Journal of chromatography.
Discontinued
Publisher:
Elsevier.
Frequency: Irregular
Country: Netherlands
Language: English
Start Year:1958 - 1994
ISSN:
Impact Factor
4.1
2022
| NLM ID: | 0427043 |
| (OCoLC): | 00987924 |
| (DNLM): | J16380000(s) |
| Coden: | JOCRAM |
| LCCN: | a 60003657 |
| Classification: | W1 JO5845 |
Investigation of the metabolism of azaperone in the horse. Urine samples collected from a horse after intramuscular administration of 40 mg of azaperone were extracted at pH 10 before and after acid hydrolysis. The extracts were concentrated and analysed by LC-MS-MS. Two N-dealkylated metabolites, N-despyridinylazaperol and N-despyridinylazaperone, and a low concentration of azaperone were detected in the unhydrolysed urine. Six metabolites; hydroxyazaperol, two hydroxyazaperones, azaperol, N-despyridinylazaperol and N-despyridinylazaperone were detected in the hydrolysed urine extracts. Using XAD-2 resin extraction, three glucuronide conjugated azape...
Determination of alclofenac in equine plasma and urine by high-performance liquid chromatography. A high-performance liquid chromatographic method to measure plasma and urinary alclofenac levels in equine biofluids is described. Isolation of the drug from plasma is achieved using liquid-liquid extraction with diethyl ether. Reversed-phase C18 solid phase extraction is used for the extraction of free and conjugated alclofenac from urine. The reproducibility and accuracy of the method were well within acceptable limits over the concentration ranges 0-10 and 0-20 micrograms/ml, respectively, for plasma and urine. Starting with 2 ml of plasma, a concentration of 0.1 microgram/ml could easily b...
Comparison of immunoaffinity chromatography combined with gas chromatography-negative ion chemical ionisation mass spectrometry and radioimmunoassay for screening dexamethasone in equine urine. A comparison of the sensitive analytical methods of radioimmunoassay (RIA) and immunoaffinity chromatography (IAC) combined with gas chromatography-negative ion chemical ionisation mass spectrometry for the specific and reliable screening of dexamethasone in equine post-race urine is presented. Results from analyses of samples collected from a mare during 144 hours post administration of 26 mg of dexamethasone sodium phosphate are described.
Rapid high-performance liquid chromatographic method for the determination of ketamine and its metabolite dehydronorketamine in equine serum. A simple, rapid and sensitive high-performance liquid chromatographic procedure has been developed for the determination of ketamine and dehydronorketamine in equine serum. Sample preparation consisted of mixing equal volumes of serum and acetonitrile-phosphoric acid (85%)-water (20:2:78, v/v/v), followed by ultrafiltration through a 10,000 molecular mass cut-off filter. Separation of these two analytes in the ultrafiltrate was accomplished on a reversed-phase phenyl column eluted with methanol-acetonitrile-phosphate buffer solution. Ketamine and dehydronorketamine were detected by a variable ...
Immunoaffinity chromatography combined with gas chromatography-negative ion chemical ionisation mass spectrometry for the confirmation of flumethasone abuse in the equine. Immunoaffinity chromatography using a synthesised immunosorbent was used to extract tritiated dexamethasone (with dexamethasone carrier) from equine urine at a recovery of 81.7 +/- 8.4% (mean +/- S.D.). A method utilising this procedure coupled to cool on-column injection gas chromatography-negative ion chemical ionisation mass spectrometry is also described for the confirmation of low levels of flumethasone in equine urine samples.
Identification of a benzhydrolic metabolite of ketoprofen in horses by gas chromatography-mass spectrometry and high-performance liquid chromatography. A benzhydrolic metabolite of ketoprofen, formed by reduction of the keto group of the drug, has been identified by gas chromatography-mass spectrometry in equine plasma and urine. After partial synthesis, its structure has been confirmed by UV, IR and 1H NMR spectroscopy. The kinetics of ketoprofen and this metabolite have been monitored in plasma by high-performance liquid chromatography. The two products were quantified in plasma up to 4 and 3 h, respectively, and were detected in urine up to 72 and 24 h, respectively, after a single intravenous administration to horses at the dose of 2.2 mg...
