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

发布时间：2019-01-11 21:19

【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,r0.991 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。
[Abstract]:In order to study the accumulation and residual risk of benzofuronazole, a broad-spectrum bactericide, in animal products through feed, the Qu ECh ERS pretreatment method was combined with high performance liquid chromatography-tandem mass spectrometry (HPLC MS/MS). A method for the detection of benzenefluronazole in four animal products (pork, chicken, beef and eggs) was established. The samples were extracted by oscillating acetonitrile, purified by N-propylethylenediamine (PSA) dispersion solid phase extraction, detected by HPLC MS/MS and quantified by external standard method. The results showed that in the range of 0.001 mg/L, there was a good linear relationship between the chromatographic peak area and the corresponding mass concentration of benzofuronazole in the four animal products, r 0.991 0. The recoveries of benzofuronazole in eggs, chicken, pork and beef at the levels of 0. 004 and 0. 1 mg/kg were 83%, 90% and 82% respectively, and the recoveries of benzofuronazole in eggs, chicken, pork and beef were 85%, 96% and 77 75%, respectively. The relative standard deviation (RSD) was 6.9 and 5.4, and about 2.6 percent and 7.2 percent and 10 percent respectively. Using the minimum addition level as the quantitative limit of the method, the quantitative limit of Benzofuronazole in the four products was 0.004 mg/kg.. The method is simple, rapid, sensitive and high throughput. It is suitable for the determination of benzofuronazole residues in animal products. A total of 120 samples (30 eggs, 30 chicken, 30 pork and 30 beef) were collected in 10 provinces of China, and no benzofuronazole residues were detected.
【作者单位】：中国农业科学院烟草研究所;
【分类号】：S859.84

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