凝胶渗透色谱-固相萃取净化-超快速液相色谱-串联质谱法检测牛肉中9种类固醇激素残留  

Determination of Nine Steroid Hormones Residues in Beef Samples by Gel Permeation Chromatography-Solid Phase Extraction-Rapid Resolution Liquid Chromatography-Tandem Mass Spectrometry

作　　者：孙汉文[1] 康占省[1] 李挥[1,2] 

机构地区：[1]河北大学化学与环境科学学院,河北省分析科学重点实验室,保定071002 [2]河北省食品质量监督检验研究院,石家庄050051

出　　处：《分析化学》2010年第9期1272-1276,共5页Chinese Journal of Analytical Chemistry

基　　金：教育部博士点基金(No20050075003);河北省自然科学基金(NoB2008000583);河北省科技支撑项目(No09227134D)资助

摘　　要：建立了凝胶渗透色谱分离-固相萃取净化-超快速液相色谱-串联质谱(GPC-SPE-RRLC-MS/MS)测定牛肉中群勃龙、勃地龙、诺龙、睾酮、美雄酮、甲基睾酮、司坦唑醇、黄体酮、苯丙酸诺龙9种类固醇激素残留的方法。试样经β-盐酸葡萄糖醛苷酶/芳基硫酸酯酶酶解,叔丁基甲醚超声提取,凝胶渗透色谱和HLB固相萃取柱净化,以乙腈-0.1%甲酸水溶液为流动相,经Agilent Plus C18柱分离后以MS/MS多反应监测扫描模式检测。方法线性相关系数r>0.999,定量限为0.2～0.7μg/kg。在3种浓度添加水平0.3,1.0,4.0μg/kg下,其平均回收率为81.4%～110%;相对标准偏差(RSD)为2.2%～9.8%。本方法已成功应用于高脂肪和基质复杂样品中9种类固醇激素残留的检测。A gel permeation chromatography solid phase extraction-rapid resolution liquid chromatographytandem mass spectrometric（GPC-SPE-RRLC-MS/MS） method was developed for the determination of 9 steroid hormones（trenbolone,boldenone,nandrolone,testosterone methandienone,methyltestosterone,stanozolol,progesterone and nandrolone phenylpropionate） in beef tissue.The beef samples were enzymatically digested with β-glucuronidase/arylsulfatase,and then extracted with tert-butyl methyl ether under ultrasonication incubation.Clean-up was carried out with gel permeation chromatography followed by a further HLB solid phase extraction.After C18 RRLC gradient elution separation using acetonitrile-0.1% aqueous formic acid as a mobile phase,the eluents were qualitatively and quantitatively determined under multi-reaction monitoring（MRM） scan type with tandem mass analyzer.The limit of quantification（LOQ） was 0.2-0.7 μg/kg,and the calibration curves showed good linearity with correlation coefficients larger than 0.999.At the spiked levels of 0.2,1.0 and 4.0 μg/kg,the mean recoveries were in the range of 81.4% to 110%,and the relative standard deviations（RSDs） were in the range of 2.2% and 9.8%（n=7）.The experimental results showed this method is sensitive,and accurate.The proposed method was used for the determination of 9 steroid hormones residues in high-fat and complex sample.

关 键 词：凝胶渗透色谱 固相萃取 超快速液相色谱-串联质谱 类固醇激素 牛肉 

分 类 号：R155.5[医药卫生—营养与食品卫生学]