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1.
Molecules ; 23(12)2018 Dec 05.
Artículo en Inglés | MEDLINE | ID: mdl-30563162

RESUMEN

A rapid, reliable, and sensitive method was developed for the determination of ten tranquilizers in swine urine. Sample preparation was based on solid-phase extraction, which combined isolation of the compounds and sample cleanup in a single step. Separation was performed on a reversed phase C18 column by gradient elution with a chromatographic run time of seven minutes, consisting of 0.1% formic acid in water and acetonitrile as the mobile phase. Multiple reaction monitoring in positive mode was applied for data acquisition. Matrix-matched calibration was used for quantification and good linearity was obtained with coefficients of determination higher than 0.99. The average recoveries of fortified samples at concentrations between 0.05 and 10 µg/L ranged from 85% to 106% with interday relative standard deviations of less than 13% in all cases. The limits of detection and limits of quantification obtained for tranquilizers in the urine were in the ranges of 0.03⁻0.1 µg/L and 0.05⁻0.25 µg/L, respectively. The applicability of the proposed method was demonstrated by analyzing real samples; diazepam was detected at concentrations between 0.3 and 0.6 µg/L.


Asunto(s)
Tranquilizantes/química , Tranquilizantes/orina , Animales , Cromatografía Líquida de Alta Presión , Cromatografía Liquida , Extracción Líquido-Líquido , Reproducibilidad de los Resultados , Sensibilidad y Especificidad , Porcinos , Espectrometría de Masas en Tándem , Tranquilizantes/aislamiento & purificación
2.
Chudoku Kenkyu ; 24(1): 27-34, 2011 Mar.
Artículo en Japonés | MEDLINE | ID: mdl-21485120

RESUMEN

The immunoassay screening of benzodiazepines in urine is one of the most important methods of drug analysis in clinical and forensic laboratories. We experienced an unusual case of poisoning wherein the result of Triage DOA immunoassay screening was negative, although Depas (etizolam) was detected in the blood of the victim who had been suspected to prescribe Depas by gas chromatography-mass spectrometry. Depas has been widely used for the treatment of anxiety in Japan. Three immunoassay screening devices (AccuSign BZO, Monitect-3, and Fastect II) were evaluated for their specificity for etizolam, its 2 major metabolites M-III and M-VI, and other metabolites of benzodiazepines in urine. With AccuSign BZO, etizolam, M-III, and M-VI could be detected at concentrations of 1,000 ng/mL in urine; however, they could not be detected even at concentrations of 25,000 ng/mL with the other kits. In the case of etizolam poisoning, the result of AccuSign BZO was positive; however, Triage DOA, which is mainly used for the detection of drugs in urine at intensive care units (ICUs) or forensic laboratories, showed negative result for benzodiazepines. The concentrations of etizolam and its metabolites in urine were measured by the established high-performance liquid chromatographic method. The concentrations of M-III and M-V were 700 and 1,600 ng/mL, respectively. AccuSign BZO demonstrated higher specificity-than the other screening kits for the detection of etizolam and its metabolites in urine. Therefore, the types of drugs detected would be increased by combining Triage DOA with AccuSign BZO in ICUs or forensic laboratories.


Asunto(s)
Azepinas/orina , Diazepam/análogos & derivados , Inmunoensayo/métodos , Juego de Reactivos para Diagnóstico , Tranquilizantes/orina , Azepinas/envenenamiento , Cromatografía Líquida de Alta Presión , Diazepam/envenenamiento , Diazepam/orina , Humanos , Inmunoensayo/instrumentación , Espectrometría de Masas , Tranquilizantes/envenenamiento
3.
J Chromatogr B Biomed Sci Appl ; 734(1): 113-20, 1999 Oct 29.
Artículo en Inglés | MEDLINE | ID: mdl-10574196

RESUMEN

A method for analysis of veterinary tranquillizers in urine using gas chromatography-mass spectrometry (GC-MS) is described. Detection limits are 5 microg/l for ketamine, azaperone and the phenothiazines (chlor-, aceto- and propionylpromazine), 10 microg/l for haloperidol, 20 microg/l for xylazine and 50 microg/l for azaperol, recoveries for all analytes were higher than 70%. Method performance in terms of within-batch, between-days and between-analysts reproducibility was studied and found to be acceptable. Compliance with European Union criteria for confirmation of GC-MS "positive" results is evaluated and discussed.


