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At least 253 records · Page 14Linked to original sources
PubMed1985

Determination of oxprenolol in human plasma by high-performance liquid chromatography, in comparison with gas chromatography and gas chromatography-mass spectrometry.

A high-performance liquid chromatographic method for the quantitative assay of oxprenolol in human plasma is described. After addition of alprenolol as internal standard, the compounds are extracted from plasma at alkaline pH into an organic phase and back-extracted into an acidic aqueous phase. Separation of the plasma components and metabolites was achieved on a reversed-phase column. Concentrations down to 66 nmol/l (20 ng/ml) can be determined with UV detection at 222 nm. This technique compares favourably with gas chromatographic and gas chromatographic-mass spectrometric methods.

Chromatography, Gas↗
PubMed1991

Determination of polysulphides in blood by gas chromatography and gas chromatography-mass spectrometry.

A sensitive and simple method to determine polysulphides in human blood, using an extractive alkylation technique and gas chromatography, has been devised. Polysulphides were alkylated with pentafluorobenzyl bromide, and then converted into bis(pentafluorobenzyl)disulphide by desulphuration with potassium cyanide. The disulphide was analysed qualitatively by mass fragmentography and quantitatively by gas chromatography with electron-capture detection. The lower limit of detection was 0.005 mumol/ml. Field testing in a suicide case confirmed the validity of the method.

Alkylation↗
PubMed1993

Determination of plasma levels of citalopram and its demethylated and deaminated metabolites by gas chromatography and gas chromatography-mass spectrometry.

Sensitive and specific methods based on gas chromatography (GC) and gas chromatography-mass spectrometry (GC-MS) for the determination of levels of citalopram, desmethylcitalopram and didesmethylcitalopram in the plasma of patients treated with citalopram are presented, as well as a GC-MS procedure for the assay of the citalopram propionic acid derivative. After addition of a separate internal standard for each drug, liquid-solvent extraction is used to separate the basic compounds from the acid compounds. The demethylated amines are derivatized with trifluoroacetic anhydride, and the acid metabolite with methyl iodide. GC-MS is performed in the electron impact mode, as mass spectrometry by the (positive-ion) chemical ionization mode (methane and ammonia) appeared to be unsuitable. The limits of quantification were 1 ng/ml for citalopram and desmethylcitalopram and 2 ng/ml for the other metabolites. The correlation coefficients for the calibration curves (range 10-500 ng/ml) were > or = 0.999 for all compounds, whether determined by GC or GC-MS.

Antidepressive Agents, Tricyclic↗
PubMed1996

Determination of cyanide and thiocyanate in blood by gas chromatography and gas chromatography-mass spectrometry.

We devised a sensitive and simple method for determining cyanide and its major metabolite, thiocyanate, in blood using an extractive alkylation technique. Pentafluorobenzyl bromide was used as the alkylating agent, and tetradecyldimethylbenzylammonium chloride was used as the phase-transfer catalyst. The derivatives obtained were analyzed qualitatively by gas chromatography-mass spectrometry and quantitatively by gas chromatography with an electron-capture detection. The detection limits of cyanide and thiocyanate were 0.01 and 0.003 mumol/ml, respectively, while the gross recovery of both compounds was 80%. The calibration curve was linear over the concentration range from 0.02 to 1.0 mumol/ml for cyanide and from 0.01 to 1.0 mumol/ml for thiocyanate. The accuracy and precision of the method were evaluated, and the coefficients of variation were found to be within 10%. Using the method, the blood levels of two victims who had died from cyanide poisoning were determined.

Chromatography, Gas↗
PubMed2004

Evaluation of fast gas chromatography and gas chromatography-mass spectrometry in the analysis of lipids.

Fast and conventional gas chromatography (GC) techniques were applied to nine different lipidic matrices (butter, lard, tallow, and peanut, corn, sunflower, soya, olive, menhaden oils). Simultaneous methylic transesterification was performed on all samples prior to GC analysis. Several practical aspects concerning high speed analysis were investigated, such as the great increase in linear velocity, the use of fast temperature ramps, column sample capacity and detection systems. Analytical results showed certain losses in resolution, balanced by a consistent reduction in analysis time. The actual time savings were variable (60-70 min) as they were dependent on the complexity of the sample while the speed enhancement factor was equal to 10.5. Peak identification was achieved by means of different information sources, such as fast GC-mass spectrometry (MS), linear retention indices and comprehensive two-dimensional (2D) gas chromatography group patterns. The method developed was shown to be applicable in routine applications on complex natural samples.

