Gas chromatographic–mass spectrometric analysis of veterinary tranquillizers in urine: evaluation of method performance

Olmos-Carmona, Marı́a-Luisa; Hernández-Carrasquilla, M

doi:10.1016/s0378-4347(99)00334-5

Cited by 43 publications

(29 citation statements)

References 6 publications

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“…This committee prepared a list of drugs that could be, or have been, used in drug-facilitated sexual assault. During the last few years, KET has been shown as a drug of quickly increasing popularity in bars, disco-dancing, and rave parties (12)(13)(14)(15)(16) and has been added to the list of socalled "club drugs" and drugs associated with sexual assault. Moore et al (12) Figure 3.…”

Section: Discussionmentioning

confidence: 99%

“…In their study, EI-GC-MS provided much better LOQs for KET and NKET (13 and 9 ng/mL, respectively) than PCI-GC-MS. In another paper by Olmos-Carona et al (16), the LOD for KET in urine was 5 ng/mL. The increasing abuse of KET during the last few years has led many urine drug testing laboratories to consider adding KET screening to their programs (12,15).…”

Section: Discussionmentioning

confidence: 99%

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Detection of Ketamine and Norketamine in Urine of Nonhuman Primates after a Single Dose of Ketamine using Microplate Enzyme-Linked Immunosorbent Assay (ELISA) and NCI-GC-MS

Negrusz

Adamowicz

Saini

et al. 2005

Journal of Analytical Toxicology

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The general anesthetic ketamine (Ketalar | Ketaject, Vetalar) (KET) is used in human and veterinary medicine for induction of anesthesia for short surgical procedures and routine veterinary examination. Its illicit use by teenagers in rave parties has been reported, and it has recently been identified as a substance associated with sexual assault. One aim of this paper was to study the elimination of KET and its major metabolite norketamine (NKET) in urine collected from five nonhuman primates that received a single dose (5 mg/kg, I.M.) of KET and to study elimination patterns to determine how long after drug administration KET and NKET can be detected. Another aim of this study was to develop and validate a highly sensitive negative ion chemical ionization-gas chromatography-mass spectrometry (NCI-GC-MS) method for the simultaneous quantitation of KET and its major metabolite NKET in urine and to analyze urine samples collected from the animals. The last aim of this study was to apply and evaluate a newly developed ELISA screening methodology for detection of KET and its metabolites in the same urine samples collected from primates which received a single dose of KET. In two monkeys, KET was detected in urine up to 3 days after drug administration (32-7070 ng/mL); in one monkey, it was detected up to 4 days (65-13,500 ng/mL); in one monkey, it was detected only on days 1 and 2 (4000 and 70 ng/mL, respectively); and in one monkey, it was detected 10 days after KET injection (22-35,000 ng/mL). NKET concentrations ranged from 63 pg/mL to 1.75 pg/mL, and it remained in the urine throughout the entire 35-day study period in 4 out of 5 animals. In one monkey, NKET was detected up to 31 days after KET administration. Urine analysis using ELISA revealed that KET and NKET can be easily detectable at 25 ng/mL. In one monkey, KET and its metabolites were detected in urine up to 4 days after drug administration, up to 7 days in two monkeys, up to 11 days in one monkey, and 16 days after KET injection in one monkey. Urine extraction followed by screening using ELISA methodology allowed for significant extension of the detection period in all animals from the study. It is believed that the KET elimination in urine of nonhuman primates is slightly faster than in humans. We propose that NCI-GC-MS be employed to detect NKET as a target compound in urine in toxicological investigations of drug-facilitated sexual assault when KET use by the perpetrator is suspected.

