Quantitative analysis of ethylenediamine in plasma by capillary column gas chromatography

A specific and sensitive method for the determination of ethylenediamine in human plasma is described. The aqueous sample is treated with m-toluoyl chloride, yielding the N,N′-bis(m-toluoyl) derivative of the diamine, which is extracted into dichloromethane and quantitated after “on column” methylation by capillary gas liquid chromatography with alkali flame ionization detection. The corresponding derivative of putrescine serves as internal standard. The assay is reproducible and calibration curves are linear over the concentration range 0.05 to 10 μg · ml^?1. The lower detection limit is about 10 ng · ml^?1. The structures of the compounds of interest eluting from the capillary column are examined by gas liquid chromatography/mass spectrometry. The assay has been applied to the analysis of ethylenediamine in plasma following the administration of aminophylline and ethylenediamine in a cross-over study to patients with bronchopulmonary diseases. The method also proves suitable for measuring other primary and secondary amines and diamines in aqueous solutions by gas liquid chromatography.     

Simultaneous determination of neopynamine and piperonyl butoxide by capillary column gas-liquid chromatography

A method is developed for the simultaneous determination of neopynamine and piperonyl butoxide by chromatography on a quartz capillary column using flame ionization detection. Benzyl mandelate is used as an internal standard. Calibration graphs are linear down to at least 3.75 mg% and 3 mg% for neopynamine and piperonyl butoxide, respectively.     

Simultaneous determination of nicotine and cotinine in plasma by capillary gas liquid chromatography with nitrogen-sensitive detection

Conclusion By the use of structural analogues of nicotine and cotinine as internal standards, the elimination of environmental sources of contamination and an exact clean-up procedure, we were able to develop a rapid and sensitive method which has acceptable accuracy and precision over the concentration range necessary in pharmacokinetic studies.

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Gleichzeitige Bestimmung von Nicotin und Cotinin in Plasma mit Hilfe der Capillar-Gas-Chromatographie

     

Improved automated simultaneous determination of isosorbide dinitrate and its metabolites in plasma by capillary column gas chromatography

An automated specific and sensitive method for the simultaneous determination of isosorbide dinitrate and its metabolites isosorbide-2-mononitrate, isosorbide-5-mononitrate, isomannide mononitrate, and isoidide mononitrate at concentrations down to 0.5, 1, 3, 2, and 2 ng/ml, respectively, in human plasma is described. The procedure involves the extraction of the drug and its metabolites together with their internal standards isomannide dinitrate and o-nitrobenzyl alcohol from plasma with dicholromethane. The analysis is carried out by fused silica capillary gas chromatography using a ⁶³Ni-electron capture detector. The method is applied to the pharmacokinetics of isosorbide dinitrate in humans.     

Simultaneous determination of paracetamol and chlorpheniramine in human plasma by liquid chromatography-tandem mass spectrometry

An analytical method for the determination of paracetamol and chlorpheniramine in human plasma has been developed, validated and applied to the analysis of samples from a phase I clinical trial. The analytical method consists in the extraction of paracetamol and chlorpheniramine with diethyl ether, followed by the determination of both drugs by an LC–MS–MS method, using 2-acetamidophenol as internal standard. The intra-assay and inter-assay precision and accuracy of this technique were good and the limit of quantitation was 0.5 μg/ml of plasma for paracetamol and 0.2 ng/ml for chlorpheniramine. The concentration working range was established between 0.5 μg/ml and 25 μg/ml for paracetamol and between 0.2 ng/ml and 50 ng/ml for chlorpheniramine. This method has been used for analyzing more than 1200 human plasma samples from a clinical study with 24 volunteers.     

Simultaneous determination of chlorpheniramine and pseudoephedrine in human plasma by liquid chromatography-tandem mass spectrometry

A sensitive and specific procedure for simultaneous quantitation of chlorpheniramine and pseudoephedrine in human plasma has been developed and validated. Analytes were extracted from plasma samples by liquid-liquid extraction, separated on a Diamonsil C18 column (250 x 4.6 mm i.d.) and detected by tandem mass spectrometry with an atmospheric pressure chemical ionization interface. Diphenhydramine was used as the internal standard. The method has a lower limit of quantitation of 0.2 and 2.0 ng/mL for chlorpheniramine and pseudoephedrine, respectively. The intra- and inter-day relative standard deviation, calculated from quality control (QC) samples were below 4.3% for chlorpheniramine and below 9.5% for pseudoephedrine. The inter-day relative error as determined from QC samples was within 4.7% for each analyte. The overall extraction recoveries of chlorpheniramine and pseudoephedrine were 77 and 61% on average, respectively. The method was successfully applied to pharmaockinetic study of chlorpheniramine and pseudoephedrine in volunteers receiving formulations containing 4 mg of chlorpheniramine maleate and 60 mg of pseudoephedrine hydrochloride.     

