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  • 1
    Electronic Resource
    Electronic Resource
    Quantitative analysis of S3341 in human plasma and urine by combined gas chromatography - negative ion chemical ionization mass spectrometry: 15 month inter-day precision and accuracy validation (1987)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 14 (1987), S. 289-293 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A new quantitative assay for the determination of S3341, an alpha-2 agonist antihypertensive drug, has been developed using combined gas chromatography-negative ion chemical ionization mass spectrometry. The [M]-. ions from TFA derivatives of S3341 (m/z 276) and the internal standard (2H4)S3341 (m/z 280) are monitored simultaneously by selected ion monitoring. For S3341 concentrations ranging from the limit of detection (0.2 ng ml-1 using 1 ml of plasma) to 5 ng ml-1, the average assay precision (CV) is approximately 7% while the average assay accuracy (percentage of error) is 4%. Validation of the day-to-day precision and accuracy was realized after analysing control plasma samples (n = 295) concurrently with the biological samples collected during the pharmacokinetic studies conducted over 15 months. The average day-to-day precision (CV) and accuracy (percentage of error) are 10% and 6% respectively, thus indicating that this assay procedure routinely provides reliable analytical data.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200140608
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    Paper (German National Licenses)
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  • 2
    Electronic Resource
    Electronic Resource
    Quantitative measurement of clenbuterol at the femtomole level in plasma and urine by combined gas chromatography/negative ion chemical ionization mass spectrometry (1990)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 19 (1990), S. 80-88 
    Details
    ISSN: 1052-9306
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A highly sensitive and specific assay was developed for the quantitative measurement of clenbuterol at the femtomole level in human plasma and urine. Clenbuterol and the internal standard (2H9)clenbuterol were measured by gas chromatography/negative ion chemical ionization mass spectrometry with methane as the reagent gas. The two compounds of interest were extracted from the biological samples at pH 13 using ethyl acetate. After two subsequent purification steps, the cleaned-up organic extract was derivatized with pentafluoropropionic anhydride. The mass spectrometer was set to monitor the abundant [M — HCl]- ions of the perfluoroacyl derivatives (m/z 368 and 377), which were generated in the ion source by an electron capture process. This assay required 1 ml of plasma or 0.5 ml of urine and the detection limit of the method was 5 pg ml-1 with a 12.8% relative standard deviation. The accuracy of the clenbuterol assay was also tested day to day with quality control specimens spiked blind to the analyst. The mean difference between the theoretical and actual values was lower than 4.1%.
    Additional Material: 6 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200190206
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    Paper (German National Licenses)
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  • 3
    Electronic Resource
    Electronic Resource
    Quantitative measurement of zacopride in human plasma and urine by combined gas chromatography/negative ion chemical ionization mass spectrometry (1994)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 23 (1994), S. 572-580 
    Details
    ISSN: 1052-9306
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A highly sensitive and specific assay was developed for routine analysis of zacopride at the femtomole level in human plasma and urine. Zacopride and the deuterated internal standard [(2H3)zacopride] were measured by gas chromatography/negative ion chemical ionization mass spectrometry with methane as the reagent gas. A multiplestep liquid-liquid extraction procedure was used to isolate the two compounds of interest from complex biological matrices. Zacopride was converted to the fluorinated derivative with pentafluoropropionic anhydride. The mass spectrometer was tuned to monitor the very intense [M — HF]-ion at m/z 435 which was generated into the ion source by a dissociative capture process. This assay was performed with 1 ml of plasma or 0.2 ml of urine, and the quantification limit of the method was calculated as 10 pg ml-1 using a suitable statistical test. The very low relative standard deviation and mean percentage error values calculated during the within-day or between-day repeatability assays have clearly demonstrated the ruggedness of the technique for the routine quantitative measurement of zacopride in plasma and urine. Some preliminary results on the pharmacokinetics of this potent drug are presented to illustrate the applicability of this new powerful gas chromatographic/mass spectrometric method.
    Additional Material: 7 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200230907
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  • 4
    Electronic Resource
    Electronic Resource
    Quantitative measurement of clonidine in human plasma by combined gas chromatography/electron capture negative ion chemical ionization mass spectrometry (1988)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 17 (1988), S. 443-448 
    Details
    ISSN: 1052-9306
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A new quantitative and selective assay was developed for the measurement of low levels of clonidine in human plasma. The drug and the deuterated internal standard (2H4)clonidine are quantified by gas chromatography/negative ion chemical ionization mass spectrometry with methane as the reagent gas. After a three-step extraction procedure, the two compounds of interest are converted to their fluorinated derivatives using 3,5-bis(trifluoromethyl)benzoyl chloride. The mass spectrometer is focused to monitor abundant and stable characteristic high-mass ions (m/z 673 and 709) which are generated in the ion source by a resonance electron capture process. This assay requires only 1 ml of plasma sample and the limit of detection of the method is 5 pg ml-1 with a relative standard deviation of less than 7%.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200170605
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  • 5
    Electronic Resource
    Electronic Resource
    Quantitative measurement of BN50727 in human plasma and urine by combined liquid chromatography/negative ion chemical ionization mass spectrometry using a particle beam interface (1994)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 23 (1994), S. 581-589 
    Details
    ISSN: 1052-9306
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A new sensitive assay has been developed for the quantitative measurement of BN50727 at the picomole level in human plasma and urine. The drug and the internal standard (BN50788) were measured by combined liquid chromatography/negative ion chemical ionization mass spectrometry with methane as the reagent gas. A simple solid-liquid extraction procedure was used to isolate BN50727 from the complex biological matrices. The mass spectrometer was tuned to monitor the intense and stable ion at m/z 333 which was generated in the ion source by a dissociative capture process. This assay was performed with 1 ml of plasma or 0.1 ml of urine and the quantification limit of the method was statistically calculated as 1 ng ml-1. The very low relative standard deviations and mean percentages of error calculated during the different within-day or between-day repeatability assays have clearly demonstrated the ruggedness of the technique for the routine determination of BN50727 in biological fluids. Some preliminary results on the pharmacokinetics of the drug are presented to illustrate the applicability of this powerful liquid chromatographic/mass spectrometric method.
