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  • 1
    Electronic Resource
    Electronic Resource
    Optimized pressure-pulse splitless injection and electron-capture, negative ionization detection for the congener specific determination of compounds of technical toxaphene (1997)
    Springer
    Fresenius' journal of analytical chemistry 358 (1997), S. 812-817 
    Details
    ISSN: 1432-1130
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The goal of the study is the optimization of the congener specific determination of compounds of technical toxaphene (CTTs). For this reason GC/ECNI-MS and CTT standard mixtures are applied. The splitless injection is improved by pressure-pulse injection which yields significantly higher abundance of the CTTs than by the conventional constant flow injection technique. The abundance of low volatile CTTs like B9-1025 (Parlar #62) is increased by factor 3 or more. The pressure-pulse injection can easily be integrated in standard (constant flow splitless injection) methods without influencing the retention times and reproducibility. The GC oven program and the flow are optimized for the separation of CTTs on a non-polar CP-Sil 2 column. Problems caused by oxygen in the ion source are discussed.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/s002160050514
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  • 2
    Electronic Resource
    Electronic Resource
    Methodik zur gemeinsamen Erfassung fungicider Pflanzenbehandlungsmittel auf Citrusfrüchten und Obst mit Hilfe der HPLC und selektiver Detektion (1987)
    Springer
    European food research and technology 184 (1987), S. 195-197 
    Details
    ISSN: 1438-2385
    Source: Springer Online Journal Archives 1860-2000
    Topics: Process Engineering, Biotechnology, Nutrition Technology
    Description / Table of Contents: Zusammenfassung Die beschriebene HPLC-Methodik erlaubt die Bestimmung von Diphenyl, o-Phenylphenol, Thiabendazol, Diphenylamin und Ethoxiquin auf Citrusfrüchten und Obst (Nachweisgrenze: 0,1 mg/kg). Die Wirkstoffe werden mit Dichlormethan extrahiert und die Extrakte nach Konzentration und Filtration direkt mit Hilfe der HPLC und selektiver Detektion analysiert. Die chromatographische Trennung erfolgt an einer RP-Säule mit einem Formiat-Puffer als Eluenten. Die Arbeitsparameter der drei in Reihe geschalteten HPLC-Detektoren wurden optimiert, so daß eine gesuchte Komponente immer von mindestens zwei Detektoren empfindlich und störungsfrei angezeigt wird.
    Notes: Summary A HPLC-method is described for the determination of diphenyl, o-phenylphenol, thiabendazole, diphenylamine, and ethoxiquin in different fruits (detection limits: 0,1 mg/kg). The compounds are extracted with dichloromethane, and after concentration and filtration steps the determination is carried out by HPLC with selective detection. Chromatographic separation of fungicides is achieved by use of a RP-18 column with a methanolic formic acid buffer as eluent. The working parameters of three different HPLC-detectors (UV-, fluorimetric-, and electrochemical detector) are optimized, and it is shown that residues of the fungicides in plant materials can be determinated at least by two detectors without interferences.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01042206
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  • 3
    Electronic Resource
    Electronic Resource
    Schnellmethode zur Bestimmung von Monohalogenessigsauren in alkoholischen Getränken (1987)
    Springer
    European food research and technology 184 (1987), S. 30-32 
    Details
    ISSN: 1438-2385
    Source: Springer Online Journal Archives 1860-2000
    Topics: Process Engineering, Biotechnology, Nutrition Technology
    Description / Table of Contents: Zusammenfassung Ein Analysenverfahren wird beschrieben, das die schnelle Bestimmung von Monohalogenessigsäure-Rückständen gestattet. Nach Extraktion mit Diethylether werden die Säuren mit PFBBr bzw. n-Butanol/BF3 derivatisiert und die Derivate der Monohalogenessigsauren anschließend capillargaschromatographisch nachgewiesen. Die Nachweisgrenze betrug für Monochloressigsäure 0,1 mg/1, für Monobrom- und Monoiodessigsäure 0,01 mg/1.
    Notes: Summary A method is described for the rapid determination of residues of halogenated acetic acids in alcoholic beverages. After extraction with diethyl ether and derivatization with PFBBr and n-butanol/BF3 the derivatives of the acids are analysed by use of gas chromatography with capillary columns. The detection limits are 0.1 mg/1 for chloroacetic acid and 0.01 mg/1 for bromo- and iodoacetic acid.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01042340
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  • 4
    Electronic Resource
    Electronic Resource
    Zur Problematik der selektiven Erfassung von PSP-Toxinen aus Muscheln (1990)
    Springer
    European food research and technology 190 (1990), S. 491-495 
    Details
    ISSN: 1438-2385
    Source: Springer Online Journal Archives 1860-2000
    Topics: Process Engineering, Biotechnology, Nutrition Technology
    Description / Table of Contents: Summary Levels of paralytic shellfish poisoning (PSP) toxins in shellfish are routinely determined by mouse bioassay: In order to improve the qualitative and quantitative determination of PSP toxins, Chromatographic techniques with fluorescence detection have been developed. These HPLC methods and the HPLC/MS coupling were used to determine a second PSP toxin which was found, in addition to saxitoxin, in canned Spanish mussels. These canned mussels were rejected in 1986 by the German food control because PSP concentrations were too high. It has been shown that these samples contained mainly dc-saxitoxin.