Quantitative determination of nitroglycerin in human plasma by capillary gas chromatography with electron-capture detection

A sensitive method for the selective determination of nitroglycerin at concentrations down to 50 pg/ml in human plasma is described. After the addition to plasma of a known amount of butane-1,2,4-triol trinitrate as internal standard, both compounds are extracted into hexane. Nitroglycerin is then quantitated by capillary gas chromatography with electron-capture detection.     

Simultaneous determination of butyltin and phenyltin compounds in oysters by capillary gas chromatography

A method is described for the simultaneous determination of butyl- and phenyltin compounds in oyster samples. The organotin compounds were extracted (as chlorides) from oyster homogenates with hydrochloric acid and benzene in the presence of 0.05% tropolone. These compounds were converted into pentyl derivatives with pentyl Grignard reagent and then analysed by capillary gas chromatography with a flame photometric detector equipped with a 393-nm filter. The recoveries of six organotin compounds added to oyster samples ranged from 71 to 74%. The detection limits of butyl- and phenyltin compounds were in the 5-9 pg range as tin. We detected significant amounts of three organotin compounds (di- and tributyltin and triphenyltin) in oyster samples.     

Automated determination of nifedipine in human plasma by capillary gas chromatography with electron capture detection

A rapid, sensitive, and reliable method for the determination of nifedipine in human plasma is described. Using a single-step solvent extraction and capillary gas chromatography combined with electron capture detection, an assay sensitivity of 2 ng/ml is achieved routinely using 0.5 ml of plasma. Intact nifedipine is quantitated and separated from its nitroso- and nitropyridine-derivatives. The suitability of the assay for pharmacokinetic studies is illustrated.     

Quantitative determination of norethisterone acetate in human plasma by capillary gas chromatography with mass-selective detection

An analytical method for the determination of norethisterone acetate (NETA) in human plasma by capillary gas chromatography-mass-selective detection (GC-MS), with testosterone acetate as internal standard, was developed and validated. After addition of the internal standard, the compounds were extracted from plasma at basic pH into diethyl ether-dichloromethane (3:2 v/v), which was then evaporated to dryness. The compounds were converted into their pentafluoropropionyl derivatives which were determined by gas chromatography using a mass selective detector at m/z 486 for NETA and m/z 476 for the internal standard. Intra-day and inter-day accuracy and precision were found suitable over the range of concentrations between 0.10 to 10 ng/ml. The method was applied to clinical samples.     

Simultaneous microanalysis of bile acids and cholesterol in bile by glass capillary column gas chromatography

Simultaneous quantitative microanalysis of bile acids and cholesterol was carried out by enzymatic hydrolysis, the formation of the ethyl ester dimethylethylsilyl ether derivatives and subsequent analysis by glass capillary gas chromatography. A complete separation and satisfactory recovery of cholesterol and the five major bile acids commonly occurring in human and hamster bile were obtained. The method is applicable to individual small animal models such as hamster from which only a small amount of bile is available.     

Selective determination of organofluorine compounds by capillary column gas chromatography with an atmospheric pressure helium microwave-induced plasma detector

Fluorinated analogs of compounds typical of those found in metabolic and other biological studies are detected with high selectivity using a gas chromatograph/microwave-induced plasma detector (GC-MIPD), which permits fluorine-selective detection by monitoring the emission at 685.6 nm. Using the described atmospheric pressure helium-sustained plasma detector, the minimum detectable level, fluorine selectivity (relative to carbon), and linear dynamic range of this GC-MIPD system were determined to be 4.8 pg-F/s, 1060, and 5000, respectively. The utility of this GC-MIPD system for the selective detection of organofluorine compounds is demonstrated by its application in the analysis of the metabolic fate of a fluorinated substrate administered to a mixture of wheat germ phosphatase and potato apyrase, as well as by analysis of synthetic mixtures.