Asunto(s)
Cromatografía de Gases y Espectrometría de Masas/métodos , Tranquilizantes/orina , Medicina Veterinaria , Animales , Azaperona/orina , Bovinos , Haloperidol/orina , Ketamina/orina , Fenotiazinas/orina , Piperazinas/orina , Piridinas/orina , Control de Calidad , Reproducibilidad de los Resultados , Sensibilidad y Especificidad , Ovinos/orina , Porcinos/orina , Xilazina/orina
5.
Ther Drug Monit ; 15(3): 224-35, 1993 Jun.
Artículo en Inglés | MEDLINE | ID: mdl-8333003

RESUMEN

This assay method allows a simultaneous determination of imipramine, desipramine, their 2-hydroxylated metabolites, and imipramine-N-oxide in 0.5 ml of plasma or 0.1 ml of urine within 35 min by an ion-paired, reversed phase (C18) high-performance liquid chromatography (HPLC) with electrochemical detection. The analytes are extracted from alkalinized plasma or urine with 5 ml of a 90/10 mixture (by vol) of diethyl either/2-propanol, back-extracted into 0.5 ml of 0.1 mol/L phosphoric acid. Urine samples are enzymatically treated with beta-glucuronidase/arylsulfatase before extraction. The electrochemical detection is performed with a glassy carbon electrode set at +0.85 V against the Ag/AgCl reference electrode. Recoveries for the analytes and the internal standard (propericiazine) from plasma or urine ranged from 66.4 to 105.7% with coefficients of variation (CVs) of < 6.8%. The intra- and interassay CVs for the analytes were < 17.4% in plasma and < 14.2% in urine. The limits of determination (a signal-to-noise ratio of 3) for imipramine, desipramine, 2-hydroxyimipramine, 2-hydroxydesipramine, and imipramine-N-oxide were 0.5, 0.3, 0.02, 0.02, and 1.0 microgram/L, respectively. Only four of the 23 psychotropic drugs, which might be coadministered with imipramine or desipramine, were considered to be the possible sources to interfere with the assay. We evaluated clinical applicability of this method by determining plasma concentration- and urinary excretion-time courses of the respective analytes in an extensive and a poor metabolizer of the debrisoquine/sparteine-type oxidation after a single oral dose of imipramine HCl (25 mg). The present method appears to be suitable not only for the therapeutic drug monitoring of imipramine and its active metabolites but also for studying the pharmacogenetically related metabolism of imipramine or desipramine.


Asunto(s)
Desipramina/sangre , Desipramina/orina , Imipramina/análogos & derivados , Imipramina/sangre , Imipramina/orina , Tranquilizantes/sangre , Tranquilizantes/orina , Arilsulfatasas/metabolismo , Calibración , Cromatografía Líquida de Alta Presión , Debrisoquina/metabolismo , Electroquímica , Glucuronidasa/metabolismo , Humanos , Hidroxilación , Masculino , Oxidación-Reducción , Fenotipo , Psicotrópicos/sangre , Sensibilidad y Especificidad , Esparteína/metabolismo , Factores de Tiempo
6.
Psychopharmacology (Berl) ; 97(3): 303-8, 1989.
Artículo en Inglés | MEDLINE | ID: mdl-2566185

RESUMEN

The pharmacokinetic properties of the iminodibenzyl antipsychotic drugs clocapramine (CCP, 3-chloro-5-[3-(4-carbamoyl-4-piperidino piperidino) propyl]-10, 11-dihydro-5H-dibenzo[b, f]azepine) and Y-516 (3-chloro-5-[3-(2-oxo-1, 2, 3, 5, 6, 7, 8, 8a-octahydroimidazo [1,2-a] pyridine-3-spiro-4'-piperidino) propyl]-10, 11-dihydro-5H-dibenzo[b, f]azepine) were investigated in dog and man. Dogs were administered CCP and Y-516 intravenously, intraperitoneally, and orally, and the concentrations of the parent drugs and their metabolites in the plasma and urine were determined. Half-life (t1/2) was approximately the same by all three administration routes, being approximately 5 h for CCP and 3 h for Y-516. Bioavailability following oral administration was 0.16 +/- 0.01 (mean +/- SD, n = 3) for CCP and 0.29 +/- 0.07 for Y-516. The fractions of dose absorbed following oral administration were 0.43 +/- 0.07 and 0.79 +/- 0.24, and the fractions of dose metabolized in the liver due to the first-pass effect were 0.63 +/- 0.05 and 0.63 +/- 0.04 for CCP and Y-516, respectively. Y-516 was detected in the plasma after intraperitoneal and oral administration of CCP. The ratio of the AUC of Y-516 to that of CCP was 0.06 following intraperitoneal administration and 0.40 following oral administration. This indicated that while the metabolism of CCP into Y-516 may occur partly in the liver due to the first-pass effect, it occurs mostly within the gastrointestinal tract itself or its mucosa.(ABSTRACT TRUNCATED AT 250 WORDS)