    Notes: Zusammenfassung Die Messung der PSP-Belastung (paralytic shellfish poisoning) von Schalentieren erfolgt vor allem mit Hilfe des Maus-Biotestes. Um PSP-Toxine sowohl qualitativ als auch quantitativ besser bestimmen zu können, wurden chromatographische Verfahren mit Fluorescenzdetektion entwickelt. Diese HPLC-Methoden sowie die Kopplung HPLC/MS gelangten zum Einsatz, um in spanischen Muschelkonserven ein neben Saxitoxin vermutetes zweites PSP-Toxin nachzuweisen. Es zeigte sich, daß in den 1986 in der Bundesrepublik Deutschland wegen zu hoher PSP-Konzentrationen beanstandeten Muschelkonserven vor allem Decarbamoyl-Saxitoxin enthalten war.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01214068
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  • 5
    Electronic Resource
    Electronic Resource
    Vorkommen und Bestimmung von Okadasäure in Muscheln der deutschen Nordseeküste (1988)
    Springer
    European food research and technology 187 (1988), S. 421-424 
    Details
    ISSN: 1438-2385
    Source: Springer Online Journal Archives 1860-2000
    Topics: Process Engineering, Biotechnology, Nutrition Technology
    Description / Table of Contents: Zusammenfassung Es wird eine HPLC-Methode zur Erfassung der zur Gruppe der DSP-Toxine zählenden Okadasdure aus Muscheln beschrieben. Nach Extraktion des Wirkstoffes aus dem homogenisierten Hepatopankreaskomplex und Reinigung des Rohextraktes durch Flüssig/flüssig-Verteilungen wird Okadasäure mit 9-Anthryldiazomethan (ADAM) zu 9-Anthrylmethyl-Okadasäure (9-AM-OA) umgesetzt. Die weitere Reinigung des derivatisierten Extraktes erfolgt durch SPE an Kieselgel. An einer RP 18-Säule mit dem Eluenten CH3CN/THF/H20 und unter Einsatz von in Reihe geschaltetem Dioden-Array- und Fluoreszenz-Detektor gelingt die empfindliche und selektive HPLC-Bestimmung von 9-AM-OA (Nachweisgrenze: 0,5 μg Okadasäure/g Hepatopankreas).
    Notes: Summary A method for the determination of okadaic acid, a typical DSP toxin, in mussels is described. The homogenized hepatopancreas is extracted and the crude extract purified by liquid/liquid partition chromatography. The derivatization of okadaic acid to 9-anthrylmethyl-okadaic acid (9-AM-OA) is achieved using the derivatization reagent 9-anthryldiazomethane (ADAM) and the clean-up is carried out by SPE with silica gel. 9-AM-OA is determined by HPLC using a RP-18 column with CH3CN/THF/H2O as the eluent. The selective and sensitive detection of 9-AM-OA is performed by coupling UV and fluorimetric detectors (detection limit: 0.5 Vg okadaic acid/g hepatopancreas).
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01122642
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  • 6
    Electronic Resource
    Electronic Resource
    Extraction and determination of biogenic amines in fermented sausages and other meat products using reversed-phase-HPLC (1993)
    Springer
    European food research and technology 197 (1993), S. 230-232 
    Details
    ISSN: 1438-2385
    Source: Springer Online Journal Archives 1860-2000
    Topics: Process Engineering, Biotechnology, Nutrition Technology
    Description / Table of Contents: Abstract A convenient method is described for the analysis of biogenic amines (BA) by means of reversed-phase-HPLC. The method is characterized by multi-channel UV detection (diodearray), subsequent post-column derivatization with o-phthaldialdehyde and 3-mercaptopro-pionic acid, and fluorescence detection. For the analysis of meat products and especially fermented sausages an optimized perchloric acid extraction process was introduced to determine putrescine, cadaverine, histamine, tyramine and 2-phenylethylamine. BA recoveries from meat ranged between 96 and 113% with a detection limit for amines of 0.5 mg/kg.
