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.
出处
《分析化学》
SCIE
EI
CAS
CSCD
北大核心
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
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
Gel permeation chromatography
Solid phase extraction
Rapid resolution liquid chromatographytandem mass spectrometry
Steroid hormones
Beef