Asunto(s)
Antipsicóticos/farmacocinética , Benzazepinas/farmacocinética , Dibenzazepinas/farmacocinética , Tranquilizantes/farmacocinética , Administración Oral , Adulto , Animales , Antipsicóticos/orina , Benzazepinas/orina , Cromatografía Líquida de Alta Presión , Dibenzazepinas/orina , Perros , Humanos , Masculino , Especificidad de la Especie , Tranquilizantes/orina
8.
Cornell Vet ; 74(1): 38-49, 1984 Jan.
Artículo en Inglés | MEDLINE | ID: mdl-6705538

RESUMEN

The metabolism of propionylpromazine in the horse was studied. Although propionylpromazine is not currently approved or recommended for use in horses, it has been used illegally to alter their performance. Propionylpromazine hydrochloride was administered intramuscularly at clinical and subclinical doses. Three metabolites were detected in urine. The major metabolite was identified as 2-(1-hydroxypropyl) promazine sulfoxide. The detection of this metabolite in routine drug testing has been described.


Asunto(s)
Caballos/orina , Promazina/análogos & derivados , Tranquilizantes/orina , Animales , Cromatografía en Capa Delgada/métodos , Doping en los Deportes , Femenino , Cromatografía de Gases y Espectrometría de Masas/métodos , Caballos/metabolismo , Espectroscopía de Resonancia Magnética/métodos , Promazina/metabolismo , Promazina/orina , Espectrofotometría Ultravioleta/métodos , Tranquilizantes/metabolismo
9.
J Anal Toxicol ; 5(1): 14-9, 1981.
Artículo en Inglés | MEDLINE | ID: mdl-6783782

RESUMEN

An evaluation of Technology Resources Inc. (TRI) Amphetamine, Barbiturate, Narcotic (G) and Narcotic (S) "Dipsticks" for drugs of abuse in urine was made. The results obtained by six individuals reading the "Dipstick" papers was compared with the analysis of the same urine samples, by a combination of TLC, EMIT, RIA and GLC. The data obtained with "Dipstick" papers, regardless of the drug tested, were clearly unreliable (high percentage of false negatives, low percentage of true positives) and the assay was unsuitable as a technique for screening urines for drugs of abuse.


Asunto(s)
Drogas Ilícitas/orina , Indicadores y Reactivos , Preparaciones Farmacéuticas/orina , Tiras Reactivas , Anfetamina/orina , Animales , Barbitúricos/orina , Reacciones Falso Negativas , Reacciones Falso Positivas , Haplorrinos , Humanos , Tamizaje Masivo/instrumentación , Tamizaje Masivo/métodos , Narcóticos/orina , Tranquilizantes/orina
12.
Res Commun Chem Pathol Pharmacol ; 10(2): 227-38, 1975 Feb.
Artículo en Inglés | MEDLINE | ID: mdl-808840

RESUMEN

The metabolic disposition.of zolazepam, a pyrazolodiazepinone, was studied in male and female Spartan rats, Beagle dogs and Rhesus monkeys. Six principal urinary metabolites were characterized by gas chromatography and combined gas chromatography-mass spectrometry. The major metabolite in male and female rats was produced by N-demethylation and hydroxylation. In addition, female rats, but not the male demethylated zolazepam at the 1-position. Male and female dogs also demethylated zolazepam in the 1-position and hydroxylated in a position other than C-6, producing a metabolite peculiar to the dog. In marked contrast, the major metabolite in the monkey involved demethylation without subsequent hydroxylation.


Asunto(s)
Azepinas/metabolismo , Tranquilizantes/metabolismo , Animales , Azepinas/orina , Cromatografía de Gases , Perros , Femenino , Fluorobencenos/metabolismo , Fluorobencenos/orina , Haplorrinos , Macaca mulatta , Masculino , Espectrometría de Masas , Pirazoles/metabolismo , Pirazoles/orina , Ratas , Factores Sexuales , Especificidad de la Especie , Tranquilizantes/orina
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