Detection of methandienone (methandrostenolone) and metabolites in horse urine by gas chromatography-mass spectrometry. The metabolic transformation of methandienone (I) in the horse was investigated. After administration of a commercial drug preparation to a female horse (0.5 mg/kg), urine samples were collected up to 96 h and processed without enzymic hydrolysis. Extraction was performed by a series of solid-liquid and liquid-liquid extractions, thus avoiding laborious purification techniques. For analysis by gas chromatography-mass spectrometry, the extracts were trimethylsilylated. Besides the parent compound I and its C-17 epimer II, three monohydroxylated metabolites were identified: 6 beta-hydroxymethand...
Thermospray liquid chromatography-mass spectrometry of corticosteroids. A high-performance liquid chromatographic method was developed for thermospray mass spectrometric analysis of steroidal hormones. Using a Nova-Pak C18 reversed-phase column and isocratic elution with a solvent comprised of 25 mM ammonium formate in 30% acetonitrile, corticosteroids were separated within 10 min. This solvent also permitted ultraviolet absorbance detection down to 220 nm with low-nanogram sensitivity. The use of acetonitrile was favourable for thermospray mass spectrometric analysis because mass spectra were obtained with a pseudomolecular ion as the base peak. A combination of ...
Identification of a tolfenamic acid metabolite in the horse by gas chromatography-mass spectrometry. A tolfenamic acid metabolite, a hydroxylated product, has been identified in equine plasma and urine samples using gas chromatography-mass spectrometry in the electron-impact and chemical-ionization modes. The method also allows the qualitative monitoring of the elimination of the drug and its metabolites from plasma. The two compounds are detected up to 48 and 24 h, respectively, after a single oral administration of a 30 mg/kg dose. The simultaneous detection of the two products increases the reliability of anti-doping control analysis.
Solid-phase extraction techniques for the determination of glycopyrrolate from equine urine by liquid chromatography-tandem mass spectrometry and gas chromatography-mass spectrometry. Glycopyrrolate (Robinul) is a quaternary ammonium salt which serves as a respiratory enhancing drug. It is reportedly used in horse racing to improve breathing. Extraction of glycopyrrolate from equine urine employing unique solid-phase extraction techniques gave a residue suitable for liquid chromatography-tandem mass spectrometry (LC-MS-MS) and gas chromatography-mass spectrometry (GC-MS). LC-MS-MS analysis employed an extract derived from 5 ml of urine subjected to cation-exchange chromatography. The daughter ion of m/z 318 monitored in the positive-ion mode was m/z 116. Recovery of glycopy...
Screening and confirmatory analysis of beta-agonists, beta-antagonists and their metabolites in horse urine by capillary gas chromatography-mass spectrometry. A method for the screening and confirmatory analysis of beta-agonists and -antagonists in equine urine is described. Following initial enzymic hydrolysis, the basic drugs and metabolites are extracted using Clean Screen DAU or Bond Elut Certify cartridges, and analysed as their trimethylsilyl ether or 2-(dimethyl) silamorpholine derivatives by capillary gas chromatography-mass spectrometry. The method proved to be very sensitive and selective for basic drugs. After administration of therapeutic doses of propranolol, metoprolol, timolol, isoxsuprine and clenbuterol to thoroughbred horses, the p...
Gas chromatographic mass-specific investigation of dextromoramide (Palfium) metabolism in the horse. Dextromoramide (Palfium) was given by intravenous injection to a Thoroughbred horse at a dosage of 20 mg and urine was collected 2, 4, 6 and 8 h after drug administration. Enzymatic hydrolysis of the urine followed by solvent extraction gave a residue which was back-extracted into 0.1 M sulphuric acid. After basification to pH 9 and solvent extraction, the resulting residue was submitted to gas chromatographic-mass spectrometric analysis. Both electron-impact and ammonia chemical-ionization mass spectra were recorded and, based on the observed fragmentation patterns, the principal metabolites ...
