色谱2012，Vol.30Issue(10)：991-1001,11.DOI:10.3724/SP.J.1123.2012.08017
液相色谱-四极杆/离子阱质谱同时确证和测定肌肉中16种同化甾体激素残留
Simultaneous identification and detection of 16 anabolic steroid hormones in muscle using liquid chromatography coupled to quadrupole/linear ion trap mass spectrometry
摘要
Abstract
A comprehensive method for simultaneous identification and detection of 16 anabolic steroid hormones (ASs, including andorgens, gestagens and their esters) in muscle samples was developed with liquid chromatography coupled to quadrupole/linear ion trap mass spectrometry (LC-Q/Trap-MS). The ASs in muscle samples were extracted with acetonitrile under ultrasonic assistance. The extract was defatted by n-hexane with liquid-liquid partitioning and followed by clean-up with NH2 solid phase extraction (SPE) cartridge. The separation of ana-lytes was carried out on a CAPCELL PAK C18 MG Ⅲ column (150 mm ×2.0 mm, 5. 0 μm) using mobile phases of 0.1 % ( v/v) formic acid in acetonitrile and 0.1% ( v/v) formic acid-5 mmol/L ammonium formate aqueous solution with gradient elution. A scheduled multiple reaction monitoring (sMRM) in positive mode as survey scan and an enhanced product ion (EPI) scan as dependent scan in an information-dependent acquisition (IDA) experiment was adopted in mass spectrometry acquisition. On-line lab-built MS/MS library and internal standards were employed for the identification and quantification. As a result, the 16 ASs showed good linearity with all correlation coefficients (r) no less than 0. 999 0 within the linear ranges. The limits of quantification (LOQs, S/N≥10) for the 16 ASs were in the range of 0. 029 -0. 36 μg/kg. At the three spiked levels (0. 5 , 2. 0 and 20 μg/kg) , the overall recoveries ranged from 89. 9% to 118% with the relative standard deviations ( RSDs) no more than 16.2% under within-laboratory reproducibility conditions. The proposed method can be used to identify and detect the 16 ASs in a single run, which makes it effective in residue surveillance of anabolic hormones in muscle samples.关键词
液相色谱/四极杆/离子阱质谱/同化甾体激素/残留/肌肉Key words
liquid chromatography (LC)/ quadruple/linear ion trap mass spectrometry (Q/ Trap-MS) / anabolic steroid hormones (ASs) / residues/ muscle分类
化学化工引用本文复制引用
张鸿伟,蔡雪,林黎明,陈亮珍,梁成珠,鲍蕾,汤志旭,牛增元,王凤美..液相色谱-四极杆/离子阱质谱同时确证和测定肌肉中16种同化甾体激素残留[J].色谱,2012,30(10):991-1001,11.基金项目
国家质检总局科技项目(2007IK144)、山东省科技发展计划项目(2008GG10009020)和山东出入境检验检疫局科研攻关项目(SK200820). （2007IK144）
