A as compared with lose of a six-electron cluster complex with drape ligands. Two molybdenum atoms have a chlorine and a dppe ligands, and the other molybdenum atom bas a chlorine and a triethylphosphine ligands. The UV-Vis spectrum has a characteristic broad hand centered at 1410 n m, which is not observed for six-electron clusters. The ESR spectrum indicates the presence of an unpaired electron consistent with the formulation of the compound as a seven-electron cluster.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01165771
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  • 21
    Electronic Resource
    Electronic Resource
    Linear and Nonlinear Optical Properties Of Racemic (±)2-(α-Methylbenzylamino)-5-Nitropyridine Single Crystals (1995)
    Springer
    Optical review 2 (1995), S. 128-131 
    Details
    ISSN: 1349-9432
    Keywords: organic crystal ; racemic form ; second-harmonic generation ; refractive index ; nonlinear optical coefficient ; crystal structure ; oriented-gas model
    Source: Springer Online Journal Archives 1860-2000
    Topics: Physics
    Notes: Abstract Linear and nonlinear optical properties of racemic (±)2-(α-methylbenzylamino)-5-nitropyridine ((±)MBANP) single crystals have been comprehensively investigated and compared with those of the enantiomorph (–)2-(α-methylbenzylamino)-5-nitropyridine ((–)MBANP) crystals. (±)MBANP crystal exhibits very high chemical and physical stability, but relatively small nonlinear optical coefficients (d31 = 6.8 pm/V, d32 = 4.7 pm/V, d33 = 0.84 pm/V). A comparison between the nonlinear optical coefficients of (±)MBANP and (–)MBANP demonstrates the validity of the oriented-gas model in molecular crystals that neglects all the contributions from intermolecular interaction.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/s10043-995-0128-5
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  • 22
    Electronic Resource
    Electronic Resource
    The synthesis and X-Ray crystallographic analysis of a stable norbornadienone: 17-Oxo-7,16-methano-7,16-diphenylcyclopenta[d,e]tribenzo[a,h,j]anthracene (1995)
    Springer
    Structural chemistry 6 (1995), S. 167-173 
    Details
    ISSN: 1572-9001
    Keywords: MM3 ; PM3 ; MMX ; crystal structure ; norbonadienone ; distorted compound
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The reaction of 4,5-didehydroacenaphthene with phencyclone yields the title compound, a stable dibenzo-fused norbornadienone (8). The X-ray structure of8 is presented and compared with the structure predicted from a MM3, PM3, and a MMX calculation. Thermal decomposition of 8 produces, 7,16-diphenylcyclopenta[d,e]tribenzo[a,h,j]anthracene (9), a hydrocarbon that is computed to have a significantly twisted polycyclic aromatic skeleton with 19 kcal/mole of strain energy.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF02286444
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  • 23
    Electronic Resource
    Electronic Resource
    Molecular Structure of 5-Methylchrysene-7,8-dihydro-7,8-trans-(e, e)-diol (1995)
    Springer
    Structural chemistry 6 (1995), S. 57-63 
    Details
    ISSN: 1572-9001
    Keywords: Hydrogen bonding ; carcinogen ; polycyclic aromatic hydrocarbon derivative ; dihydrodiol ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The crystal structure of the weak carcinogen 5-methylchrysene-7,8-dihydro-7,8-trans-(e,e)-diol is reported. This molecule contains a distorted bay region as a result of the presence of the 5-methyl group as found in 5-methylchrysene and 5,6- and 5, 12-dimethylchrysene. One torsion angle in this bay region is 20
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF02263528
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  • 24
    Electronic Resource
    Electronic Resource
    Synthesis and structure of 13- and 26-membered crown ethers, derivatives of resorcinol (1995)
    Springer
    Russian chemical bulletin 44 (1995), S. 2353-2360 
    Details
    ISSN: 1573-9171
    Keywords: resorcinol-based crown ethers ; crystal structure ; intramolecular nonbonded C-H...O contacts
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract 13- and 26-Membered crown ethers have been synthesized based on resorcinol and 1,8-dichloro-3,6-dioxaoctane. The products with substituents in the benzene ring have been prepared by alkylation of 13-membered crown ether. Complexing properties of the macrocycles have been studied with the use of ion-selective membrane electrodes. The structures of 13- and 26-membered crown ethers have been established by X-ray structural analysis.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00713607
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  • 25
    Electronic Resource
    Electronic Resource
    Oxidation of 1-hydrazino-3,3-dimethyl-3,4-dihydroisoquinoline. X-ray, spectroscopic, and quantum-chemical study of the structure of 3,3-dimethyl-3,4-dihydroisocarbostyryl azine (1995)
    Springer
    Russian chemical bulletin 44 (1995), S. 2364-2370 
    Details
    ISSN: 1573-9171
    Keywords: dihydroisoquinoline derivatives ; crystal structure ; electronic, IR, and1H NMR spectra ; quantum-chemical calculation
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract 3,3-Dimethyl-3,4-dihydroisocarbostyryl azine (2) has been synthesized by oxidation of l-hydrazino-3,3-dimethyl-3,4-dihydroisoquinoline (1). The crystal and molecular structures of compound 2 were determined. It has been established that in the solid state, compound2 exists as an azine tautomer. The IR, electronic, and NMR spectral data indicate that in solution the tautomeric form of2 does not change. A possible mechanism of the oxidation of1 to2 is suggested.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00713609
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  • 26
    Electronic Resource
    Electronic Resource
    Crystal Structure of 2-Debenzoyl, 2-Acetoxy Paclitaxel (Taxol®): Conformation of the Paclitaxel Side-Chain (1995)
    Springer
    Pharmaceutical research 12 (1995), S. 337-341 
    Details
    ISSN: 1573-904X
    Keywords: 2-debenzoyl, 2-acetoxy paclitaxel ; docetaxel ; paclitaxel side-chain ; crystal structure ; solid state conformation ; intramolecular hydrogen bonding ; intermolecular hydrogen bonding
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Crystals of the C2-acetate analog of paclitaxel, grown from a mixture of isopropyl alcohol and methanol, belong to the space group P2l with a = 9.058(3), b = 18.306(5), c = 15.043(1) Å, β = 97.09(1)°, Z = 2, V = 2475.1(9)Å3, D calc = 1.269 gcm−3 and µ = 0.75 cm−1. The structure was determined by direct methods and refined to R(F) = 0.054 and wR(F) = 0.057 for 605 variables and 3496 observed reflections. The paclitaxel side chain possesses a conformation similar to that observed in the crystal structure of docetaxel (Taxotere®). A three dimensional network of hydrogen bonds is formed through solvent molecules and stabilizes the crystal lattice.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1023/A:1016236014766
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  • 27
    Electronic Resource
    Electronic Resource
    Structure ofp-tetrakis-(4-nitrophenylazo)calix[4]-arene-4-picoline (1∶4) complex (1995)
    Springer
    Journal of inclusion phenomena and macrocyclic chemistry 22 (1995), S. 33-40 
    Details
    ISSN: 1573-1111
    Keywords: Calixarene-dye ; crystal structure ; inclusion compound