Rapid determination of methandrostenolone in equine urine by isotope dilution liquid chromatography-tandem mass spectrometry. Urine samples were spiked with [17-methyl-2H3]methandrostenolone as internal standard and extracted with a mixture of dichloromethane and cyclohexane. The organic phase was concentrated and injected onto a short octyl-silica column (30 mm x 4.6 mm I.D.) for separation of methandrostenolone and 17-epimethandrostenolone. The effluent from the column was connected to a Sciex TAGA 6000E triple quadrupole mass spectrometer equipped with an atmospheric pressure ion source for sampling of ions generated by a heated pneumatic nebulizer with corona discharge ionization. This ion source produced abundan...
Thin-layer chromatographic screening procedure for some drugs in horse plasma. A thin-layer chromatographic screening procedure for some basic, neutral and acidic drugs was developed using 3 ml of horse plasma. Chloroform-2-propanol (95:5, v/v) was used as the extraction solvent. The drugs were identified by a high-performance thin-layer chromatographic plate and spraying successively with some detection reagents. In this study, the extraction recovery rates and the detection limits were determined at the same time.
Determination of leucine enkephalin and methionine enkephalin in equine cerebrospinal fluid by microbore high-performance liquid chromatography and capillary zone electrophoresis coupled to tandem mass spectrometry. The performance of microbore high-performance liquid chromatography and capillary zone electrophoresis, both equipped with on-line tandem mass spectrometric detection capability, was evaluated critically for the determination of endogenous amounts of leucine enkephalin and methionine enkephalin in equine cerebrospinal fluid. Using an identical sample clean-up and enrichment procedure, capillary zone electrophoresis-mass spectrometry is limited in its concentration detection capacity owing to its much smaller injection volume. Leucine enkephalin was identified in post-mortem equine cerebrospina...
Screening of steroids in horse urine and plasma by using electron impact and chemical ionization gas chromatography-mass spectrometry. Gas chromatography with chemical ionization mass spectrometry and selected-ion monitoring provided a sensitive method for the screening and confirmation of steroids in horse urine and plasma. Chemical ionization mass spectrometry was more sensitive than the electron impact ionization mass spectrometry for most of the steroids except for testosterone, prednisone-metabolite-2 and prednisolone-metabolite-2. The chromatographic conditions used in this study provided clean separation of different natural and synthetic steroids. Approximately 75-85% of the steroids added to plasma and approximately ...
Comparison of the use of mass spectrometry and methylene unit values in the determination of the stereochemistry of estranediol, the major urinary metabolite of 19-nortestosterone in the horse. The stereochemistry of an isomer of 5-estrane-3,17 alpha-diol, the major metabolite of 19-nortestosterone in horse urine has been established by the use of methylene unit (MU) values. The empirical MU values of the bis-trimethylsilyl (TMS) derivatives of the eight available isomers of 5-androstane-3,17-diol and four isomers of 5-estrane-3,17 beta-diol were determined by capillary gas chromatography using three different columns. From this data the theoretical MU values for the bis-TMS derivatives of the four 5-estrane-3,17 alpha-diol isomers were predicted. Comparison of the experimentally det...
Screening and confirmation of drugs in horse urine by using a simple column extraction procedure. A simple and reproducible column (Clean Screen-DAU, copolymeric bonded-phase silica column) extraction procedure has been described for the screening and confirmation of drugs in horse urine. The recovery of drugs by the column extraction was better than or comparable to the recovery by the liquid-liquid extraction, which is commonly used in the equine analytical laboratories. The column extraction provided broad coverage of drugs, separated extracts into three fractions (acidic/neutral, steroids, basic), produced a cleaner extract, and eliminated the need for special liquid-liquid extraction ...
Metabolism and pharmacokinetic studies of propionylpromazine in horses. The propionylpromazine concentrations in plasma after intramuscular administration to horses were determined using gas chromatography with nitrogen-phosphorus detection. After hydrolysis by beta-glucuronidase/arylsulphatase, the parent drug and three metabolites were detected in urine. The metabolites were identified as 2-(1-hydroxypropyl)promazine, 2-(1-propenyl)promazine and 7-hydroxypropionylpromazine by gas chromatography-mass spectrometry. No N-demethylated or sulphoxidated metabolites of propionylpromazine were observed in the horse urine.
