QuEChERS-超高效液相色谱-串联质谱法同时测定动物源性食品中5种双酰胺类杀虫剂的残留

Simultaneous determination of 5 kinds of bisamide insecticides residues in animal-derived foods by QuEChERS-ultra performance liquid chromatography-tandem mass spectrometry

目的建立超高效液相色谱-串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry,UPLC-MS/MS)检测猪肉、猪肝、鸭肉、鸡肉和鱼肉等动物源性食品中5种双酰胺类杀虫剂(氟苯虫酰胺、氯虫苯甲酰胺、溴氰虫酰胺、四氯虫酰胺、环溴虫酰胺)残留量的分析方法。方法采用QuEChERS前处理技术,样品用乙腈提取,提取液经盐析脱水,吸附剂净化,用ACQUITY UPLC BEH C18色谱柱梯度洗脱分离,电喷雾离子源离子化,负离子多反应监测模式检测。结果5种双酰胺类杀虫剂在2.0~50.0 ng/mL的质量浓度范围内线性关系良好,相关系数(r)大于等于0.9983。在3.0、6.0和12.0μg/kg 3个添加水平下,5种双酰胺类杀虫剂的回收率范围为79.6%~112.4%,相对标准偏差(relative standard deviations,RSDs)为0.4%~6.9%(n=6),方法检出限和定量限范围分别为0.7~1.0μg/kg和2.0~3.0μg/kg。结论本方法操作简单、灵敏度和准确度高、重现性好,可同时检测动物源性食品中5种双酰胺类杀虫剂的残留量,为其日常监管提供技术支持。

Objective To establish an method for the determination of the residues of 5 kinds of bisamide insecticides(cyantraniliprole,chlorantraniliprole,tetraclofenac,chlorfenapyr,flubendiamide)in pork,pork liver,duck meat,chicken,fish and other animal-derived foods by ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).Methods The QuEChERS pretreatment technology was adopted,the samples were extracted with acetonitrile,and the extracts were subjected to salting-out dehydration,adsorbent purification,gradient elution and separation on an ACQUITY UPLC BEH C18 column,followed by ionization with an electrospray ion source,and anion multi-reaction monitoring mode detection.Results The linear relationships were good within the mass concentration range of 2.0-50.0 ng/mL,and the correlation coefficients(r)were greater than or equal to 0.9983.At the 3 kinds of addition levels of 3.0,6.0 and 12.0μg/kg,the recovery rates of the 5 kinds of bisamide insecticides ranged from 79.6%to 112.4%,and the relative standard deviations(RSDs)were 0.4%-6.9%(n=6),and the limits of detection and quantification were 0.7-1.0μg/kg and 2.0-3.0μg/kg,respectively.Conclusion This method is simple to operate,high in sensitivity and accuracy,good in reproducibility,and can simultaneously detect the residues of 5 kinds of bisamide insecticides in animal-derived foods,thus providing technical support for their daily supervision.