Screening of over 100 drugs in horse urine using automated on-line solid-phase extraction coupled to liquid chromatography-high resolution mass spectrometry for doping control

Kwok, Wai‐Him; Choi, Timmy L.S.; Tsoi, Yeuki Y.K.; Leung, Gary N. W.; Wan, Terence S.M.

doi:10.1016/j.chroma.2017.02.020

Cited by 21 publications

(13 citation statements)

References 30 publications

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“…Apart from the simple water samples, the practical online SPE‐UHPLC technique was also used for the analysis of biological samples, such as milk , urine , plasma , serum , cattle manure‐based biogas , and cells . Recently, an online SPE‐UHPLC method was reported to analyze dried blood spot and the selective, accurate, and precise responses of the target compounds generally meeting the accepted regulated bioanalysis guidelines were observed over the range of 5–1000 ng/mL in whole blood .…”

Section: Online Sample Preparation‐uhplc Techniquesmentioning

confidence: 99%

Recent advances of online coupling of sample preparation techniques with ultra high performance liquid chromatography and supercritical fluid chromatography

Liang

Zhou

2018

J of Separation Science

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Ultra high performance liquid chromatography and supercritical fluid chromatography techniques are favored because of their high efficiency and fast analysis speed. Although many sample preparation techniques have been coupled with common liquid chromatography online, the online coupling of sample preparation with the two popular chromatography techniques have gained increasing attention owing to the increasing requirements of efficiency and sensitivity. In this review, we have discussed and summarized the recent advances of the online coupling of sample preparation with ultra high performance liquid chromatography and supercritical fluid chromatography techniques. The main sample preparation techniques that have been coupled with ultra high performance liquid chromatography online are solid-phase extraction and in-tube solid-phase microextraction, while solid-phase extraction and supercritical fluid extraction are the main techniques that have been coupled with supercritical fluid chromatography online. Especially, the strategies for online coupling of sample preparation with chromatography techniques were summarized. Typical applications and growing trends of the online coupling techniques were also discussed in detail. With the increasing demands of improving the efficiency, throughput, and analytical capability toward complex samples of the analysis methods, online coupling of sample preparation with chromatography techniques will acquire further development.

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Section: Online Sample Preparation‐uhplc Techniquesmentioning

confidence: 99%

Recent advances of online coupling of sample preparation techniques with ultra high performance liquid chromatography and supercritical fluid chromatography

Liang

Zhou

2018

J of Separation Science

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“…With the aim to develop quick methods incorporating as many drug targets as possible to analyse up to 154 horse urine samples for pre‐race testing in Hong Kong, a new method has been developed using solid‐supported liquid extraction (SLE) in preference to the more traditional liquid–liquid extraction (LLE) 3–5 or solid‐phase extraction (SPE) 6–9 . In recent times, quick sample preparation techniques have been used to develop wide‐scope drug screening methods, including (a) online SPE 10–12 and (b) dilute‐and‐shoot 13–19 . In Hong Kong, pre‐race test results must be reported at least 30 min before the relevant horses are scheduled to race.…”

Section: Introductionmentioning

confidence: 99%

A high‐throughput and broad‐spectrum screening method for analysing over 120 drugs in horse urine using liquid chromatography–high‐resolution mass spectrometry