Determination of methandrostenolone and its metabolites in equine plasma and urine by coupled-column liquid chromatography with ultraviolet detection and confirmation by tandem mass spectrometry. Monitoring steroid use requires an understanding of the metabolism in the species in question and development of sensitive methods for screening of the steroid or its metabolites in urine. Qualitative information for confirmation of methandrostenolone and identification of its metabolites was primarily obtained by coupled-column high-performance liquid chromatography-tandem mass spectrometry. The steroids and a sulphuric acid conjugate were isolated and identified by their daughter ion mass spectra in the urine of both man and the horse following administration of methandrostenolone. Spontaneo...
Screening, confirmation and quantification of boldenone sulfate in equine urine after administration of boldenone undecylenate (Equipoise). Methods for screening by thin-layer chromatography, quantification by high-performance liquid chromatography with ultraviolet detection and confirmation by gas chromatography-mass spectrometry of boldenone sulfate in equine urine after administration of boldenone undecylenate (Equipoise) are presented. Sample work-up was done with C18 liquid-solid extraction followed by solvolytic cleavage of the sulfate ester. Confirmatory evidence of boldenone sulfate in equine urine was obtained from 2 h to 42 days following a therapeutic intramuscular dose of Equipoise. The use of 19-nortestosterone sulfat...
Purification of specific heterologous F(ab)2 fragments with DEAE-Zeta-Prep cartridges for ion-exchange chromatography. A simple two-step procedure for purifying F(ab)2 fragments of horse immunoglobulins is described. In the first step, the horse plasma is diluted, made up to 12% (w/v) with ammonium sulphate and digested with pepsin. In the second step, the previously dialyzed solution is chromatographed. Instead of a normal ion-exchange resin, a DEAE-cellulose, covalently linked to a synthetic vinyl polymer, was used (DEAE-Zeta-Prep). With this assembly it is possible to perform chromatography at a high flow-rate without the problems related to the use of large columns. The yield and purity of the final produc...
Isolation and quantitation of cadmium-, zinc- and copper-metallothioneins by high-performance liquid chromatography-atomic absorption spectrometry. Metallothioneins (MTs) were separated and quantitated by reversed-phase high-performance liquid chromatography (RP-HPLC), in direct combination with atomic absorption spectrometry (AAS) for quantitation of the metal contents in MTs. MTs were eluted from an RP-8 column with a gradient of Tris buffer pH 7.0 and methanol, and were detected by UV absorbance (220 nm). Commercially available purified MTs from horse kidney and rabbit liver were analyzed for purity and metal composition. One lot of horse kidney yielded only 50% of the estimated value. In some cases, the certified metal content differe...
Determination of clenbuterol and mabuterol in equine plasma by ion-pair liquid chromatography with electrochemical detection. Chromatographic and electrochemical characteristics. A method for the routine determination of the beta-adrenergic drugs clenbuterol and mabuterol in equine plasma has been developed. The drugs were isolated from alkalinized plasma by liquid-liquid extraction. The organic phase was evaporated to dryness and the residue was dissolved in the mobile phase prior to injection. The recoveries were 98% and 95% for clenbuterol and mabuterol, respectively. The drugs were separated by reversed-phase high-performance liquid chromatography and quantitated by a use of a coulometric detector set at +0.75 V vs. the internal reference electrode. The influence o...
Gas chromatographic analysis of flunixin in equine urine after extractive methylation. A quantitative method for the analysis of flunixin, 2-(2-methyl-3-trifluoromethylanilino) nicotinic acid, in equine urine by gas chromatography with nitrogen-phosphorus detection has been developed. Flunixin and the internal standard, mefenamic acid, N-(2,3-xylyl) anthranilic acid, were analysed after extractive methylation of the carboxylic acid group using methyl iodide. The extraction and alkylation conditions of flunixin and mefenamic acid have been studied. The detection limit of the method was 0.25 mumol/l flunixin in urine (74 ng/ml). Flunixin was found to be conjugated to 96.5% in equi...