Screening for basic drugs in equine urine using direct-injection differential-gradient LC–LC coupled to hybrid tandem MS/MS

Stanley, Shawn M.R.; Foo, Hsiao Ching

doi:10.1016/j.jchromb.2006.03.034

Cited by 41 publications

(41 citation statements)

References 20 publications

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“…The determination of the abuse of several drugs and illicit substances is frequently performed in urine since large volumes of sample is available, and its collection is easy and non-invasive [1][2][3]. In addition, urine testing provides a relatively long detection window for drugs.…”

Section: Introductionmentioning

confidence: 99%

High-Throughput Screening of Drugs of Abuse in Urine by Supported Liquid–Liquid Extraction and UHPLC Coupled to Tandem MS

Maquille

Guillarme

Rudaz

et al. 2009

Chroma

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A qualitative method, involving supported liquid-liquid extraction (SLE) and ultra high pressure liquid chromatography coupled to tandem mass spectrometry (UHPLC-MS-MS), was developed for the rapid tentative identification of various drugs of abuse in urine. In this study, 28 drugs and metabolites were covered by the screening procedure. Before analysis, urine samples were extracted by SLE and good extraction recoveries were obtained for most investigated compounds. The UHPLC strategy was then selected for the rapid separation of amphetamines, cocaine, opiates and related compounds in urine. Using columns packed with sub-2 lm particles, analysis time was reduced down to 2 min, while maintaining acceptable performance. Finally, the detection was by tandem MS operating in the single reaction monitoring (SRM) mode. The most intense transition was selected for the different drugs and SRM dwell times set at 5 ms, to maintain sufficient data points across the narrow UHPLC peaks. The tentative identification of the drugs of interest, including amphetamines, opiates and cocaine, was based on both, retention times and mass spectrometry information. With the proposed method, limits of detection were estimated at about 1 ng mL -1 and the applicability was assessed by successfully analyzing several samples of drug abusers. Finally, this study demonstrates the potential of UHPLC coupled to tandem MS for the rapid screening of drugs of abuse in urine.

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Section: Introductionmentioning

confidence: 99%

High-Throughput Screening of Drugs of Abuse in Urine by Supported Liquid–Liquid Extraction and UHPLC Coupled to Tandem MS

Maquille

Guillarme

Rudaz

et al. 2009

Chroma

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“…Recently, hydrophilic interaction chromatography (HILIC) has become the technique preferred for the analysis of polar and ionizable compounds, [114][115][116] as occurred in the detection of myo-inositol trispyrophosphate (ITPP) in equine urine and plasma which is a new drug, capable of increasing the amount of oxygen in hypoxic tissues and is an ideal candidate as doping agent in racehorses. [117,118] LC-MS instruments equipped with mass analyzers with MS/MS capabilities, such as triple quadrupole (QqQ) [104][105][106]108] and triple quadrupole/linear ion trap (QTrap), [101,106,110,112,119] have been implemented successfully in common screening methods in equine doping control. These LC-MS/MS systems provide analyses with high sensitivity and specificity which are critical prerequisites for the detection of banned compounds in trace concentration levels in complex biological samples.…”

Section: Mass Spectrometric Techniques In the Equine Doping Controlmentioning

confidence: 99%

“…A sensitive EPI scan function is triggered when a MRM survey scan signal exceed the defined independent data acquisition criteria. [119] • Thirty-two negatively ionizable acidic dugs in plasma and 11 positively ionizable neutral drugs in urine by using two SPE columns. A sensitive EPI scan function is activated when an MRM survey scan signal exceeds the defined information dependent acquisition (with dynamic background substraction) criteria.…”

