摘要
目的建立Qu ECh ERS-超高效液相色谱-串联三重四级杆质谱法(UPLCMS/MS)测定鸡肉基质中3类8种兽药残留的检测技术。方法鸡肉样品采用酸化乙腈提取,盐析后取乙腈相,用十八烷基硅烷(C18)和PSA吸附剂分散固相萃取净化,采用Waters ACQUITYTM BEH C18色谱柱(100 mm×2.1 mm×1.7μm)分离后于电喷雾正离子源(ESI+)和多反应监测(MRM)模式下进行测定,基质标准曲线结合稳定同位素内标法定量。结果 8种目标化合物阴性加标水平在1、2和4μg/kg下,回收率为81.2%~94.1%,RSD在4.2%~14.3%。8种目标化合物的检出限在0.1~0.2μg/kg,定量限在0.2~0.5μg/kg。对30件鸡肉样品进行目标化合物的检测,未检测到超限量的兽药残留。结论 UPLC-MS/MS法操作简便、快速,灵敏度和准确度高,包含种类较宽,具有拓展性,适用于鸡肉中该类兽药残留的日常监测。
Objective To develop a method for determination of 8 veterinary drug residues in chicken matrix by Qu ECh ERS-ultra performance liquid chromatography tandem mass spectrometry. Methods Chicken samples were extracted with acid acetonitrile,salting out,and then the organic phase were cleaned up by C18 and PSA. A Waters ACQUITYTM BEH C18column( 100 mm × 2. 1 mm × 1. 7 μm) was used for LC separation,ESI positive ion scan was used with multiple reaction monitoring( MRM)mode and quantified by matrix-matched external standard method. Results At the spiked level of 1,2 and 4 μg / kg,the recoveries of each compound were in the range of 81. 2%- 94. 1% with the relative standard deviations of 4. 2%- 14. 3%. The qualitative limits of detections were 0. 1- 0. 2 μg / kg and the quantitative limits were 0. 2- 0. 5 μg / kg for the 8 targets compounds. The established method was applied to the detection of the 8targets compounds in 30 chicken samples,and none of the 8 veterinary drugs exceeded the residue limits. Conclusion The method is simple,rapid,high sensitivity and good stability,with a wide variety and a certain development. It can be used for the daily monitoring of the veterinary drug residues in chicken.
作者
张楠
范赛
薛颖
刘平
刘伟
吴国华
赵榕
Zhang Nan Fan Sai Xue Ying Liu Ping Liu Wei Wu Guohua Zhao Rong(Beijing Center for Disease Control and Prevention,Beijing 100013, China)
出处
《卫生研究》
CAS
CSCD
北大核心
2017年第1期89-93,共5页
Journal of Hygiene Research
基金
国家自然科学基金(No.81302431)