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The structure of thep-tetrakis-(4-nitrophenylazo)calix[4]arene-4-picoline (1∶4) complex has been determined by X-ray crystallography. Crystals are monoclinic, space groupC2/c,a=24.9097) Å,b=8.425(6) Å,c=33.81(1) Å, β=101.13(2)°,D c =1.330 g/cm3,Z=4, finalR value =0.067. The cone conformation adopted by this azocalixarene is disturbed by the positions of the picoline molecules. Two of them are inside the macorocycle cavity and the two others are outside.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00706496
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  • 28
    Electronic Resource
    Electronic Resource
    New synthesis and complexing properties ofp-tert-butyldihomooxacalix[4]arene. Structure of its 1∶2 complex with tetrahydrofuran (1995)
    Springer
    Journal of inclusion phenomena and macrocyclic chemistry 22 (1995), S. 119-130 
    Details
    ISSN: 1573-1111
    Keywords: Calixarene ; complexation ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract A new method is described for the synthesis of isolatedp-tert-butyldihomooxacalix[4]arene (CALO) with a 24% yield. The ability of CALO to form complexes in the solid state with small neutral molecules has been studied; the potential guests were common solvents bearing various chemical functions. The powder obtained after evaporation of the solvent has been characterized by the X-ray powder diffraction technique. Analysis of the patterns shows the non-complexation of linear alkanes and alcohols, but formation of complexes when the guest is cyclic or when it bears an amine or a ketone function. As illustration of the possible arrangement of molecules in complexes, the structure of the 1:2 complex with tetrahydrofuran (THF) is presented: the crystals are monoclinic, space groupP21/c,a=9.459(2) Å,b=17.286(2) Å,c=30.469(6) Å, β=92.52(2)o,V=4977(2) Å3,Z=4,D c=1.099 Mg m−3, λ=1.54178 Å, μ=5.6 cm−1,R=0.086 for 3590 reflections withF〉4σ (F); one of the THF molecules is inside the cavity of the macrocycle, while the other, in the interhost space, exhibits disorder. In the CALO molecule, three out of the fourtert-butyl groups are disordered which may induce the disorder of the THF molecule.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00707687
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  • 29
    Electronic Resource
    Electronic Resource
    Inclusion compounds of (±) gossypol. Structure of the gossypol-n-valeric acid (1/2) coordinato-clathrate (1995)
    Springer
    Journal of inclusion phenomena and macrocyclic chemistry 22 (1995), S. 187-201 
    Details
    ISSN: 1573-1111
    Keywords: Inclusion compounds ; gossypol ; crystal structure ; hydrogen bonds
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The crystal structure of the inclusion compound of gossypol withn-valeric acid as a guest molecule has been determined by X-ray structure analysis. The crystals of C30H30O8·(C5H10O2)2, are triclinic, space group $$P\bar 1$$ ,a=6.912(2),b=14.506(3),c=19.387(4) Å, α=78.85(2)°, β=83.92(3)°, γ=86.78(3)°V=1895(1) Å3,Z=2,D x=1.267 g cm−3, μ (CuK α)=0.768 mm−1,T=292 K. The structure has been solved by direct methods on intensity data collected for a twinned crystal and refined to the finalR value of 0.062 for 1606 observed reflections and 470 refined parameters. Gossypol-n-valeric acid (1/2) coordinato-clathrate is not isostructural with any of the previously investigated gossypol inclusion compounds but shows some structural similarities to gossypol-acetic acid (1/1). The host and one of the carboxylic acid molecules are connected via hydrogen bonds into molecular assemblies of a column type which are further bonded to centrosymmetric dimers of the secondn-valeric acid molecule. In effect, host and guest molecules are assembled into layer-type H-bonded aggregates. Structural features common to gossypol-n-valeric acid (1/2) and other earlier reported gossypol inclusion compounds are discussed.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00707082
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  • 30
    Electronic Resource
    Electronic Resource
    Lattice dynamics of (Ba/K)BiO3 (1995)
    Springer
    Journal of superconductivity 8 (1995), S. 595-598 
    Details
    ISSN: 1572-9605
    Keywords: (Ba/K)BiO3 ; lattice dynamics ; electron phonon coupling ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Electrical Engineering, Measurement and Control Technology , Physics
    Notes: Abstract The Lattice dynamics of Ba.6K.4BiO3 was investigated by inelastic neutron scattering on a superconducting single crystal (T c =26 K (midpoint)). At low frequencies the dispersion curves are very similar to those observed in BaPb.75Bi.25O3. Differences were found in the bond bending vibrations of the BiO6 octahedra which indicate that the binding in the K-doped compound is more ionic. Rather anomalous features were observed in the high frequency Bi-O bond stretching vibrations which resemble those observed in the high T c cuprates La1.85Sr.15CuO4 and YBa2Cu3O7. The observed frequency shifts are interpreted as the consequence from a strong electron phonon coupling. The data are compared to the results obtained on non superconducting Ba.98K.02BiO3.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00727434
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  • 31
    Electronic Resource
    Electronic Resource
    Enantiomeric separation and sensitive determination of D, L-amino acids derivatized with fluorogenic benzofurazan reagents on pirkle type stationary phases (1995)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 9 (1995), S. 10-17 
    Details
    ISSN: 0269-3879
    Keywords: 4-fluoro-7-nitro-2,1,3-benzoxadiazole ; NBD-F ; 4-(N,N-dimethylaminosulphonyl)-7-fluoro-2,1,3-benzoxadiazole ; BDD-F ; enantimoeric separation ; D,L-amino acid ; biological sample ; Pirkle type stationary phase ; HPLC ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: The enantiomeric separations of D, L-amino acids derivatized with fluorogenic reagents, 4-fluoro-7-nitro-2,1,3-benzoxadiazole (NBD-F), 4-(N,N-dimethylaminosulphonyl)-7-fluro-2,1-3,-benzoxadiazole (DBD-F) and 4-aminosulphonbly-7-fluoro-2,1,3- benzoxadiazole (ABD-F) by high-performance liquid chromatography (HPLC) ON various Pirkle type chiral stationary phases (CSPs, Sumichiral OA series) with citric acid in methanol as a mobile phase were studied. Since the least retention and no separation was observed for the derivatives of racemic phenylalanine methyl-ester,-amide and a drug without an α-carboxyl group, the carboxylic acid group of the amino acid derivatives seemed to contribute to the enantioselective fixation of the derivatives through hydrogen bonding on the N-acyl-amino acid amide moiety of the CSP. The enantioselective retention of the derivatives was attained through the (S) or (R) configuration of valine, phenylglycine, naphthylglycine, naphthylethylamine or the tert-leucine moiety in the CSP. The 2, 1, 3-benzoxadazole (benzofurazan) moiety in the derivatives helps the effective fixation of the derivatives through a π-πinteraction with an aromatic moiety such as a 3, 5-dinitrophenyl group in the Pirkle type chiral stationary phases.D-Amino acids in biological samples were easily determined utilizing the present derivatization with NBD-F, enantiomeric separation and fluorometric detection (530 nm em/470nm ex) following deproteinization of biological samples (serum or brain homogenate) with methanol and centrifugation. The applications of the method were clearly demonstrated by the following results; D-Ala was detected in sera of healthy volunteers at a level of 0.48-3.10μM. D-Lys was found in the serum of a patient with myeloma and requiring renal dialysis, and D-Ser was found in rat and bovine cerebrum. Peak identification was performed by use of different types of stationary phases especially those bearing the opposite configuration to that of the chiral centre.
    Additional Material: 7 Ill.
