高效液相色谱法快速测定三种果蔬中甲苯氟磺胺和苯氟磺胺残留量

甲苯氟磺胺和苯氟磺胺均为杀菌剂,中等毒性,分解产物可转化为有毒物质,现行国标规定的检测方法为气相色谱-质谱联用法,但操作复杂、仪器普及率不高、适用范围有限。本试验建立了一种高效液相色谱法测定三种果蔬(黄瓜、番茄、葡萄)中甲苯氟磺胺和苯氟磺胺残留量的方法。样品采用QuEChERS方法进行前处理,以乙腈-0.1%甲酸水溶液-乙腈为流动相,梯度洗脱,采用高效液相色谱二极管阵列检测器分析。结果显示,QuEChERS前处理的吸附剂组合为750 mgMgSO4+50 mgC18+250 mgPSA+50 mgGCB,对样品进行净化处理后,上清液澄清,略带色泽,化合物平均回收率在79%以上;甲苯氟磺胺和苯氟磺胺在各自浓度范围内线性关系良好(R2=0.9999),加标回收率为79.73%~97.39%,精密度RSD为1.68%~4.21%(n=6),检出限分别为12.5μg/kg和15.1μg/kg,定量限分别为41.9μg/kg和50.2μg/kg。该方法操作简便、灵敏度高、结果准确可靠,能很好地满足上述三种果蔬中甲苯氟磺胺和苯氟磺胺残留量的分析检测。

Determination of Dichlofluanid and Tolylfluanid Residues in Fruits and Vegetables by High Performance Liquid Chromatography

Dichlofluanid and tolylfluanid are fungicides with medium toxic,and the decomposition products change into toxic substances,the detection method is gas chromatograph-mass spectrometry in the current national standards,but it is complex,low penetration and limited scope.A method for the simultaneous determination of dichlofluanid and tolylfluanid in fruits and vegetables(cucumber,tomato,grape)was developed by using high performance liquid chromatography.Samples were extracted by QuEChERS method.The HPLC-DAD method was perfored with acetonitrile and 0.1%formic acid water as mobile phase by the gradient elution.The adsorbent combinations of QuEChERS were 750 mgMgSO4+50 mgC18+250 mgPSA+50 mgGCB.After the sample was purified,the supernatant was clear and slightly colored,and the average recovery rate of the compound was over 79%.The standard curves of dichlofluanid and tolylfluanid showed good linearities(R2=0.9999).The recoveries at three levels ranged from 79.73%to 97.39%,the relative standard deviations of precision(n=6)were between 1.68% and 4.21%.The limits of detection were 12.5μg/kg and 15.1μg/kg,the limits of quantification were 41.9μg/kg and 50.2μg/kg.This established method is simple,sensitive,accuracy and reliable,it can be applied to the determination of dichlofluanid and tolylfluanid residues analysis in cucumber,tomato and grape.