Chromatography, Gas↗
PubMed2004

Determination of thiodiglycol, a mustard gas hydrolysis product by gas chromatography-mass spectrometry after tert-butyldimethylsilylation.

A method for determining thiodiglycol (TDG), a mustard gas hydrolysis product in water, serum and urine samples using gas chromatography-mass spectrometry (GC-MS) after tert-butyldimethylsilylation (TBDMS) is described. Quantitation of TDG was performed by measuring the respective peak area on the extracted ion chromatogram of m/z 293, using an internal standard, the TDG homologue, thiodipropanol, peak area of which was measured as m/z 321. The presence of salts in the sample solution not only suppressed the loss of TDG by vaporization during the evaporation of water, but also facilitated the rate of production of di-silylated derivative, bis(tert-butyldimethylsilyoxylethyl)sulfide (TDG-(TBDMS)2). Under the pretreatment conditions used, in which 0.5 ml of water sample supplemented with 100 microM potassium chloride was evaporated to dryness under reduced pressure, followed by reaction with N-methyl-N-(tert-butyldimethylsilyl)trifluoroacetamide at 60 degrees C for 1 h, TDG-(TBDMS)2 was reproducibly detected with about a 55% recovery and a limit of detection (LOD, scan mode, S/N = 3) of 5.4 ng/ml. TDG was also determined by GC-MS from a 0.5 ml serum sample (after perchloric acid deproteinization) and from a 0.1 ml urine sample, after TBDMS derivatization. The LOD was determined to be 7.0 and 110 ng/ml for serum and urine, respectively.

Gas Chromatography-Mass Spectrometry↗
PubMed2006

Odour fingerprint acquisition by means of comprehensive two-dimensional gas chromatography-olfactometry and comprehensive two-dimensional gas chromatography/mass spectrometry.

The analysis of complex matrices, such as perfumes, by means of gas chromatography-olfactometry (GC-O) can be rather imprecise due to the co-elutions, leading to a possible masking of odour-active trace-level compounds by major interferences or agglomeration of olfactive impressions resulting in unreliable olfactive characterization. To overcome these limits an innovative technique, comprehensive two-dimensional gas chromatography-olfactometry (GC x GC-O), was applied, revealing several relevant co-elutions, as in the linalool and linalyl acetate zones. A total of 177 compounds, out of these 135 odour-active, were detected by GC-O, while about 481 out of 818 compounds presented odour-activity through GC x GC-O analyses. In addition, GC/mass spectrometry (GC/MS) and GC x GC/MS analyses were also performed. Peak assignment was achieved by means of different information sources, such as GC/MS, GC x GC/MS, LRI, injection of standards and olfactive impressions.

Chromatography, Gas↗
PubMed1976

Studies on monoterpene glucosides and related natural products. XXXI. Gas chromatography and gas chromatography-mass spectrometry of iridoid and secoiridoid glucosides.

A total of 33 iridoid and secoiridoid glucosides were detected by gas chromatography on several columns such as OV-1 or OV-17. Representative glucosides were then subjected to gas chromatography-mass spectrometry, giving some characteristic peaks that permitted the discrimination of both types of glucosides from other compounds in most instances. The successful detection of both types of glucosides in several plant extracts showed the applicability of this combination of methods to small amounts of plant materials.

Chromatography, Gas↗
PubMed1977

Gas chromatographic determination of sulphur compounds in town gas.

The gas chromatographic (GC) determination of the sulphur compounds in town gas (in the Nagoya area) was studied by using a flame-photometric detector (FPD) and the cold-trap method with liquid oxygen. The column packings used were 25% TCEP on Shimalite (AW, DMCS), 25% TCP on Shimalite (AW, DMCS), 10% PPE on Shimalite TPA, Porapak Q and silica gel. The major components identified were carbonyl sulphide, hydrogen sulphide, carbon disulphide, thiophene and tetrahydrothiophene (THT). The identities of thiophene and THT were also confirmed by GC combined with the use of a quadrupole mass spectrometer. The average concentrations and standard deviations of thiophene and THT were 8.8 +/- 1.8and 124 +/- 35 ng per 0.051, respectively. The latter value corresponds to 0.7 ppm, which is relatively high for the concentration of an odorant.