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    URL: http://dx.doi.org/10.1002/bmc.1130090103
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  • 32
    Electronic Resource
    Electronic Resource
    Mannitol prevents methionine sulphoxidation mediated electrophoretic heterogeneity of apolipoprotein A-I (1995)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 9 (1995), S. 28-31 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: Hybrid isoelectic focusing of apolipoprotein A-I in polyacrylanide gels with immobilized pH-gradients under non-denaturing conditions resulted in the occurrence of additional bands which could prevent the specific and sensitive detection of genetic variants. Hybrid isoelectric focusing of tow chromatographically distinguishable apolipoprotien A-I isoforms that differ by sulphoxidaton of methionine residues, apo A-I(Met) and apo A-I(MetSO), revealed that the additional bands were caused by this post-translational modification. Several antioxidative additives and conditions were compared for their ability to prevent methionine sulphoxidation in apoliporotein A-I In the presence of 200 g/L mannitol in the gel, apolipoprotein A/I focused as a single band. Since methionine sulphoxidation in proteins is a general phenomenon either taking place in vivo or in vitro by isoelectric focusing, we conclude that isoelectric focusing in the presence of mannitol will improve the quality of resolution of many proteins in gels with immobilized pH-gradients.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bmc.1130090106
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  • 33
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    Electronic Resource
    A highly sensitive method to quantify triazolam and its metabolites with liquid chromatography - mass spectrometry (1995)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 9 (1995), S. 48-51 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: We established a highly sensitive method to determine triazolam and its major metabolites, α-hydroxytriazolam and 4-hydroxytriazolam, in human plasma and urine with a liquid chromatography-mass spectrometry system which incorporates an atmospheric chemical ionization interface. A plasma sample and a urine sample after solvent extraction were injected into an ODS column of reversed phase with a mobile phase in a linear solvent gradient of initially 50 mM ammonium acetate (pH 4.0) 50%: methanol 50% and 15 min later methanol 100%; quantification limits of as low as 20 pg/mL at an SNR of 3 were obtained for each compound. With diazepam as an internal standard, recovery yields of 84, 81, and 77% were obtained for triazolam, α-hydroxytriazolam and 4-hydroxytriazolam, respectively.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bmc.1130090110
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  • 34
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    Electronic Resource
    Sensitive determination of salmon calcitonin, by means of pre-column derivatization, HPLC and fluorometric determination (1995)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 9 (1995), S. 52-55 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A high sensitive analytical method for salmon calcitonin (sCT) was established by means of derivatization with a fluorescence labelling agent, DBD-F, followed by HPLC separation and fluorescence detection at 558 nm with excitation at 430 nm.Under optimized conditions (DBD-F, 0.1 M borate buffer (pH 8.5): acetonitrile (70:30, v/v)), three molecules of DBD-F reacted with one sCT molecule in the presence of 1 mM sodium dodecyl sulphate (SDS) at 50 oC for 3 h. The detection limit for the sCT derivative was 20 fmol. A linear relationship was obtained between the amount of sCT on column and the peak heights in the range of 35-8000 fmol.
    Additional Material: 7 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bmc.1130090111
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  • 35
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    Electronic Resource
    N-glycosylation site mapping of recombinant tissue plasminogen activator by micellar electrokinetic capillary chromatography (1995)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 9 (1995), S. 59-67 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: This report describes the N-glycosylation mapping of recombinant tissue plasminogen activator (rt-PA) using micellar electrokinetic capillary chromatography. The carbohydrate structures were tentatively assigned by comparison with the anion-exchange fractionated oligosaccharides and by a comparison with previously reported data. The separation was shown to rely mainly on the degree of sialylation of the oligosaccharides, allowing a quantitative determination of the proportion of neutral and mono- to tetrasialylated structures. Significant differences in the oligosaccharide distribution of the two variants of rt-PA, which differ by the presence (type I) or the absence (type II) of oligosaccharides at the Asn-184 site, were observed. The distribution of the oligosaccharides at each of the rt-PA glycosylation sites was then determined. Glycopeptides were prepared by tryptic digestion of rt-PA and isolated using two consecutive chromatographic procedures. The glycopeptides were finally treated with N-glycanase, and the resulting oligosaccharides were analysed by capillary electrophoresis. Oligosaccharide mapping revealed that the Asn-448 and Asn-184 sites carry the same population of complex-type oligosaccharides but that the relative amounts of each oligosaccharide vary markedly. High-pH anion-exchange chromatography performed on the desialylated oligosaccharides at each glycosylation site showed that the degree of microheterogeneity was related not only to the degree of sialylation but also to structural differences in the oligosaccharide sequences. From the results as a whole, we concluded that the Asn-448 site contains a greater proportion of heavily sialylated structures and has a higher degree of microheterogeneity. The Asn-117 site was demonstrated to contain a significant number of monosialylated structures (18.4%) in addition to the high-mannose-type oligosaccharides.
    Additional Material: 7 Ill.
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    URL: http://dx.doi.org/10.1002/bmc.1130090202
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  • 36
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    Electronic Resource
    Determination of glutathione and related aminothiols by gas chromatography with flame photometric detection (1995)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 9 (1995), S. 85-89 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A selective and sensitive method for the determination of glutathione (GSH) and related aminothiols such as cysteine (Cys), cysteinylglycine (CysGly) and γ-glutamylcysteine (γ-GluCys) by gas chromatography (GC) has been developed. GSH and related aminothiols were converted into their N, S-isopropoxycarbonyl methyl ester derivatives and measured by GC with flame photometric detection using a short capillary column (5 m × 0.53 mm i.d.) of cross-linked DB-1. The calibration curves were linear in the range 1-25 nmol for GSH and in the range 0.2-5 nmol for other aminothiols, and the detection limits of GSH, Cys, CysGly and γ-GluCys were approximately 5, 0.2, 0.3 and 0.5 pmol per injection respectively. This method was successfully applied to blood samples without prior clean-up, and GSH and related aminothiols in these samples could be analysed without any influence from coexisting substances. Overall recoveries of GSH and other aminothiols added to blood samples were 88-107%. The analytical results of free and total blood GSH and related aminothiols in normal subjects are presented.
    Additional Material: 2 Ill.
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    Masthead (1995)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 9 (1995) 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bmc.1130090301
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  • 38
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    Determination of guanase activity in normal and pathological sera by high-performance liquid chromatography (1995)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 9 (1995), S. 130-134 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A simple HPLC assay for serum guanase based on the direct determination of enzymatically formed xanthine was applied to normal and pathological sera. The procedure is sensitive, precise (CV below 5%) and suitable for routine purposes, and the method requires only 50 μL of sample. Using this method the reference range as determined from the sera of 40 healthy adult controls is 0-1.1 U/L. In patients with various liver diseases serum guanase activities were found to be increased 5- to 50-fold compared with the normal mean value.
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  • 39
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    Stereoselective analysis of nadolol in human plasma (1995)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 9 (1995), S. 226-228 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A steroeselective method, involving a single liquid-liquid extraction step, was developed and validated for the analysis of nadolol in human plasma. The assay involved extraction of nadolol and desmethyl-nadolol as internal standard (IS) from alkalinized plasma into dichloromethane. The organic solvent was separated and evaporated under nitrogen at 40°C. A chiral derivatization scheme with (R)-(-)-napthylethylisocyanate (50 μL of 0.1% solution in dichloromethane for 60 min) was employed to convert the enantiomers of nadolol into the corresponding diastereomeric derivatives. The residue was reconstitutd in the mobile phase and injected onto a C-18 column. The mobile phase was a mixture of methanol: tetrahdrofuran: water (52:7:41 by vol) containing about 0.001% v/v of both phosphoric acid and tetramethylethylenediamine. Fluorimetric detection was performed at excitation 230 and emission 330 nm. The assay was specific for the enantiomers of nadolol and the lower limit of quantitation was 2 ng/mL for of the enantiomers. Analysis of quality control samples resulted in precision estimates of 7% RSD for inter-assay and 10.1% RSD for intra-assay and the predicted concentrations deviated less than 9.4% of the nominal values for the four enantiomers. The extraction recoveries of the individual enantiomer was about 70%. Stability of nadolol enantiomers were established for four freeze/thaw cycle periods and in the autosampler at 5°C for at least 116 h.
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  • 40
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    Announcement (1995)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 9 (1995), S. i 
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    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bmc.1130090513
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  • 41
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    Evaluation of a narrow-bore HPLC column for trace level analysis of tetracyclines - a comparison with a conventional column (1995)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 9 (1995), S. 251-253 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/bmc.1130090603
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  • 42
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    Preliminary results on the LC-separation of non-steroidal anti-inflammatory agents in conventional and narrow-bore RP setups applying columns with different internal diameters (1995)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 9 (1995), S. 261-262 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Additional Material: 1 Ill.