Section: Mass Spectrometric Techniques In the Equine Doping Controlmentioning

confidence: 99%

Challenges in detecting substances for equine anti‐doping

Fragkaki

Kioukia‐Fougia

Kiousi

et al. 2017

Drug Testing and Analysis

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The artificial increase of the physical capability of horses using drugs is well known in racing and other equine sports. Both illicit and therapeutic substances are regarded as prohibited substances in competition in most countries. Some countries make distinctions for a few, specific drugs which are, however, allowed for use in other countries. The primary objective in the case of doping control is the detection of any trace of drug exposure, either parent drug or any of its metabolites, using the most powerful analytical methods which are generally based on chromatographic/mass spectrometric techniques. Of major concern in horseracing is the absence of a single organization regulating the anti-doping framework; instead of this, individual racing authorities provide rules and regulations often resulting in variations in the applied doping control programmes of different countries. The aim of this paper is to review the recent literature (approximately from 2012 to mid-2016) to highlight the numerous and diverse challenges faced in doping control of racing and equestrian sports, including the detection of designer drugs (anabolic steroids or stimulants) and of other emerging prohibited substances, such as peptides and noble gases in horse urine and plasma. Moreover, the application of 'omics' techniques (especially of metabolomics) deserves attention for establishing possible fingerprints of drug abuse as well as the evolution of instrumental analysis resulting a powerful ally in the fight against doping in equine sports.

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“…Numerous protocols for CDDZ determination considering different purposes and techniques have been reported: forensic (Miyaguchi et al, 2006), pharmaceutical (Ellaithy et al, 2001;Suzuki et al, 2004), environmental (El-Baqary et al, 2007), drug monitoring and pharmacological (Otsubo et al, 1995;Inoue et al, 2000;Aresta et al, 2002;Laloup et al, 2005;Stanley and Foo, 2006). However, these articles present limited throughput and restrict sensitivity.…”

Section: Introductionmentioning

confidence: 99%

Quantification of chlordesmethyldiazepam by liquid chromatography–tandem mass spectrometry: application to a cloxazolam bioequivalence study

Oliveira‐Silva

Oliveira

Mendes

et al. 2009

Biomedical Chromatography

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A rapid, sensitive and specific LC-MS/MS method was developed and validated for quantifying chlordesmethyldiazepam (CDDZ or delorazepam), the active metabolite of cloxazolam, in human plasma. In the analytical assay, bromazepam (internal standard) and CDDZ were extracted using a liquid-liquid extraction (diethyl-ether/hexane, 80/20, v/v) procedure. The LC-MS/MS method on a RP-C18 column had an overall run time of 5.0 min and was linear (1/x weighted) over the range 0.5-50 ng/mL (R > 0.999). The between-run precision was 8.0% (1.5 ng/mL), 7.6% (9 ng/mL), 7.4% (40 ng/mL), and 10.9% at the low limit of quantification-LLOQ (0.500 ng/mL). The between-run accuracies were 0.1, -1.5, -2.7 and 8.7% for the above mentioned concentrations, respectively. All current bioanalytical method validation requirements (FDA and ANVISA) were achieved and it was applied to the bioequivalence study (Cloxazolam -- test, Eurofarma Lab. Ltda and Olcadil -- reference, Novartis Biociências S/A). The relative bioavailability between both formulations was assessed by calculating individual test/reference ratios for Cmax, AUClast and AUC0-inf. The pharmacokinetic profiles indicated bioequivalence since all ratios were as proposed by FDA and ANVISA.

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Screening for basic drugs in equine urine using direct-injection differential-gradient LC–LC coupled to hybrid tandem MS/MS

Cited by 41 publications

References 20 publications

High-Throughput Screening of Drugs of Abuse in Urine by Supported Liquid–Liquid Extraction and UHPLC Coupled to Tandem MS

High-Throughput Screening of Drugs of Abuse in Urine by Supported Liquid–Liquid Extraction and UHPLC Coupled to Tandem MS

Challenges in detecting substances for equine anti‐doping

Quantification of chlordesmethyldiazepam by liquid chromatography–tandem mass spectrometry: application to a cloxazolam bioequivalence study

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