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Screening and confirmation methods of the major urinary metabolite of finasteride–carboxy-finasteride by liquid chromatography–mass spectrometry and liquid chromatography–tandem mass spectrometry

作     者:Jianli Zhang 

作者机构:China Anti-Doping AgencyThe State Sport General AdministrationBeijing100029China 

出 版 物:《Acta Pharmaceutica Sinica B》 (药学学报(英文版))

年 卷 期:2012年第2卷第2期

页      面:220-226页

核心收录:

学科分类:1007[医学-药学(可授医学、理学学位)] 02[经济学] 0202[经济学-应用经济学] 

主  题:Metabolite of finasteride Carboxy-finasteride Urine Doping control LC–MS LC–MS/MS 

摘      要:Screening and confirmation methods of the major urinary metabolite of finasteride–carboxy-finasteride for doping control purpose were developed.Liquid–liquid extraction was adopted for the sample preparation.Analytes were detected by positive electrospray ionization in single quadrupole and triple quadrupole mass spectrometer.In the screening method,selected ion monitoring(SIM)mode was used to monitor m/z 403 for carboxy-finasteride.In the confirmation method,product ion mode was used to monitor the precursor ion m/z 403.The limit of detection was below 2 ng/mL for the screening method.Good linearity was obtained in the range 10.0–500.0 ng/mL.The intra-run and inter-run precision calculated from quality control(QC)samples was less than 5.3%.The accuracy as determined from QC samples was within ±6.6%.The screening method was applied for the analysis of excretion samples,allowing the detection of carboxy-finasteride for up to 49 h in urine specimen collected after an oral administration of 5 mg of finasteride.

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