QuEChERS与高效液相色谱-串联质谱联用快速检测动物源产品中苯并烯氟菌唑残留  

Rapid analysis of benzovindiflupyr in animal-origin food using Qu ECh ERS coupled with high performance liquid chromatographytandem mass spectrometry

作　　者：隋程程 尤祥伟[1] 李义强[1] 姜桦韬 张广雨 

机构地区：[1]中国农业科学院烟草研究所,山东青岛266101

出　　处：《农药学学报》2017年第5期659-664,共6页Chinese Journal of Pesticide Science

摘　　要：为研究广谱性杀菌剂苯并烯氟菌唑通过饲料在动物源产品中的积累和残留风险,采用Qu ECh ERS前处理方法与高效液相色谱-串联质谱(HPLC–MS/MS)相结合,建立了苯并烯氟菌唑在4种动物源产品(猪肉、鸡肉、牛肉和鸡蛋)中的检测方法。样品用乙腈振荡提取,经N-丙基乙二胺(PSA)分散固相萃取净化后,HPLC–MS/MS检测,外标法定量。结果表明:在0.001~1 mg/L范围内,4种动物源产品中苯并烯氟菌唑的色谱峰面积与其相应的质量浓度间呈良好的线性关系,r>0.991 0。在0.004、0.01和0.1 mg/kg 3个添加水平下,苯并烯氟菌唑在鸡蛋、鸡肉、猪肉和牛肉中的回收率分别为83%~90%,82%~96%,85%~96%和77%~97%,相对标准偏差(RSD)分别为6.9%~11%,5.4%~8.7%,2.6%~7.3%和7.2%~10%。以最小添加水平作为方法的定量限,苯并烯氟菌唑在4种产品中的定量限均为0.004 mg/kg。所建方法具有简单、快速、灵敏、高通量等特点,适用于动物源产品中苯并烯氟菌唑的残留检测。在全国10个省份抽取120个样品(鸡蛋、鸡肉、猪肉和牛肉各30个)进行了监测,均未检出苯并烯氟菌唑残留。In order to study the accumulation and residual risk of the broad-spectrum fungicide benzovindiflupyr in animal-origin food, a rapid and simple method based on QuEChERS and high performance liquid chromatography-tandem mass spectrometry （I-IPLC-MS/MS） was developed for the determination of benzovindiflupyr in four animal-origin foods （pork, chicken, beef and egg）. Samples were extracted with acetonitrile, cleaned up by dispersive solid phase extraction with primary secondary amine, and detected by HPLC-MS/MS using external standard method for quantification. The result showed that, in the range of 0.001-1 mg/L, the peak area in the chromatography and the mass concentration of the corresponding benzovindiflupyr in different animal-origin foods were in good linearity with the correlation coefficients （r） higher than 0.991 0. The average recoveries of benzovindiflupyr were 84%-90%, 82%-96%, 85%-96% and 77%-97%, with relative standard deviations of 6.9%-11%, 5.4%-8.7%, 2.6%-7.3% and 7.2%-10% in egg, chicken, pork and beef, respectively. The limit of quantifications （LOQ） was 0.004 mg/kg, which was defined as the lowest spiking level with satisfactory recovery results. This method is simple, rapid, sensitive and high-throughput. Therefore it is suitable for the residual detecting of benzovindiflupyr in animal-origin foods. A survey of 120 animal- origin food samples collected in 10 provinces of China was conducted, and no benzovindiflupyr was detected in any samples.

关 键 词：QU ECH ERS 高效液相色谱-串联质谱 快速检测 动物源产品 苯并烯氟菌唑 残留 

分 类 号：S482.2[农业科学—农药学]