固相萃取-气相色谱-质谱联用法测定人尿中11种蛋白同化激素
GC-MS Determination of 11 Anabolic Steroids in Human Urine with Solid-Phase Extraction
摘 要
建立了固相萃取(SPE)-气相色谱-质谱联用(GC-MS)同时测定尿样中11种蛋白同化激素的分析方法,并将该方法用于美雄酮(MADE)阳性尿的分析.尿样前处理采用含500 mg填料的C18 SPE柱净化浓缩,然后进行酶解,最后由液-液萃取获得待测样品.为了提高灵敏度,待测样品采用硅烷化衍生后进行GC-MS分析.在选择离子监测(SIM)模式下,采用甲睾酮(MT)为内标进行定量分析,方法检出限为0.1~2.0 μg·L-1;分析加标实际样品,回收率在70.5%~121%,相对标准偏差为1.1%~13.9%.
固相萃取
蛋白同化激素
人尿
GC-MS
SPE
Anabolic steroids
Human urine
Abstract
Hyphenated GC-MS was applied to the simultaneous determination of 11 anabolic steroids in human urine. Urine sample was treated with C18 solid phase extraction (SPE) column to purify and concentrate the analytes. The eluate from the SPE column was evaporated to dryness and enzymehydrolyzed in PBS of ca. pH 7,extracted with tert. butyl methyl ether,and dried by blowing with nitrogen. To improve sensitivity of determination,prederivatization of the sample solution with silane was performed. GC-MS determination was carried out using methyl testosterone as internal standard and with the SIM mode. Detection limits (S/N=3) obtained were in the range of 0.1-2.0 μg·L-1. Tests for recovery and precision were made on the base of substantial samples,and values of average recovery found were in the range of 70.5%-121.0%,and values of RSD′s (n=5) were in the range from 1.1% to 13.9%.
中图分类号 O657.37
所属栏目 试验与研究
基金项目 福建省自然科学基金资助项目(B0510006);福州大学人才基金资助项目(0041826260,0041826486);“高校新世纪优秀人才支持计划”资助项目.
收稿日期 2008/2/17
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备注张卓旻(1980-),男,闽侯人,博士,讲师,从事色谱分析.
引用该论文: ZHANG Zhuo-min,SHANGGUAN Liang-min,LIU Wei,ZHANG Lan. GC-MS Determination of 11 Anabolic Steroids in Human Urine with Solid-Phase Extraction[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2008, 44(9): 810～814
张卓旻,上官良敏,刘薇,张兰. 固相萃取-气相色谱-质谱联用法测定人尿中11种蛋白同化激素[J]. 理化检验－化学分册, 2008, 44(9): 810～814
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参考文献
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【2】International Olympic Committee. Report of the inter-national olympic committee medical commission[M].Innsbruck: International Olympic Committee,1974．
【3】Brook R V. Detection of anabolic steroids by radio immunoassay[J]. Brit J Sports Med,1975,9:89-98．
【4】毕红钢,周同惠.人尿中几种雄激素及蛋白同化激素的HPLC测定[J].药学学报,1989,4(3):207-211．
【5】Gonzalo-Lumbreras R,Izquierdo-Hornillos R. Method development for corticosteroids and anabolic steroids by micellar liquid chromatography[J]. J Chromatogr B,2003,794:215-225．
【6】Uralets V P. Analysis of anabolic steroids in body fluids by capillary gas chromatography with a two-channel detection system and a computer[J]. J Chromatogr,1983,279:695-708．
【7】Adatia R. An important method for steroid profile analysis using capillary gas chromatography[J]. Chromatographia,1988,25:598-606．
【8】Fuh M R,Huang S Y,Lin T Y. Determination of residual anabolic steroid in meat by gas chromatography-ion trap-mass spectrometer[J]. Talanta,2004,64:408-414．
【9】Hernandez-Carrasquilla M. Gas chromatography-mass spectrometry analysis of anabolic compounds in bovine hair: evaluation of hair extraction procedures[J]. Anal Chim Acta,2001,434:59-66．
【10】Yu N H,Ho E N M,Leung D K K,et al. Screening of anabolic steroids in horse urine by liquid chromatography-tandem mass spectrometry[J]. J Pharm Biomed Anal,2005,37:1031-1038．
【11】Marcos V,Perogordo E,Espinosa P,et al. Multiresidue analysis of anabolic compounds in bovine hair by gas chromatography-tandem mass spectrometry[J]. Anal Chim Acta,2004,507:219-227．
【12】Hatton C K,Catlin D H. Detection of androgenic anabolic steroids in urine[J]. Clin Lab Med,1987,7:655-668．
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