Wong

Chan

Choi

et al. 2020

Drug Testing and Analysis

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A high‐throughput method has been developed for the doping control analysis of 124 drug targets, processing up to 154 horse urine samples in as short as 4.5 h, from the time the samples arrive at the laboratory to the reporting deadline of 30 min before the first race, including sample receipt and registration, preparation and instrument analysis and data vetting time. Sample preparation involves a brief enzyme hydrolysis step (30 min) to detect both free and glucuronide‐conjugated drug targets. This is followed by extraction using solid‐supported liquid extraction (SLE) and analysis using liquid chromatography–high‐resolution mass spectrometry (LC–HRMS). The entire set‐up comprised of four sets of Biotage Extrahera automation systems for conducting SLE and five to six sets of Orbitrap for instrumental screening using LC–HRMS. Suspicious samples flagged were subject to confirmatory analyses using liquid chromatography–triple quadrupole mass spectrometry. The method comprises 124 drug targets from a spectrum of 41 drug classes covering acidic, basic and neutral drugs. More than 85% of the targets had limits of detection at or below 5 ng/mL in horse urine, with the lowest at 0.02 ng/mL. The method was validated for qualitative identification, including specificity, sensitivity, extraction recovery and precision. Method applicability was demonstrated by the successful detection of different drugs, namely (a) butorphanol, (b) dexamethasone, (c) diclofenac, (d) flunixin and (e) phenylbutazone, in post‐race or out‐of‐competition urine samples collected from racehorses. This method was developed for pre‐race urine testing in Hong Kong; however, it is also suitable for testing post‐race or out‐of‐competition urine samples, especially when a quick total analysis time is desired.

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“…Mass spectrometry‐based methods are the most powerful tools in modern analytical toxicology. When coupled with a very robust chromatography setup and an optimized sample preparation procedure, hundreds of substances can be monitored in a single analytical run . Different types of mass analyzers which can acquire a huge quantity of data in a short time are available.…”

Section: Introductionmentioning

confidence: 99%

“…Different types of mass analyzers which can acquire a huge quantity of data in a short time are available. High‐resolution mass spectrometry approaches have become prominent . The number of analytical targets allowed per method is dependent on the comprehensive sample preparation strategy, chromatographic separation, and fine tuning of the instrumentation.…”

Section: Introductionmentioning

confidence: 99%

Comprehensive analysis by liquid chromatography Q‐Orbitrap mass spectrometry: Fast screening of peptides and organic molecules

et al. 2018

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The number of substances nominally listed in the prohibited list of the World Anti-Doping Agency increases each year. Moreover, many of these substances do not have a single analytical target and must be monitored through different metabolites, artifacts, degradation products, or biomarkers. A new analytical method was developed and validated for the simultaneous analysis of peptides and organic molecules using a single sample preparation and LC-Q-HRMS detection. The simultaneous analysis of 450 target molecules was performed after cleanup on a mixed-mode solid-phase extraction cartridge, combined with untreated urine. The cleanup solvent and reconstitution solvent were the most important parameters for achieving a comprehensive sample preparation approach. A fast chromatographic run based on a multistep gradient was optimized under different flows; the detection of all substances without isomeric coelution was achieved in 11 minutes, and the chromatographic resolution was considered a critical parameter, even in high-resolution mass spectrometry detection. The mass spectrometer was set to operate by switching between positive and negative ionization mode for FULL-MS, all-ion fragmentation, and FULL-MS/MS . The suitable parameters for the curved linear trap (c-trap) conditions were determined and found to be the most important factors for the development of the method. Only FULL-MS/MS enables the detection of steroids and peptides at concentrations lower than the minimum required performance levels set by World Anti-Doping Agency (1 ng mL ). The combination of the maximum injection time of the ions into the c-trap, multiplexing experiments, and loop count under optimized conditions enabled the method to be applied to over 10 000 samples in only 2 months during the 2016 Rio Summer Olympic and Paralympic Games. The procedure details all aspects, from sample preparation to mass spectrometry detection. FULL-MS data acquisition is performed in positive and negative ion mode simultaneously and can be applied to untargeted approaches.

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Screening of over 100 drugs in horse urine using automated on-line solid-phase extraction coupled to liquid chromatography-high resolution mass spectrometry for doping control

Cited by 21 publications

References 30 publications

Recent advances of online coupling of sample preparation techniques with ultra high performance liquid chromatography and supercritical fluid chromatography

Recent advances of online coupling of sample preparation techniques with ultra high performance liquid chromatography and supercritical fluid chromatography

A high‐throughput and broad‐spectrum screening method for analysing over 120 drugs in horse urine using liquid chromatography–high‐resolution mass spectrometry

Comprehensive analysis by liquid chromatography Q‐Orbitrap mass spectrometry: Fast screening of peptides and organic molecules

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