Carbon Disulfide↗
PubMed1978

Gas chromatographic and capillary column gas chromatographic--mass spectrometric determination of synthetic anabolic steroids. I. Methandienone and its metabolites.

The determination of methandienone (I) (17 alpha-methyl-17 beta-hydroxyandrosta-1,4-dien-3-one) in human urine by gas chromatography and capillary column gas chromatography--mass spectrometry has been studied. After oral administration to man two major metabolites were detected, the structures of which have been identified as 17-epi-methandienone (II) and 6 beta-hydroxy-17-epi-methandienone (III). These metabolites are exclusively excreted in the unconjugated form. At least two more metabolites are extractable from the free fraction of the urine but no measurable amounts of I itself were found. The rate of metabolism and urinary excretion seems to be reasonably fast. The total amount of recovered I in the form of the metabolites II and III is about 5%. Extraction and clean-up procedures and chromatographic details are presented.

Chromatography, Gas↗
PubMed2002

Analysis of endosulfan isomers and endosulfan sulfate in air and tomato leaves by gas chromatography with electron-capture detection and confirmation by gas chromatography-mass spectrometry.

Rapid analytical methods for the determination of endosulfan isomers and endosulfan-sulfate in air and plant samples were developed. The insecticides were trapped from air using a column containing Florisil and extracted with a low volume of ethyl acetate, assisted by sonication. Pesticide residues were determined by gas chromatography with electron-capture detection using a nonpolar capillary column. Residue identities were confirmed by gas chromatography coupled with mass spectrometry. Recoveries of these compounds from air samples were always higher than 78% with an RSD lower than 11% and the detection limits obtained were at least 0.3 ng/l air. Leaf samples were homogenised with ethyl acetate and extracts cleaned-up on an aluminium oxide column. Pesticides were eluted with a hexane-ethyl acetate (80:20, v/v) mixture. Recoveries obtained from plant samples were higher than 78% with an RSD lower than 14% and detection limits in leaves were 0.02 microg/g for each pesticide. These methods were applied to study the volatilisation of endosulfan from tomato leaves under laboratory conditions. A volatilisation rate near 1% of the initial amount of endosulfan per hour was obtained during the first 24 h at room temperature.

Air↗
PubMed1984

Gas chromatographic analysis of volatiles in fluid and gas inclusions.

Most geological samples and some synthetic materials contain fluid inclusions. These inclusions preserve for us tiny samples of the liquid and/or the gas phase that was present during formation, although in some cases they may have undergone significant changes from the original material. Studies of the current composition of the inclusions provide data on both the original composition and the change since trapping. These conclusions are seldom larger than 1 millimeter in diameter. The composition varies from a single major compound (e.g., water) in a single phase to a very complex mixture in one or more phases. The concentration of some of the compounds present may be at trace levels. We present here some analyses of inclusion on a variety of geological samples, including diamonds. We used a sample crusher and a gas chromatography-mass spectrometry (GC-MS) system to analyze for organic and inorganic volatiles present as major to trace constituents in inclusions. The crusher is a hardened stainless-steel piston cylinder apparatus with tungsten carbide crushing surfaces, and is operated in a pure helium atmosphere at a controlled temperature. Samples ranging from 1 mg to 1 g were crushed and the released volatiles were analyzed using multi-chromatographic columns and detectors, including the sensitive helium ionization detector. Identification of the GC peaks was carried out by GC-MS. This combination of procedures has been shown to provide geochemically useful information on the processes involved in the history of the samples analyzed.

Aluminum Oxide↗
PubMed2001

Application of a new analytical method using gas chromatography and gas chromatography-mass spectrometry for the azide ion to human blood and urine samples of an actual case.