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    URL: http://dx.doi.org/10.1002/bmc.1130090607
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  • 43
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    Improved protein separation using capillary electrophoresis and phytic acid (1995)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 9 (1995), S. 269-270 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bmc.1130090611
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  • 44
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    Potentiometric detection of carboxylic aliphatic acids in CZE using ion-selective liquid-membrane electrodes (1995)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 9 (1995), S. 257-258 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bmc.1130090605
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  • 45
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    Chromatographic investigation of the glycosylation pattern of alpha-1-acid glycoprotein secreted by the HEPG2 cell line; a putative model for inflammation? (1995)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 9 (1995), S. 199-204 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: In certain pathophysiological conditions, such as rheumatoid arthritis, there are alterations in the glycosylation pattern of the acute phase protein, alpha-1-acid glycoprotein (AGP). These changes are likely to be functionally significant, however, verification of the latter role requires a system which reflectsin vivo glycosylation changes in AGP and also produces sufficient quantities of the protein for further study. The human hepatoma cell line HepG2 is documented as displaying a shift in the glycosylation pattern of glycoproteins from normal state to acute phase after stimulation with inflammatory mediators. We have isolated AGP from the culture medium of HepG2 cells both before and after stimulation with a cytokine preparation and analysed the glycosylation pattern of each preparation, after enzymatic release, by high pH anion-exchange chromatography. Before stimulation, the glycosylated population was similar to a profile which was of AGP isolated from normal plasma; however, cytokine stimulation resulted in a shift to a profile which was consistent with that of AGP from a rheumatoid arthritis sufferer. Thus a HepG2 cell culture system is capable of being a crude model of the changes in glycosylation of acute phase proteins although it has a tendency to produce oligosaccharide chains which are not fully sialylated.
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    Comparative chromatographic study on the chiral separation of the 1-naphthylamine derivative of ketoprofen on cellulose-based columns of different sizes (1995)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 9 (1995), S. 289-290 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/bmc.1130090621
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  • 47
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    Capillary electrophoretic separation of some pharmaceutically important polypeptides (1995)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 9 (1995), S. 291-291 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Additional Material: 1 Tab.
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    URL: http://dx.doi.org/10.1002/bmc.1130090622
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  • 48
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    Rapid determination of O- and P-cresol isomers in urine from workers exposed to toluene by high-performance liquid chromatography using a graphitized carbon column (1995)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 9 (1995), S. 302-304 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A simple and rapid procedure is described that permits the simultaneous determination of o- and p- cresol in urine of workers or other individuals exposed to toluene. The urine samples are enzymatically hydrolysed and analysed by high-performance liquid-chromatography with a detetion limit of 0.2 mg/L, one fifth of the biological threshold limit value for o-cresol (1 mg/g ), a specific marker of toluene exposure. A graphitized carbon column Hybercarb-S, that exhibits an excellent selectivity for aromatic positional isomers, was used with 1% phosphoric acid-acetonitrile (70:30, v/v) as mobile phase and a detection wavelength of 271 nm. The overall accuracy for o-cresol determination was 4.5% at 5 mg/L and 8% at 0.5 mg/L. The cresol isomers were sufficiently resolved from endogenous materials to avoid the need for any extraction step, and the method appears suitable for monitoring workers accurately under the permissible level of exposure for occupational medicine purpose.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/bmc.1130090625
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  • 49
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    Improvement of achiral resolution in capillary zone electrophoresis by use of cyclodextrin additives (1995)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 9 (1995), S. 267-268 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bmc.1130090610
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  • 50
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    Suppression of chiral recognition of 3-hydroxy-1, 4-benzodiazepines during micellar electrokinetic capillary chromatography with bile saltsThe complete articles has been published in J. Chromatogr. A., 704, 238 (1995). (1995)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 9 (1995), S. 276-276 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bmc.1130090614
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  • 51
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    From dipeptides to oligopeptides: Analysis by capillary electrophoresis/electrospray mass spectrometry (1995)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 9 (1995), S. 283-284 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bmc.1130090618
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  • 52
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    Determination of unbound L-tryptophan in human plasma using high-performance liquid chromatography with fluorescence detection (1995)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 9 (1995), S. 305-308 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: An assay for the measurement of unbound L-tryptophan concentrations in plasma was developed using reverse-phase HPLC with fluorescence detection. Unbound L-tryptophan from plasma was obtained using the Amicon MPS-1 ultrafiltration device. L-tryptophan binding to the membrane in the ultrafiltration device was not significant. A linear relationship between the peak-area ratios (peak-area of L-tryptophan to internal standard) and concentrations of L-tryptophan was obtained in the range of 0.1 μg/mL to 2.5 μg/L. The intra-assay precision was less than 10% for each control (0.18 μg/mL, 0.75 μg/mL and 2.0 μg/mL). The inter-assay precision was less than 15% for each control; the accuracy for each control, expressed as percent difference from nominal (%DFN), was less than 12%. This method was used to determine unbound L-tryptophan concentrations in plasma from nine male subjects who participated in a clinical study.
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  • 53
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    Masthead (1995)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 9 (1995) 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bmc.1130090101
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  • 54
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    Determination of 5-hydroxytryptamine, 5-hydroxyindoleacetic acid and tryptophan in plasma and urine by HPLC with fluorimetric detection (1995)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 9 (1995), S. 23-27 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: Using native fluorescence detection, 5-hydroxytryptamine (5-HT), 5-hydroxyindoleacetic acid (5-HIAA) and tryptophan were resoved from themselves and other naturally occurring compounds using reversed-Phase HPLC within 5 min. Deproteinated platelet-poor plasma (ppp) and crude diluted urine were injected directly into the chromatograph. Careful selection of the HPLC column is important and various octadecyl silica (ODS) and base deactivated silic (BDS) columns were evaluated. Pre-treatment of an ODS column with tetrabutylammonium ions gave good selectivity. Between pH5 and 6 the compounds were well resolved from each other. The limit of quantitatiave detection of 5-HT and 5-HIAA was 3.5 nmol/L. The overal chromatogram obtained using native fluorescence is cleaner than that obtained with the more commonly employed electrochemical (EC) systems although the chromatography is effectively the same. For analysis of 5-HT in plasma, collection in EDTA was more efficient than lithium heparin. Plasma 5-HT in healthy volunteers was mean 61 (SD=±73) nmol/L, n=20; urine 5-HIAA gave mean 28.95 (SD=±0.98)μmol/L, (n=12). Whole blood 5-HT analysis is unreliable in comparison with platelet-poor plasma.
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    Measurement of clozapine and norclozapine in plasma/serum by high performance liquid chromatography with ultraviolet detection (1995)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 9 (1995), S. 36-41 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A simple method for the measurement of clozapine and its N-desmethyl metabolite in human pläsma or serum by high performance liquid chromatography is described. An internal standard (aqueous nortriptyline, 4 mg/L) (50 μL) and Tris buffer (2 mol/L, pH 10.6) (100 μL) are added to plasma/serum (200 μL) and the analytes and internal standard extracted into methyl tert-butyl ether (200 μL). The extracts are analysed on a 150 mm column containing Spherisorb S5SCX using methanol containing ammonium perchlorate (35 mmol/L, pH 6.7) as eluent at a flow rate of 1.5 mL/min. Detection is by ultraviolet absorption (215 nm). The limit of detection is better than 0.05 mg/L for both analytes and the intra-assay precision (CV) for clozapine and norclozapine was 5.3 and 7.3% at 0.5 mg/L and 2.6 and 2.8% at 1.5 mg/L, respectively. The method can be applied to the measurement of these compounds in plasma after acute overdosage, for the assessment of compliance in patients apparently refractory to therapy and to identify interactions between clozapine and other neuroleptic and antidepressant drugs which may effect toxicity.