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Section: Discussionmentioning

confidence: 99%

Section: Discussionmentioning

confidence: 99%

Detection of Ketamine and Norketamine in Urine of Nonhuman Primates after a Single Dose of Ketamine using Microplate Enzyme-Linked Immunosorbent Assay (ELISA) and NCI-GC-MS

Negrusz

Adamowicz

Saini

et al. 2005

Journal of Analytical Toxicology

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“…Olmos-Carmona and Hernández-Carrasquilla isolated seven tranquilisers from urine using C18 SPE cleanup [388]. Samples required dilution in TEA to minimise residual silanol effects.…”

Section: Sedativesmentioning

confidence: 99%

Current trends in sample preparation for growth promoter and veterinary drug residue analysis

Kinsella

O’Mahony

Malone

et al. 2009

Journal of Chromatography A

180

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A comprehensive review is presented on the current trends in sample preparation for isolation of veterinary drugs and growth promotors from foods. The objective of the review is to firstly give an overview of the sample preparation techniques that are applied in field. The review will focus on new techniques and technologies, which improve efficiency and coverage of residues. The underlying theme to the paper is the developments that have been made in multi-residue methods and particularly multi-class methods for residues of licensed animal health products, which have been developed in the last couple of years. The role of multi-class methods is discussed and how they can be accommodated in future residue surveillance.

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“…1. The determination of phenothiazines in urine has been carried out by conventional fluorescence [4,5], immunoassay [6], photometry [7], GC [8], or LC-MS [9].…”

Section: Introductionmentioning

confidence: 99%

“…Extraction methods based on SPE have proved to be a valuable alternative to liquid-liquid extraction (LLE) procedures because they are less laborious and time-consuming, reducing the total amount of organic solvents and the manipulation of the extracts. There are some SPE methods reported to extract phenothiazines from biological fluids, using C18 SPE cartridges, for application in GC-MS [8], and recently using an Oasis  (Waters, Milford, MA, USA) cartridge, for application in HPLC-UV-Vis [44], a sorbent scarcely used in the literature, despite the promising results published [45]. In our case we have developed a new SPE procedure to extract the phenothiazines from the urine samples, compatible with the applied FASI methodology.…”

Section: Introductionmentioning

confidence: 99%

Development and validation of a capillary electrophoresis method for the determination of phenothiazines in human urine in the low nanogramper milliliter concentration range using field-amplified sample injection

et al. 2005

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A capillary zone electrophoresis (CZE) method with ultraviolet-visible detection has been established and validated for the determination of five phenothiazines: thiazinamium methylsulfate, promazine hydrochloride, chlorpromazine hydrochloride, thioridazine hydrochloride, and promethazine hydrochloride in human urine. Optimum separation was obtained on a 64.5 cm x 75 microm bubble cell capillary using a buffer containing 150 mM tris(hydroxymethyl)aminomethane and 25% acetonitrile at pH 8.2, with temperature and voltage of 25 degrees C and 20 kV, respectively. Naphazoline hydrochloride was used as an internal standard. Field-amplified sample injection (FASI) has been applied to improve the sensitivity of the detection. Considering the influence of parameters affecting the on-line preconcentration (nature of preinjection plug, sample solvent composition, injection times, and injection voltage) and due to the significant interactions among them, in this paper we propose for the first time the application of a multivariate approach to carry out the study. The optimized conditions were as follows: preinjection plug of water for 7 s at 50 mbar, electrokinetic injection for 40 s at 6.2 kV, and 32 microm of H3PO4 in the sample solvent. Also, a solid-phase extraction (SPE) procedure is developed to obtain low detection limits and an adequate selectivity for urine samples. The combination of SPE and FASI-CZE-UV allows adequate linearities and recoveries, low detection limits (from 2 to 5 ng/mL), and satisfactory precisions (3.0-7.2% for an intermediate RSD %).

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Gas chromatographic–mass spectrometric analysis of veterinary tranquillizers in urine: evaluation of method performance

Cited by 43 publications

References 6 publications

Detection of Ketamine and Norketamine in Urine of Nonhuman Primates after a Single Dose of Ketamine using Microplate Enzyme-Linked Immunosorbent Assay (ELISA) and NCI-GC-MS

Detection of Ketamine and Norketamine in Urine of Nonhuman Primates after a Single Dose of Ketamine using Microplate Enzyme-Linked Immunosorbent Assay (ELISA) and NCI-GC-MS

Current trends in sample preparation for growth promoter and veterinary drug residue analysis

Development and validation of a capillary electrophoresis method for the determination of phenothiazines in human urine in the low nanogramper milliliter concentration range using field-amplified sample injection

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