    Additional Material: 6 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200230908
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  • 6
    Electronic Resource
    Electronic Resource
    A rapid and highly sensitive method for the quantitative determination of dexamethasone in plasma, synovial fluid and tissues by combined gas chromatography/negative ion chemical ionization mass spectrometry (1990)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 19 (1990), S. 295-302 
    Details
    ISSN: 1052-9306
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A new, simple and highly sensitive assay is developed for the quantitative measurement of very low levels of dexamethasone in human plasma, synovial fluid and tissues following a topical administration of the drug. Dexamethasone and the internal standard, flumethasone, are measured by gas chromatography/negative ion chemical ionization mass spectrometry with methane as the reagent gas. After a three-step extraction procedure, the two compounds of interest are converted to their trimethylsilyl ether derivatives using trimethylsilylimidazole and formamide as the base catalyst. Under soft derivatization conditions only one chromatographic peak corresponding to the trisubstituted derivative is observed. The mass spectrometer is focused to monitor abundant and stable characteristic high-mass ions (m/z 446 and 464) which are generated in the ion source by an electron capture process. This assay requires only 1 ml of plasma or 0.5 ml of synovial fluid and the detection limit of the method is equal to 0.1 ng ml-1 with a relative standard deviation lower than 6%.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200190504
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    Paper (German National Licenses)
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  • 7
    Electronic Resource
    Electronic Resource
    Quantitative measurement of 4-hydroxy tamoxifen in human plasma and mammary tumours by combined gas chromatography/negative chemical ionization mass spectrometry (1993)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 22 (1993), S. 395-402 
    Details
    ISSN: 1052-9306
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A highly sensitive and specific assay was developed for the quantitative measurement of 4-hydroxy tamoxifen (4-OH Tam) at the femtomole level in human plasma and mammary tumours. The drug and deuterated internal standard (4-OH Tam D4) were measured by gas chromatography/negative chemical ionization mass spectrometry with methane as the reactant gas. The two compounds of interest were isolated from the complex biological matrices using a solid-phase extraction procedure with Extrelut 1 columns. Soft operating conditions were required to convert 4-OH Tam to the fluorinated derivatives with pentafluorobenzyl chloride. The mass spectrometer was tuned to monitor the abundant and stable molecular ions at m/z 581 and 585 which were generated in the ion source by an electron capture process. This assay required only 0.5 ml of plasma or 0.5 g of mammary tissue, and the quantification limits of the method were 20 pg ml-1 for the body fluids or 100 pg g-1 for the tissue samples. The very low relative standard deviation and mean percentage error calculated during the different within-day or day-to-day repeatability assays have clearly demonstrated the ruggedness of the technique for routine analysis of 4-OH Tam.
    Additional Material: 6 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200220706
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    Paper (German National Licenses)
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  • 8
    Electronic Resource
    Electronic Resource
    A highly sensitive assay of melatonin at the femtogram level in human plasma by gas chromatography/negative ion chemical ionization mass spectrometry (1994)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 23 (1994), S. 499-509 
    Details
    ISSN: 1052-9306
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A highly sensitive and specific assay was developed for routine analysis of melatonin at the femtogram level in human plasma. Melatonin and the deuterated internal standard [(2H4)melatonin] were measured by gas chromatography/negative ion chemical ionization mass spectrometry with methane as the reagent gas. A simple liquid-liquid extraction procedure was used to isolate the two compounds of interest from the complex biological matrix. Melatonin was converted to the fluorinated derivative with pentafluoropropionic anhydride. The mass spectrometer was tuned to monitor the very intense and stable ions at m/z 320 and 323 which were generated into the ion source by a dissociative capture process. This assay was conducted with 1 ml of plasma and the quantification limit of the method was statistically calculated as 0.5 pg ml- 1. The very low relative standard deviations and mean percentages of error calculated during the within-day or between-day repeatability assays have clearly demonstrated the ruggedness of the technique for the routine quantitative measurement of melatonin in plasma. Some results on the melatonin circadian rhythm are presented to illustrate the applicability of this powerful gas chromatographic/mass spectrometric method.
    Additional Material: 7 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200230807
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    Paper (German National Licenses)
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