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

中文关键词:  QuEChERS  超高效液相色谱-串联质谱法  动物源性食品  双酰胺类杀虫剂

英文关键词:QuEChERS  ultra performance liquid chromatography-tandem mass spectrometry  animal-derived foods  bisamide insecticides

中文摘要:

      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12.0 μg/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0.7~1.0 μg/kg和2.0~3.0 μg/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。

英文摘要:

      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 12.0 μg/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?1.0 μg/kg and 2.0?3.0 μg/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.