[Screening, quantification and confirmation of beta-blockers in urine using gas chromatography-mass spectrometry].
A method was developed to perform the screening, quantification and confirmation of the five beta-blockers, propranolol, carteolol, bisoprolol, esmolol, and sotalol, in human urine using gas chromatography-mass spectrometry (GC-MS). In sample preparation, conjugated and unconjugated beta-blockers in urine were extracted separately, and the extracts were combined. The extracts were derivatized with N-methyl-N-trimethylsilyl-trifluoroacetamide (MSTFA) and N-methyl-bis(trifluoroacetamide) (MBTFA). The optimal conditions of GC-MS were established, and the progresses of screening by selected ion monitoring (SIM) mode and confirmation by full scan (SCAN) mode were completed. At last, the quantification curves of the five beta-blockers in spiked urine were established by SIM mode. The limits of detection were 0.2 -1.0 ng/mL. Overall recoveries were 70.5% - 103.4%, and the relative standard deviations were lower than 15%. In addition, the method was successfully applied to the analysis of the positive urine of propranolol, and the urinary excretion curve was also established accordingly. It is significant to prohibit the abuse of beta-blockers in doping control.
Shangguan
Liangmin
L
Key Laboratory of Analysis and Detection for Food Safety, Ministry of Education, Sport Science Research Center, Fuzhou University, Fuzhou 350002, China. shangguan789@163.com
Liu
Wei
W
Zheng
Xiangyang
X
Zhang
Lan
L
D000319:Adrenergic beta-Antagonists / Q000737:chemistry / Q000378:metabolism / Q000652:urine*; D000328:Adult; D004300:Doping in Sports; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D006801:Humans; D057230:Limit of Detection; D008297:Male; D015813:Substance Abuse Detection / Q000379:methods*; D016482:Urinalysis / Q000379:methods*
D000319:Adrenergic beta-Antagonists