We have established a practical and reliable method to identify and quantify the azide ion in human whole blood and human urine by transforming the ion into pentafluorobenzyl azide (PFBN3). PFBN3 was simply derived from a reaction of the ion with an excess amount of pentafluorobenzyl bromide (PFBBr). The excess amount of PFBBr was removed from the products by its reaction with sodium thiosulfate. PFBN3 in the sample was detected in high sensitivity by gas chromatography with nitrogen-phosphorus detector (GC-NPD) and gas chromatography-mass spectrometry (GC-MS). The lower detection limits of the ion by GC-NPD were 5 ng/ml for human whole blood sample and 0.5 ng/ml for human urine sample at S/N=3. On the other hand, they were 100 ng/ml for human whole blood sample and 10 ng/ml for human urine sample by the full-scan mode of GC-MS. The analytical method was applied to identification and quantification of the ion in the actual whole blood and urine samples of the victims in an actual criminal case.

Azides↗
PubMed1982

Analyses of nicotine and cotinine in tissues by capillary gas chromatography and gas chromatography-mass spectrometry.

Selective extraction and chromatographic techniques have been developed to measure low nanogram quantities of nicotine and cotinine in tissues. Analyses were performed by capillary column gas chromatography with a specific nitrogen-phosphorus detector and by gas chromatography-mass spectrometry. With close structural analogues for internal standards, high quantitative accuracy and precision were demonstrated for the range 5-1000 ng per g of tissue. The sensitivity limit was 2-3 ng/g for both compounds. The advantage of these techniques compared to previously published methods is increased selectivity; the other methods were developed for analysis of biological fluids and are not readily adaptable to more complex biological matrices such as tissue homogenates. With the newly developed techniques, we were able to perform a pharmacokinetic study of nicotine and cotinine in mouse liver following a single intraperitoneal injection of nicotine.

Animals↗
PubMed1979

Determination of therapeutic and toxic concentrations of doxepin and loxapine using gas-liquid chromatography with a nitrogen-sensitive detector, and gas chromatography-mass spectrometry of loxapine.

A gas-liquid chromatographic procedure is presented for the determination of therapeutic and toxic serum levels of doxepin and loxapine, using a nitrogen-phosphorus-sensitive detector. Amitriptyline is used as the internal standard. The method is accurate, sensitive and specific with no derivatization required prior to analysis. An advantage of the procedure is the small serum sample size needed for analysis and the selectivity and sensitivity of the detector, with the limit of detection being 3 and 2 microgram/l for doxepin and loxapine, respectively. Nine cases of doxenin and loxapine misuse are presented. Serum doxepin concentrations ranged from 113 to 439 microgram/l, with a loxapine concentration of 192 microgram/l observed in one patient. The presence of the tricyclics was identified and confirmed by gas chromatography-mass spectrometry and the mass spectrum of loxapine is reported.

Adult↗
PubMed1990

Determination of metrifonate and dichlorvos in whole blood using gas chromatography and gas chromatography-mass spectrometry.

Analytical methods for determining metrifonate and dichlorvos in whole blood and a sampling procedure suitable for pharmacokinetic studies in man are described. Metrifonate concentrations were determined after chloroform extraction using gas chromatography-nitrogen-phosphorus detection. The within-assay coefficients of variation were 4 and 9% at 19.4 and 0.8 mumol/l (limits of determination), respectively. Dichlorvos was determined using gas chromatography-mass spectrometry of toluene extracts. The within-assay coefficients of variation were 2 and 5% at 225 and 50 nmol/l (limits of determination), respectively. Since both substances are chemically unstable, the blood was collected by dripping it directly from the vein into 0.74 M phosphoric acid.

Chromatography, Gas↗
PubMed1981

Simultaneous determination of blood concentrations of methohexital and its hydroxy metabolite by gas chromatography and identification of 4'-hydroxymethohexital by combined gas--liquid chromatography--mass spectrometry.

A simple, sensitive and selective method is described for the simultaneous determination of low concentrations (less than 50 ng/ml) of underivatized methohexital and its hydroxy metabolite in small (0.1 ml) samples of human and rat plasma or whole blood by gas chromatography with nitrogen-selective detection. Moreover, the main metabolite in rat and man was identified as 4'-hydroxymethohexital by comparison of chromatograms from gas--liquid chromatography (GLC) with data obtained from GLC--mass spectrometry and 1H-nuclear magnetic resonance spectrometry of this metabolite, produced both by incubating methohexital with isolated rat liver microsomes and by isolating this metabolite from rat urine.

Animals↗