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    URL: http://dx.doi.org/10.1002/bmc.1130090108
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  • 56
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    Potentials of chemiluminescence detection in flow injection analysis: Determination of penicillamine applying a quinine-Ce (IV) system (1995)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 9 (1995), S. 287-288 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/bmc.1130090620
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  • 57
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    Chiral separation of naphthalene-2, 3-dialdehyde labelled peptides by cyclodextrin-modified electrokinetic chromatography (1995)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 9 (1995), S. 295-301 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: The chiral separation of several dipeptide enantiomers, derivatized by naphthalene-2,3-dialdehyde (NDA), was achieved by use of cyclodextrin-modified micellar electrokinetic chromatography (CD-MEKC). The dipeptides contained one or two chiral centers. In the case of several dipeptides containing two chiral centers, all four of the optical isomers could be separated and baseline resolved in less than 15 min with 20 mM γ-CD and 50 mM sodium dodecyl sulphate (SDS) in the background electrolyte. The order of elution of these derivatized dipeptides was explained by considering important chemical equlibria in the SDS, CD and peptide system. Additionally, the influence of geometric location of the chiral center, the structure of the side-chain and the effect of CD concentration on the resolution are discussed.
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    Degradation of organophosphorus and carbamate pesticides in soils - HPLC determination (1995)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 9 (1995), S. 18-22 
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    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: Best conditions suited for the extraction and trace analysis of dimethoate, malathion, methyl-parathion, carbaryl, carbendazim and carbofuran in soils, using HPLC, were established, Theis was followed by studies related to persistence of residues in different soils, Half-life and take for 95% dissipation were determined in each case, Higher Ph, moderate mosture and hihg calcium carbonate content aided degradation while organic matter increased persistence.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/bmc.1130090104
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  • 59
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    Gas chromatographic determination of enantiomers as diastereomers following pre-column derivatization and applications to pharmacokinetic studies: A review (1995)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 9 (1995), S. 1-9 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: The introduction of chiral chromatographic methods has revolutionized the art of separationand quantitation of chiral drugs in biological fluids. A large number of chiral derivatization reagents for various funtional grups are available commercially. Therefore, Pre-column derivation methods have become attractive and simple for the gas chromatographic assays in biologcal fluids. The intent of this article is to review the pre-column chiral derivatization reagents employed in gas chromatographic separations and analyses of enantiomers. A discussion of numerous procedures necessary to develop a quantitative gas chromatographic assay method for drug enantiomers is presented. In this regard, quantitative gas chromatographic assays based on this approach have been applied to investigate the stereoselective pharmacokinetics of several chiral drug such as fenfluramine, norfenfluramine, methylphenidate, etodolac, propranol, suprofen and methoxyphenamine.
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    URL: http://dx.doi.org/10.1002/bmc.1130090102
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    Purification of murine immunoglobulin M from spent tissue culture supernatant by one-step gel filtration chromatography procedure (1995)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 9 (1995), S. 42-47 
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    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: Optimal purification of immunoglobulin M (IgM) grown as spent tissue culture supernatant can be achieved by a straightforward size-exclusion chromatography procedure. Preparative isolation of IgM was achieved by precipitation with saturated ammonium sulphate to achieve a 45% solution. IgM was then purified by gel filtration chromatography with a solution of 100 mM Tris+150 mM NaCl at pH 8. Denaturing electrophoresis and Western immunoblotting revealed two prominent bands at 80 and 25 kDa, indicative of the heavy and light chains of IgM respectively. The specific immunoreactivity of this IgM was assessed by a modified enzyme antigen capture assay. In contrast to affinity and ion-exchange chromatographies, gel filtration allows retention of IgM immunoreactivity.
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    URL: http://dx.doi.org/10.1002/bmc.1130090109
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    Masthead (1995)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 9 (1995) 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bmc.1130090201
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  • 62
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    High-performance liquid chromatographic assay for the quantitation of nadolol in human plasma using fluorescence detection (1995)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 9 (1995), S. 75-79 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A rapid and sensitive HPLC-fluorescence assay was developed and validated for the determination of nadolol, a β-blocker, in human plasma. Nadolol and the internal standard (desmethyl nadolol) were extracted from alkalinized plasma into methyl-tert.-butyl ether. The organic solvent was evaporated under nitrogen at 40°C. The residue was reconstituted in the mobile phase and injected on to a C18 silica column (25 cm × 4.6 mm i.d.) at a flow rate of 1.4 mL/min. The mobile phase was 0.05 M monobasic ammonium phosphate (pH 4.2) and acetonitrile (84:16, v/v). Fluorimetric detection was performed at excitation 230 nm and emission 330 nm. The nominal retention times were 3.3 and 4.3 min for the internal standard and nadolol, respectively. The lower limit of quantitation was 5 ng/mL and linearity (R2 ≥ 0.994) of the standard curve was demonstrated between 5 and 500 ng/mL. The analysis of quality control (QC) samples at 60, 200 and 400 ng/mL resulted in precision estimates ≤7.0% relative standard deviation (RSD) for the inter-assay and ≤6.3% RSD for intra-assay. The predicted concentrations of the QC samples deviated 〈10% from the nominal values. The extraction recovery of nadolol from human plasma was 64%. Nadolol was stable in human plasma at -20°C for at least 5 months and for at least three freeze-thaw cycles. Nadolol and the internal standard were stable in the autosampler at 5°C for at least 40 h. Overall, the assay was accurate, precise, sensitive, specific and reproducible for the analysis of nadolol in plasma. The validated assay procedure was applied to study the pharmacokinetics of nadolol after administration of single and multiple doses to human subjects.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/bmc.1130090204
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    A sensitive high-performance liquid chromatographic assay for the cholecystokinin-b antagonist, CI-988, in human and monkey plasma (1995)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 9 (1995), S. 94-97 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A sensitive and specific high-performance liquid chromatographic assay for the non-peptide cholecystokinin subtype B receptor antagonist, CI-988, in human and cynomolgus monkey plasma has been developed and validated. The method involves isolation of CI-988 and internal standard by batch robotic solid phase extraction with a C18 cartridge, liquid chromatographic separation on a C18 column and quantitation by fluorescence detection. The human plasma assay is linear from 0.25 to 500 ng/mL for a 1.00-mL plasma aliquot. Assay precision for CI-988 based on human plasma quality control samples was within ±7.2% relative standard deviation with an accuracy of ±5.6% relative error. The monkey plasma assay is linear from 1.00 to 250 ng/mL for a 0.500-mL plasma aliquot. Assay precision based on monkey plasma quality control samples was within ±11.0% relative standard deviation with an accuracy of ±2.6% relative error.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bmc.1130090208
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  • 64
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    Reversed-phase high-performance liquid chromatography of fullerenes with tetrahydrofuran-water as a mobile phase and sensitive ultraviolet or electrochemical detection (1995)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 9 (1995), S. 110-111 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: Fullerenes (C60 and C70) were separated on a reversed-phase high-performance liquid chromatography column with a mobile phase of tetrahydrofuran-water (70:30, v/v) and detected with ultraviolet or electrochemical detection. A baseline resolution of C60 and C70 was achieved with a capacity factor values of 7.6 and 10.8 respectively and a resolution of 3.7. The detection limit for C60 was 0.1 pmol on column and was nearly the same for both detection methods.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bmc.1130090212
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  • 65
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    Isolation and characterization of new porphyrin metabolites in human porphyria cutanea tarda and in rats treated with hexachlorobenzene by HPTLC, HPLC and liquid secondary ion mass spectrometry (1995)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 9 (1995), S. 113-122 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: Porphyrin metabolisms in human porphyria cutanea tarda (PCT) and in rats treated with hexachlorobenzene (HCB) have been studied in detail by high performance thin layer chromatography (HPTLC), high performance liquid chromatography (HPLC) and liquid secondary ion mass spectrometry (LSIMS). The analyses of porphyrin metabolites in the urine, faeces and liver biopsies of patients with PCT have shown that apart from uroporphyrin I and III and their expected decarboxylation intermediates and products, a complex mixture of many other porphyrins are present. The new porphyrins identified are: meso-hydroxyuroporphyrin III, β-hydroxypropionic acid uroporphyrin III, hydroxyacetic acid uroporphyrin III, peroxyacetic acid uroporphyrin III, β-hydroxypropionic acid heptacarboxylic acid porphyrin III, hydroxyacetic acid heptacarboxylic porphyrin III and peroxyacetic acid pentacarboxylic porphyrin III.
