title: Determination of raloxifene in urine by liquid chromatography-tandem mass spectrometry for doping.
abstract: Raloxifene is one of the selective estrogen receptor modulators and is often used to prevent and treat osteoporosis in postmenopausal women. Because of the indirect impact on serum testosterone levels and the potential ability for performance enhancement, it is banned by the World Anti-Doping Agency (WADA). This study established a fast, sensitive and selective liquid chromatography-tandem mass spectrometry method to quantify total raloxifene (unchanged and glucuronidated) in human urine for doping analysis. Urines from six healthy volunteers were collected 240 h after taking a single dose of raloxifene. The concentrations of urinary raloxifene were analyzed by the established method after sample preparation, including hydrolysis with β-glucuronidase. The lowest limit of quantification was 0.5 ng/mL. Linearity was observed for raloxifene concentrations ranging from 0.5 to 100 ng/mL, with a correlation coefficient of 0.999. The recoveries were >92.81%. Inaccuracies were below ±5%, and precisions varied from 2.18 to 5.37%. The results showed that urinary raloxifene was immediately detectable within 4 h after the administration of only a single dose of raloxifene. Such a result indicates a violation of the WADA rules. Furthermore, ingesting raloxifene would be detectable after 6 days in the urine of males or >10 days in the urine of female.
authors.affiliation: Graduate Institute of Athletics and Coaching Sciences, National Taiwan Sport University, No. 250, Wen-Hua 1st Road, Kweishan, Taoyuan County 33301, Taiwan.
authors.forename: Ting-Ting
authors.initials: TT
authors.lastname: Chen
authors.forename: Tai-Yuan
authors.initials: TY
authors.lastname: Huang
authors.forename: Ryh-Nan
authors.initials: RN
authors.lastname: Pan
authors.forename: Guo-Ping
authors.initials: GP
authors.lastname: Chang-Chien
authors.forename: Mei-Chich
authors.initials: MC
authors.lastname: Hsu
mesh_terms: D000328:Adult; D002853:Chromatography, Liquid / Q000379:methods*; D004300:Doping in Sports; D005260:Female; D005966:Glucuronidase; D064368:Healthy Volunteers; D006801:Humans; D008297:Male; D020849:Raloxifene Hydrochloride / Q000652:urine*; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D015813:Substance Abuse Detection / Q000379:methods*; D053719:Tandem Mass Spectrometry / Q000379:methods*; D055815:Young Adult
chemical_list: D020849:Raloxifene Hydrochloride; D005966:Glucuronidase