超高效液相色谱-串联质谱法快速测定金银花中77种农药残留

Determination of 77 pesticides residues in Flos Lonicerae by ultra high performance liquid chromatography-tandem mass spectrometry

采用QuEChERS方法,利用超高效液相色谱-串联质谱技术,建立了金银花中77种常见农药残留的测定方法。金银花样品利用酸性乙腈溶液提取,乙二胺-N-丙基硅烷(PSA)净化,采用正离子多反应监测(MRM)模式,基质外标法定量。结果表明,在优化后的条件下,77种农药在0.005~100μg/L范围内线性关系良好,相关系数(r2)大于0.999,检出限为0.01~3.50μg/kg,回收率为72.8%~123.1%,相对标准偏差(RSD)为3.3%~8.5%。该方法适于金银花中常见农药的快速测定。

A muhiresidue analytical method for 77 common pesticides in Flos Lonicerae was developed by QuEChERS purification and ultra high performance liquid chromatography-tandem mass spectrometry determination. The sample was extracted by acidified acetonitrile, cleaned by primary secondary amine （PSA） , analyzed by the positive ion mode and multiple reaction monitoring （MRM） , and quantified by the matrix external standard method. Under the optimized conditions, the 77 pesticides showed good linearities in the range of 0. 05 ~ 100 μg,/L, with the correlation coefficients （ r^2 ） higher than 0. 999. The limits of detection for this method were 0. 01 ~ 3.50 μg/kg, and the recoveries were in the range of 72. 8% to 123.1% with the relative standard deviations from 3.3% to 8.5 %. The method is suitable for the rapid determination of the common pesticides in Flos Lonicerae.