    Additional Material: 13 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bmc.1130090302
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  • 66
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    Use of liquid chromatography for the determination of interactions between bioactive compounds (1995)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 9 (1995), S. 157-161 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: Molecular interactions can be easily determined both by thin-layer and high performance liquid chromatography. The theory and practice of the determination of molecular interactions and the various methods for the calculation of complex stability are presented. Examples of the applications of liquid chromatographic methods for the measurements of molecular interactions are also discussed.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bmc.1130090402
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  • 67
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    Determination of free fatty acids in blood, tagged with 4-(2-carbazoylpyrrolidin-1-yl)-7-(N, N-dimethylaminosulfonyl)-2, 1, 3-benzoxadiazole, by high-performance liquid chromatography with fluorescence detection (1995)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 9 (1995), S. 162-170 
    Details
    ISSN: 0269-3879
    Keywords: Tagging reagent ; pre-column derivatization ; free fatty acid in rat serum and human plasma ; fluorescence detection ; high-performance liquid chromatography ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: The free fatty acids in blood were determined by high-performance liquid chromatography (HPLC) after pre-column tagging with 4-(2-carbazoylpyrrolidin-1-yl)-7-(N,N-dimethylaminosulphonyl)-2, 1, 3-benzoxadiazole (DBD-ProCZ). The tagging conditions were optimized with palmitic acid (C16:0) and linoleic acid (C18:2) as representative free fatty acids, saturated and unsaturated, respectively. Under the mild reaction conditions of room temperature for 90 min in dimethylformamide (DMF) containing 1-ethyl-3-(3-dimethylaminopropyl)-carbodiimide hydrochloride (EDC, 0.2 M)/pyridine (2%), all the fatty acids tested were tagged with the DBD-ProCZ to produce highly fluorescent derivatives which emit light at 550 nm (excitation at 450 nm). The fluorescence wavelenghts were essentially the same for all fatty acids, whereas the intensities were different for individual fatty acids. The derivatives obtained from ten free fatty acids were completely separated by reversedphase chromatography with two isocratic elution conditions. The on-column detection limit (signal-to-noise ratio of 3) with proposed HPLC separation and fluorescence detection is in the range of 19 (palmitic acid) -176 fmol (palmitoleic acid). The free fatty acids in rat serum and human plasma were successfully determined using the present method.
    Additional Material: 9 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bmc.1130090403
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  • 68
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    Availabilty of phenylisothiocyanate for the amino acid sequence/configuration determination of peptides containing D/L-amino acids (1995)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 9 (1995), S. 195-196 
    Details
    ISSN: 0269-3879
    Keywords: Phenylisothiocyanate ; PITC ; D/L-amino acid sequence ; peptide containing D-amino acid ; HPLC ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A potential use for phenylisothiocyanate (PITC), the most popular Edman reagent, is presented for analysis of the amino acid sequence and configuration in peptides containing D/L-amino acids. After derivatization with PITC of the N-terminal amino acid (L-Tyr) of an enkephalin analogue, [D-Ala2, D-Leu5]-enkephalin, followed by cleavage/cyclization with trifluoroacetic acid at 50°C for 5 min, the liberated 2-anilino-5-thiazolinone-L-Tyr (ATZ-L-Tyr) was further treated with 20% aqueous trifluoroacetic acid at 50°C for 10 min. The resultant phenylthiohydantoin (PTH)-L-Tyr was then separated on a chiral stationary phase (a penylcarbamoylated cyclodextrin column), retaining its configuration. The residual sequence and configurations of the peptide (D-Ala-Gly-L-Phe-D-Leu) were also determined by separating the corresponding PTH-D- or L-amino acids on chiral columns. This method may be applicable to an automatic Edman sequence analyzer for the configuration determination of peptides containing D/L-amino acids.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bmc.1130090410
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  • 69
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    High-performance liquid chromatography with fluorescence detection of ebiratide using 4-(N, N-dimethylamino-sulphonyl)-7-fluoro-2, 1, 3-benzoxadiazole as a fluorogenic reagent (1995)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 9 (1995), S. 216-220 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A sensitive high-performance liquid chromatography (HPLC) method with fluorescence detection has been developed and applied to the determination of ACTH4-9 analogue (ebiratide), 4-(N,N-Dimethylamino-sulphonyl)-7-fluoro-2,1,3-benzoxadiazole (DBD-F) was used as a fluorogenic labelling reagent.Ebiratide in 0.1 m borate buffer (pH 9.0) was reacted with DBD-F in acetonitrile solution at 50°C for 30 min. After cooling, the mixture was seperated by a reversed-phase HPLC. Then DBD-ebiratide was monitored at 580 nm with the excitation at 440 nm. The calibration curve was liner up to 10 pmol on column (r=0.999) with the detection limit of 0.25 pmol (signal-to-noise=3).
    Additional Material: 7 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bmc.1130090505
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  • 70
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    Simultaneous determination of nadolol enantiomers in human plasma by high-performance liquid chromatography using fluorescence-detection (1995)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 9 (1995), S. 140-145 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A high-performance liquid chromatographic assay is described for the separation and quantification of nadolol isomers in human plasma. The isomers were quantified using reverse-phase HPLC and fluorometric detection after derivatization with the chiral reagent R(-)-1-(naphthyl)ethylisocyanate [R(-)-NEI]. The N-isopropyl analogue (one isomer) of nadolol was used as the internal standard. The method was reproducible based on precision studies where the percent relative standard deviation was less than 15%. The lower limit of quantitation for each isomer was 2.5 ng/mL. This method was used to evaluate the pharmacokinetic profile of nadolol isomers in human subjects following both single and multiple oral dosing.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bmc.1130090306
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  • 71
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    Determination of salicylic acid in plasma by gas chromatogrphy using steam as carrier gas (1995)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 9 (1995), S. 155-156 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A gas Chromatogrphy method using steam as the carrier gas was established for the determination of salicylic acid in plasma. A 0.5 mL plasma sample was mixed with 0.5 mL of 6N HCl and then extracted with 2 mL of dichloromethane. The dichloromethane was evaporated to dryness and the residue was redissolved in 0.5 mL of water and then analysed by gas Chromatogrphy using steam as the carrying gas. The result was calculated by external standardization.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bmc.1130090310
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  • 72
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    TLC characterization of liposomes containing D-myo-inositol derivatives (1995)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 9 (1995), S. 175-178 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: The thin-layer chromatographic (TLC) behaviour of liposomes containig inositol phosphates (IPs) was studied. The liposomes contained different concentrations of D-myo-inositol 1, 4, 5-trisphosphate (IP3), D-myo-inositol 1, 2, 6-trisphosphate (α-trinositol, PP 56, a novel Perstorp Pharma derivative), D-myo-inositol 1, 3, 4, 5-tetrakisphosphate (IP4), D-myo-inositol 1, 3, 4, 5, 6-pentakisphosphate (IP5) and D-myo-inositol 1, 2, 3, 4, 5, 6-hexakisphosphate (IP6). Migration of all liposome batches was compared to that of control liposomes (containing only triple-distilled water), and to that of free phosphatidylcholine (PC); the same amount of lipid was used in all situations.Thin-layer chromatography was performed on silica gel as adsorbent. As solvent we used an n-buthanol: ethanol: water mixture in a 4:3:3 volume ratio. Significant differences were found between PC and all liposome batches, as well as between control liposomes and the ones containing IP3, α-trinositol, IP4, or IP5, in various concentrations. Liposomes containing IP6 migrate completely differently compared not only to phosphatidylcholine and control liposomes, but also to the ones containing other IPs (〈10-3 M). Unlike the other IPs studied, liposome-entrapped IP6 elicits dose-independent contractions of the isolated rat aorta. This suggests that liposomes loaded with IP6 undergo, during or after their preparation, physico-chemical alterations that eventually change their drug-delivery capacity.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bmc.1130090405
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  • 73
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    Announcement (1995)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 9 (1995), S. i 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bmc.1130090411
