QuEChERS-超高效液相色谱-串联质谱法快速检测鸡肉中8种常见兽药残留

Rapid detection of 8 veterinary drug residues in chicken by QuEChERS-ultra performance liquid chromatography tandem mass spectrometry

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.