    Notes: Zusammenfassung Eine Methode zur Analyse von biogenen Aminen (BA) mittels RP-HPLC wird beschrieben. Die Methode ist charakterisiert durch Mehrkanal-UV-Detektion (Diodenarray), anschließende Nachsäulen-derivatisierung mito-Phthaldialdehyd und 3-Mercapto-propionsäure und Fluorescenzdetektion. Zur Bestimmung von Putrescin, Cadaverin, Histamin, Tyramin und 2-Phenylethylamin wird ein optimierter Extraktionsprozeß unter Verwendung von Perchlorsäure vorgestellt. Die Ausbeuten der BA im Fleisch betragen zwischen 96 und 113% bei einer Nachweisgrenze von 0,5 mg/kg.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01185276
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  • 7
    Electronic Resource
    Electronic Resource
    Gas chromatographic separation of polychlorinated biphenyls on a new apolar capillary column (1994)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 17 (1994), S. 851-858 
    Details
    ISSN: 0935-6304
    Keywords: High resolution gas chromatography ; Chlorinated hydrocarbons ; Polychlorinated biphenyls ; PCB indicator congeners ; Coelution ; Toxic PCB congeners ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Eighty one polychlorinated biphenyls (PCBs) and nineteen chlorinated pesticide standards have been analyzed on a newly developed apolar high resolution gas chromatography (HRGC) column. Emphasis was placed on the determination of PCB indicator congeners which are part of national regulations, and of toxic coplanar PCB congeners.The new column enables almost unambiguous quantification of the PCB indicator congeners (PCB 138 can be separated from both PCB 163 and PCB 164; PCB 28 and PCB 31 were also separated and no coelution was observed for PCB 52, PCB 118, and PCB 180). The new column furnished better results than CP-Sil 8 for the analysis of PCB indicator congeners in a sample of seal blubber.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/jhrc.1240171208
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  • 8
    Electronic Resource
    Electronic Resource
    Synthesis, isolation, and chromatography of perdeuterated α-1,2,3,4,5,6-hexachlorocyclohexane (1995)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 18 (1995), S. 643-646 
    Details
    ISSN: 0935-6304
    Keywords: Gas chromatography/Mass spectrometry ; Chiral GC ; Deuterium-labeled compounds ; Hexachlorocyclohexane ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Perdeuterated α-1,2,3,4,5,6-hexachlorocyclohexane (α-PDHCH) was synthesized and isolated in pure form. α-PDHCH was baseline separated from unlabeled α-HCH by high resolution gas chromatography on different stationary phases. α-PDHCH was also resolved into its enantiomeric forms by application of a chiral GC phase. Furthermore, chiral chromatography of a mixture of labeled α-PDHDH and unlabeled α-HCH resulted in four peaks. Standard solutions of α-PDHCH are recommended both as recovery standard for sample clean-up and as internal standard for the quantitation of chlorinated hydrocarbons with GC/MS or GC/ECD in environmental samples.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/jhrc.1240181006
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  • 9
    Electronic Resource
    Electronic Resource
    Partial structure elucidation of the most abundant octa and nonachlorotoxaphene congeners in marine mammals by using conventional electron ionization mass spectrometry and mass spectrometry/mass spectrometry (1993)
    Springer
    Fresenius' Zeitschrift für analytische Chemie 347 (1993), S. 502-512 
    Details
    ISSN: 1618-2650
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Conventional electron ionization (EI) mass spectrometry (MS) and MS/MS techniques were applied to the analysis of two abundant octa and nonachlorobornanes isolated from seals of the Baltic sea and originating from technical toxaphene. The exact sterical structures of the two compounds were previously determined using nuclear magnetic resonance (NMR) spectroscopy by two independent research groups. The MS and MS/MS data generated in this study allowed partial structure elucidation of these polychlorobornanes, in particular revealing the distribution of the Cl substituents between the six-membered carbon ring, the bridge and the bridgehead in the parent bornane structure. Fragmentation of the six-membered carbon ring and the bridge by retro-Diels-Alder (RDA) and related mechanisms was discovered by studying specific parent/daughter ion transitions. The detailed fragmentation pathways formulated may be applicable to the structure elucidation of other toxaphene congeners and the monitoring of strategic transitions is highly selective for the detection of these compounds in technical toxaphene and in environmental samples.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00324244
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  • 10
    Electronic Resource
    Electronic Resource
    An unequivocal1H NMR structural assignment of TOX8 and TOX9, the two most abundant toxaphene congeners in marine mammals (1994)
    Springer
    Fresenius' Zeitschrift für analytische Chemie 349 (1994), S. 552-558 
    Details
    ISSN: 1618-2650
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The structure of the two most abundant toxaphene congeners has unequivocally been established by 500 MHz1H NMR spectroscopy as 2-endo,3-exo,5-endo, 6-exo,8,8,9,10,10-nonachlorobornane (TOX9) and as 2-endo,3-exo,5-endo,6-exo,8,8,10,10-octachlorobornane (TOX8). Semiempirical calculations (AM1 and PM3-MNDO) were carried out for both structures. The distance information found by nuclear Overhauser enhancement (NOE) for the protons is in agreement with the energy minimized AM1 and PM3-MNDO structures. For these definitively established NMR data for TOX8 and TOX9, together with literature data for other toxaphene isolates, a set of rules has been derived for1H chemical shifts in polychlorinated bornane structures. A set of rules is also proposed for assigning systematical nomenclature to NMR-derived polychloro bornane structures.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00323993
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