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  • 74
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    Optimization of enantiomeric separations for basic compounds in capillary zone electrophoresis using neutral and anionic cyclodextrins as chiral selectors (1995)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 9 (1995), S. 265-266 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bmc.1130090609
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  • 75
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    Microcolumn liquid chromatography of macromolecules in the critical mode (1995)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 9 (1995), S. 273-275 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bmc.1130090613
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  • 76
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    Determination of nitroimidazole residues in poultry tissues, serum and eggs by high-performance liquid chromatography (1995)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 9 (1995), S. 238-242 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A simple high-performance liquid chromatographic (HPLC) method was developed for determination of dimetridazole and metronidazole residues in poultry muscle, liver, serum and eggs. The drug residues were extracted from tissues and egg samples with acetonitrile followed by solid-phase extraction clean-up and HPLC analysis with photodiode array detector. Serum samples were treated with trichloroacetic acid, centrifuged and analysed without further clean-up. The detection limits were 2 ng/g and 5 ng/mL of analysed tissue (egg) and serum samples, respectively. Average recoveries for spike levels of 10 and 20 ng/g ranged from 82 to 94%, and coefficients of variation were below 10%.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bmc.1130090510
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  • 77
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    One day conference on miniaturization in liquid chromatography versus capillary electrophoresis (1995)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 9 (1995), S. 249-249 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bmc.1130090602
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  • 78
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    A comparative study for the determination of ibuprofen in pharmaceutical preparations using different internal column diameters (1995)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 9 (1995), S. 259-260 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Additional Material: 2 Tab.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bmc.1130090606
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  • 79
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    Announcement (1995)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 9 (1995), S. i 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bmc.1130090113
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  • 80
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    Investigation of enantioselective ofloxacin - albumin binding and displacement interactions using capillary affinity zone electrophoresis (1995)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 9 (1995), S. 68-74 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: The direct chiral separation of ofloxacin by capillary affinity zone electrophoresis using serum albumins from different animal sources as chiral selector in the supporting electrolyte is described. In addition, the effects of displacers on the mobility and enantioselectivity of ofloxacin were studied. Firstly, the separation behaviour of the enantiomers of the ofloxacin (OFLX) and tryptophan (Trp) was compared. The influence of albumin types, including chemically modified bovine serum albumins (BSAs), and buffer types on the migration behaviour of enantiomers was investigated. The results showed that stereoselectivity of Trp is independent of the type of albumin used. However, chiral separation of OFLX depends on the biological species of albumin. Use of chemically modified BSA led to poorer resolution of enantiomers. Only with acetylated BSA could chiral separation of Trp be achieved. Using Good's buffer solutions (DIPSO and HEPES) as a supporting electrolyte affected the migration times of OFLX enantiomers. Finally, a variety of displacers were added to the buffer along with the protein, and the effects on separation behaviour were observed. The displacers included warfarin, ketoproten, diazepam, propranolol, benzoinphenylbutazone, digitoxin and octanoic acid. From the results obtained, it is concluded that capillary affinity zone electrophoresis using albumin as a chiral selector may allow screening of OFLX-displacer interactions.
    Additional Material: 7 Ill.
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    URL: http://dx.doi.org/10.1002/bmc.1130090203
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    The development of a sensitive myo-inositol analyser using a liquid chromatograph with a post-label fluorescence detector (1995)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 9 (1995), S. 146-149 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A sensitive liquid chromatographic analysis for myo-inositol was developed using glycocyamine as the postlabelling reagent. The sensitivty was 500 pmol/injection. The system was applied to analyse myo-inositol in sera from eight patients with chronic renal failure. The average concentration of serum myo-inositol was 498.6 ± 257.0 μmol/L before haemodialysis, and 244.0 ± 131.1 μmol/L after haemodialysis. These results indicated that the kidney is the main site of myo-inositol metabolism.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bmc.1130090307
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  • 82
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    Masthead (1995)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 9 (1995) 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bmc.1130090601
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  • 83
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    Injection-generated solvent and pH gradients for sample enrichment on injection of large volumes in microcolumn liquid chromatography (1995)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 9 (1995), S. 254-256 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bmc.1130090604
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  • 84
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    LC-study of lonazolac, naproxen and related non-steroidal anti-inflammatory drugs in a classical and a narrow-bore setup applying UV and fluorescence detection (1995)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 9 (1995), S. 263-264 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bmc.1130090608
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  • 85
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    Temperature control in capillary electrophoresis systems (1995)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 9 (1995), S. 271-272 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bmc.1130090612
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  • 86
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    An LC assay using a microcolumn coupled to a U-shaped optical cell for high sensitivity UV absorbance detection of oxcarbazepine and its major metabolite in microdialysates (1995)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 9 (1995), S. 277-278 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bmc.1130090615
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  • 87
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    Determination of oxeladin in human plasma by gas chromatography - mass spectrometry (1995)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 9 (1995), S. 32-35 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A capillary gas chromatographic method with mass-selective detection was developed for the determination of oxeladin in human plasma. Plasma samples (1 mL) were alkalinized and extracted using 5 mL of hexane: isoamyl alcohol (99:1). The method was demonstrated to be sensitive (limit of quantitation at 1 ng/mL), linear between 1 and 150 mg/mL, accurate and precise enough (mean error and mean coefficient of variation at the limit of quantitation were 2.3 and 13.3%, respectively) to support pharmacokinetic evaluation of the drug at doses down to 30 mg.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bmc.1130090107
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    High-performance liquid chromatography and fluorometric detection of arachidonylethanolamide (anandamide) and its analogues, derivatized with 4-(N-chloroformylmethyl-N-methyl) amino-7-N, N-dimethylaminosulphonyl-2,1,3-benzoxadiazole (DBD-COCl) (1995)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 9 (1995), S. 56-57 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: The endogeneous ligand for the cannabinoid receptor, arachidonylethanolamide (anandamide) and its analogues, oleinylethanolamide, palmitylethanolamide and eicosapentaenoylethanolamide, were derivatized with a fluorogenic reagent, 4-(N-chloroformylmethyl-N-methyl)amino-7-N, N-dimethylaminosulphony 1-2,1,3-benzoxadiazole (DBD—COCl). They were separated on a reversed phse HPLC with a mobile phase of acetonitrile: water. The fluorometric detection of the derivatives was made at 560 nm with excitation at 450 nm and the detection limits for anandamide was 20 fmol on column. The structures of DBD—CO-ethanolamides were confirmed by liquid chromatography-atmospheric pressure chemical ionization - mass spectrometry (LC—APCI—MS).
