摘要
采用安捷仑5975GC／MS对猪尿中20种同化激素进行同时检测。对于10．0g尿液样品，采用β-葡糖苷酸酶（来自Helix pomatia）对提取物水解后，加入过饱和NaCl，经乙腈提取，用过C18小柱和NH2小柱净化后七氟丁酸酐对其进行衍生，最后利用GC／MS进行检测。采用外标法定量，以S／N≥3确定的，检出限均能达到0．25μg／kg。通过对3个添加水平的回收实验表明，平均回收率为77．0％-111．0％。
A highly sensitive, specific and credible method for the simultaneous determination of 20 anabolic steroids in urine of pig performed by GC/MS was developed. Samples of urine of pig（ 10.0 g） were deconju- gated by Helix pomatia juice, extracted with acetonitrile, cleaned-up through dual columns of C18 and NH2, the extracts obtained were derivatized with heptafluorobutyric anhydride, following formation of the di-heptafluorobutyryl（di-HFB） derivative, and then identification and quantification were carried out by capillary gas chromatography-mass spectrometry. For quantitation, the external standards were used and the method was validated with blank samples fortified at 0.5, 2.5 and 2.5 μg/kg with 10.0 g sample. The detection limits were less than 0.25 μg/kg for all analytes. Overall recovery and repeatability （ relative standard deviations, RSD） ranged from 77.0% to 111.0%, and from 4.3% to 23.2%, respectively.
出处
《分析化学》
SCIE
EI
CAS
CSCD
北大核心
2009年第2期251-254,共4页
Chinese Journal of Analytical Chemistry
基金
国家质检总局(No.2005IK033)资助项目
关键词
同化激素
气相色谱-质谱联用
猪尿
Anabolic steroid, gas chromatography/mass spectrometry, urine
