摘要
建立了亚临界水萃取及液相色谱-串联质谱法(LC-MS/MS)检测猪肉中β-受体激动剂和氯霉素的方法。样品酶解后,经亚临界水萃取,C18粉未净化,目标物经Agilent XDB-C18柱(4.6 mm×50 mm,1.8μm)分离,采用液相色谱-串联质谱法多反应监测(MRM)模式检测,基质匹配溶液内标法定量。优化条件下,沙丁胺醇和莱克多巴胺在1.0～32.0μg/L范围内线性关系良好,其定量下限(S/N>10)为0.5 ng/g,检出限(S/N>3)为0.25 ng/g;克伦特罗和氯霉素在0.2～6.4μg/L范围内线性关系良好,其定量下限(S/N>10)为0.1 ng/g,检出限(S/N>3)为0.05 ng/g,相关系数均大于0.99。猪肉基质在3个加标水平下,回收率为79.2%～113.6%,相对标准偏差(RSDs)为3.2%～12.0%。该方法的灵敏度、准确度和精密度均符合兽药残留测定的技术要求,适用于猪肉中β-受体激动剂和氯霉素残留的检测。
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 μm）.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/N10） of 0.5 ng/g and detection limits（S/N3）of 0.25 ng/g,and 0.2-6.4 μg/L for clenbuterol and chloramphenicol with quantitation limits（S/N10） of 0.1 ng/g and detection limits（S/N3）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.
出处
《分析测试学报》
CAS
CSCD
北大核心
2013年第7期789-795,共7页
Journal of Instrumental Analysis
基金
国家质量监督检验检疫总局科技计划项目(2011IK233)
质检公益行业科研专项项目(201110019-04)
质检公益行业科研专项项目(201010045)
上海市研发基地平台项目(11DZ2210700)
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
subcritical water
liquid chromatography-tandem mass spectrometry（LC-MS/MS）
pork
chloramphenicol
β-agonists
