Kim, Yongseok Jeon, Mijin Min, Hophil Son, Junghyun Lee, Jaeick Kwon, Oh-Seung Moon, Myeong Hee Kim, Ki Hun 2024-01-19T22:33:42Z 2024-01-19T22:33:42Z 2021-09-03 2018-06 0951-4198 https://pubs.kist.re.kr/handle/201004/121335 RationaleIn addition to the development of adequate screening methods for multiple compounds, the World Anti-Doping Agency (WADA) requires anti-doping laboratories to analyze prohibited substances and their metabolites from various classes. This task presents a difficult challenge for all agencies and interests involved in the field of doping control. MethodsA screening method is reported in which hybrid sample preparation was performed using a combination of weak cation-exchange solid-phase extraction (WCX-SPE) and the Dilute and Shoot' strategy in order to take advantage of both the methodologies. Target substances were extracted using a WCX cartridge and reconstituted with a diluted sample aliquot that included 20% of an untreated urine sample. The target substances were further analyzed by high-performance liquid chromatography/triple quadrupole mass spectrometry (LC/MS). ResultsThe SPE procedure was optimized using a cartridge-washing step, elution conditions, and elution volume. The cartridge-washing step, which was performed using 10% methanol, improved the overall recovery of target substances. Since the recovery was observed to vary according to the pH of the eluting solution, we applied an elution step using both an acid and a basic organic solvent to achieve complementary recovery. Reconstitution of the diluted aliquot sample was performed to recover the polar substances. ConclusionsThe method was validated and applied to real samples in accordance with the external quality assessment scheme of WADA and to the previously reported samples that had provided positive test results. This novel method using hybrid sample preparation and LC/MS could be useful to screen multiple classes of the 264 targeted substances in anti-doping analysis. English WILEY Development of a multi-functional concurrent assay using weak cation-exchange solid-phase extraction (WCX-SPE) and reconstitution with a diluted sample aliquot for anti-doping analysis Article 10.1002/rcm.8119 1 RAPID COMMUNICATIONS IN MASS SPECTROMETRY, v.32, no.11, pp.897 - 905 RAPID COMMUNICATIONS IN MASS SPECTROMETRY 32 11 897 905 N scie scopus 000432226100008 2-s2.0-85047505172 Biochemical Research Methods Chemistry, Analytical Spectroscopy Biochemistry & Molecular Biology Chemistry Spectroscopy Article CHROMATOGRAPHY/TANDEM MASS-SPECTROMETRY MOLECULARLY IMPRINTED POLYMERS ENVIRONMENTAL WATER SAMPLES HORMONE-RELEASING PEPTIDES HUMAN URINE LC-MS/MS ETHYL GLUCURONIDE DRUGS TIME METABOLITES antidoping anlysis Mass spectrometry solid phase extraction liquid chromatography