色谱2011，Vol.29Issue(8)：712-717,6.DOI:10.3724/SP.J.1123.2011.00712
液相色谱-串联质谱结合谱库检索法同时测定猪组织中12种类固醇激素
Determination of 12 steroid hormone residues in pig tissues by liquid chromatography-tandem mass spectrometry combining with library search
摘要
Abstract
A method was developed for the simultaneous determination and identification of 12 steroid hormone residues in pig tissues, including stanolone, aldosterone, boldenone, danazol, metandienone, methyltestosterone, nadrolone, norethindrone, progesterone, stanozolol, testosterone and testosterone propionate, using liquid chromatography-tandem triple-quadrupole linear ion trap mass spectrometry(LC-MS/MS). Homogenized pig tissue samples were purified with a Waters MCX solid phase extraction column after enzymatic hydrolysis by β-glucuroni-dase, then separated on a Venusil MP C18, column (100 mm x2. 1 mm, 3 μm) using gradient elution with the mobile phases of acetonitrile and water with 0. 1% (v/v) formic acid. A multiple reaction monitoring (MRM) as survey scan and an enhanced product ion (EPI) scan as dependent scan were performed in an information dependent acquisition (IDA) experiment. The compound identification was carried out by library search with a newly developed MS/MS library based on EPI spectra at three different collision energies in positive mode. The results showed that the limits of detection (LODs, S/N = 3) were in the range of 0. 2 -0. 5 μg/kg for the steroid hormones, and with a good linearity (r > 0. 99) ranged from 0. 5 to 100. 0 μg/L. The average recoveries (n =6) of the 12 steroid hormones spiked in pig tissue samples at 5. 0μg/kg ranged from 72. 0% to 98. 1% with the relative standard deviations (RSDs) between 3. 1% and 12. 5%. The method was applied for the qualitative and quantitative determination of steroidhormone residues in pig tissues with sensitive and accurate characteristics.关键词
液相色谱-串联质谱/类固酵激素/猪组织Key words
liquid chromatography-tandem mass spectrometry ( LC-MS/MS)/ steroid hormones / pig tissues分类
化学化工引用本文复制引用
蔡勤仁,冯家望,张毅,彭玉芬,薛良辰,杜志峰..液相色谱-串联质谱结合谱库检索法同时测定猪组织中12种类固醇激素[J].色谱,2011,29(8):712-717,6.基金项目
国家质量监督检验检疫总局科技项目(2009IK156) （2009IK156）