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bmc.1130090112
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  • 89
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    Dye - ligand affinity chromatography on continuous beds (1995)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 9 (1995), S. 80-84 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: Continuous beds derivatized with three triazine dyes (Cibacron Blue 3G-A, Pricon Red HE-3B and Pricon Red H-3B) were used for chromatographic purification of dehydrogenases from yeast enzyme concentrate. All three columns, which were prepared by a very simple and cost-effective method, provided strong binding of glucose-6-phosphate dehydrogenase and lactate dehydrogenase. The Cibacron Blue 3G-A column showed high affinity for alcohol dehydrogenase. Under the same conditions, the Pricon Red HE-3B column showed a lower affinity and the Pricon Red H-3B column showed none. The adsorbed dehydrogenases were eluted specifically from the columns in high yields (71-113% by desorption with the coenzymes NADP, NADH and NAD respectively). Non-specific binding of human serum albumin and transferrin to these columns was also investigated. Enzyme assays and analyses by capillary electrophoresis showed that the continuous beds derivatized with triazine dyes gave a high degree of purification.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bmc.1130090205
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  • 90
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    Direct separation of tranylcypromine enantiomers and their profile in an atypical depressive patientPresented at the International Symposium on Molecular Chirality, April 24-27, 1994, Kyoto, Japan. (1995)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 9 (1995), S. 98-101 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: An isocratic and simple high-performance liquid chromatographic method is developed for the diirect resolution of the tranylcypromine (TCP) enatiomers. The method involves the use of an S-18-crown-6-ether chiral stationary phase known as the Crownpak CR (+) column. The stereochemical separation factor (α) obtained was 1.30 and the stereochemical resolution factor (Rs) was 0.69 when using a mobile phase consisting of 0.1 N perchloric acid containing 12% methanol at 23°C. The method has been used to monitor and identify, qualitatively, the profile of enantiomers of TCP in urine of an atypical depressive patient. It was found that the (-)-S-TCP concentration is significantly higher than the (+)-R-enantiomer.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bmc.1130090209
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  • 91
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    Occurrence of D-aspartic acid in rat brain pineal gland (1995)
    New York, NY : Wiley-Blackwell
    Biomedical Chromatography 9 (1995), S. 106-109 
    Details
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: We found a high concentration (1030 pmol per pineal gland) of D-aspartic acid (D-Asp) in the pineal gland of 6-week-old Sprague-Dawley (SD) rats. The content of D-Asp decreased with age, being 210 and 33 pmol per pineal gland in 28- and 45-week-old rats respectively. The proportion of D-Asp [(D-Asp/total Asp) × 100] also decreased with age, declining from 66% to 10% between 6 and 45 weeks after birth. The proportion of D-Asp did not differ between the sexes. The concentration of D-Asp was higher at night (at 2.00 a.m. 2830±485 pmol per pineal gland) than during the day (at 10.00 a.m. 1030±200 and at 3:00 p.m. 682±194 pmol per pineal gland), suggesting that biosynthesis of D-Asp in the pineal gland occurs at night. D-Asp was found to be distributed in the cytosol of pinealocytes, but its biological role remains unclear.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bmc.1130090211
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  • 92
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    Editorial (1995)
    New York, NY : Wiley-Blackwell
    Journal of Chemometrics 9 (1995), S. 1-2 
    Details
    ISSN: 0886-9383
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cem.1180090102
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  • 93
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    Deconvolution algorithms for instrumental applications: A comparative study (1995)
    New York, NY : Wiley-Blackwell
    Journal of Chemometrics 9 (1995), S. 3-20 
    Details
    ISSN: 0886-9383
    Keywords: Deconvolution algorithms ; Instrumental analysis ; Spectrometry ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Deconvolution algorithms for measurand reconstruction are considered. Their metrological and numerical properties are briefly characterized. Six algorithms most frequently used for instrumental applications are selected for closer analysis. Their comparative study is based on the use of spectrometric-type synthetic data, calorimetric-type synthetic data and spectrometric real-world data. Conclusions concerning computational complexity and accuracy of the compared algorithms as well as their metrological applicability are drawn.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cem.1180090103
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    FT-NIR Atlas, Michael Buback and Hans Peter Vogele, VCH, Weinheim, 1993, ISBN 3-527-28567-9, iv + 1067 pp., hardcover DM 880 (1995)
    New York, NY : Wiley-Blackwell
    Journal of Chemometrics 9 (1995), S. 67-68 
    Details
    ISSN: 0886-9383
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cem.1180090107
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    Masthead (1995)
    New York, NY : Wiley-Blackwell
    Journal of Chemometrics 9 (1995) 
    Details
    ISSN: 0886-9383
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cem.1180090201
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  • 96
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    Masthead (1995)
    New York, NY : Wiley-Blackwell
    Journal of Chemometrics 9 (1995) 
    Details
    ISSN: 0886-9383
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cem.1180090301
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  • 97
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    Application of procrustean methods to mid-and near-infrared spectral data (1995)
    New York, NY : Wiley-Blackwell
    Journal of Chemometrics 9 (1995), S. 125-135 
    Details
    ISSN: 0886-9383
    Keywords: Procrustean analysis ; FT-IR spectroscopy ; NIR spectroscopy ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Procrustean methods allow the fitting of a given matrix to another given matrix observed on the same objects. In the traditional approach orthogonal constraints are imposed upon the transformation matrix, whereas in the alternative approach Procrustean analysis may be performed without such constraints. The two methods (with and without constraints) were compared on data dealing with mid- and near-infrared spectra of oil. The aim was to reconstruct the mid-infrared spectral information using data from the near-infrared spectra. Unconstrained Procrustean analysis proved to be the more efficient for both the calibration and verification sets. Furthermore, the analysis of the transformation matrix between the two infrared ranges made it possible to indicate wavelengths and wave numbers corresponding to the same chemical groups.
    Additional Material: 7 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cem.1180090204
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    A combined theory for PCA and PLS (1995)
    New York, NY : Wiley-Blackwell
    Journal of Chemometrics 9 (1995), S. 91-123 
    Details
    ISSN: 0886-9383
    Keywords: H-principle ; PCA ; PLS regression ; latent variable models ; quadratic models ; sensitivity analysis ; outlier tests ; prediction variances ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: We present here an algorithmic approach to modelling data that includes principal component analysis (PCA) and partial least squares (PLS). In fact, the numerical algorithm presented can carry out PCA or PLS. The algorithm for linear analysis and extensions to non-linear analysis applies to both PCA and PLS. The algorithm allows for combination of PCA and PLS types of models and therefore extends modelling to new types of models that involve combination of regression models and ‘selection of variation’ models, which is the idea of PCA-type models. The fact that the algorithm carries out both PCA and PLS shows that PCA and PLS are based on the same theory. This theory is based on the H-principle of mathematical modelling. The algorithm allows tests for outliers, sensitivity analysis and tests of submodels. These aspects of the algorithm are treated in detail. We compute various measures of sizes, e.g. of components, of the covariance matrix, of its inverse, etc. that show how much the algorithm has selected at each step. The analysis is illustrated by data from practice.
    Additional Material: 11 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cem.1180090203
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    Pattern recognition analysis of near-infrared spectra by robust distance method (1995)
    New York, NY : Wiley-Blackwell
    Journal of Chemometrics 9 (1995), S. 169-178 
    Details
    ISSN: 0886-9383
    Keywords: minimum volume ellipsoid (MVE) estimators ; robust distance method ; pattern recognition ; Hotelling's T2 statistics ; near-infrared spectra ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A method for pattern recognition analysis of near-infrared spectra has been developed using robust distances determined by minimum volume ellipsoid (MVE) estimators of multivariate location and scatter. Classical methods such as the Mahalanobis distance method often fail in the presence of a moderate number of outliers in a training data set, while robust distance methods can tolerate a considerably larger proportion of outliers in a training data set Outliers can be detected by their relatively large robust distances and can be excluded from a training set without a priori knowledge of the nature of the data set. In this paper the properties of a robust distance method are examined using near-infrared spectra of sulfamethoxazole and mixtures with its major degradation products, sulfanilic acid and sulfanilamide. The robust distance method successfully detected unacceptable samples (71.4%-89.3% (α = 0.05) or 78.6%-92.9% (α = 0.10)) even when they were inadvertently included in the training data set.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cem.1180090304
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    Data analyses or problem formulations? (1995)
    New York, NY : Wiley-Blackwell
    Journal of Chemometrics 9 (1995), S. 226-228 
    Details
    ISSN: 0886-9383
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cem.1180090309
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