分析测试学报2013，Vol.32Issue(7)：789-795,7.DOI:10.3969/j.issn.1004-4957.2013.07.002
亚临界水萃取及液相色谱-串联质谱法检测猪肉中β-受体激动剂与氯霉素残留
Determination of β-Agonists and Chloramphenicol Residues in Pork by Subcritical Water Extraction and Liquid Chromatography-Tandem Mass Spectrometry
摘要
Abstract
A liquid chromatography-tandem mass spectrometric (LC-MS/MS) method with subcritical water extraction was developed for the determination of β-agonists and chloramphenicol in pork.Enzymatic hydrolysis was firstly used during the preparation of pork,then the target compounds were extracted with subcritical water and cleaned up by C18.The LC separation was performed on an Agilent XDB-C18 column(4.6 mm ×50 mm,1.8 μ m).The veterinary drugs were determined by MS/MS in MRM mode and quantified by the matrix-matched internal standard method.The calibration curves showed good linearities in the ranges of 1.0-32.0 μg/L for salbutamol and ractopamine with quantitation limits(S/N ＞ 10) of 0.5 ng/g and detection limits(S/N ＞3)of 0.25 ng/g,and 0.2-6.4 μg/L for clenbuterol and chloramphenicol with quantitation limits (S/N＞ 10) of 0.1 ng/g and detection limits (S/N ＞ 3) of 0.05 ng/g.The correlation coefficients were all larger than 0.99.The recoveries of veterinaries in pork at three spiked levels ranged from 79.2％ to 113.6％ with relative standard deviations(RSDs)of 3.2％-12.0％.The sensitivity,accuracy and precision of the method could meet the technical standard for veterinary drugs determination,and the method was suitable for the determination of β-agonists and chloramphenicol in pork.关键词
亚临界水/液相色谱-串联质谱/猪肉/氯霉素/β-受体激动剂Key words
subcritical water/liquid chromatography-tandem mass spectrometry (LC-MS/MS)/pork/chloramphenicol/β-agonists分类
化学化工引用本文复制引用
潘煜辰,周瑶,伊雄海,邓晓军,陈舜胜,杨惠琴,朱坚..亚临界水萃取及液相色谱-串联质谱法检测猪肉中β-受体激动剂与氯霉素残留[J].分析测试学报,2013,32(7):789-795,7.基金项目
国家质量监督检验检疫总局科技计划项目(2011IK233) （2011IK233）
质检公益行业科研专项项目(201110019-04) （201110019-04）
质检公益行业科研专项项目(201010045) （201010045）
上海市研发基地平台项目(11DZ2210700) （11DZ2210700）
