UPLC-MS/MS同时检测蔬菜中三种杀菌剂残留的研究

Simultanous Determination of Three Fungicides in Vegetables by UPLC-MS/MS

为建立同时检测蔬菜中烯酰吗啉、霜脲氰和唑嘧菌胺残留的分析方法,样品经乙腈提取,十八烷基硅烷(C18)分散固相萃取净化,以HSS T3色谱柱分离待测物,甲醇和0.1%甲酸水为流动相梯度洗脱,正负离子分段扫描和多反应检测模式(MRM)检测,基质匹配标准溶液外标法定量。结果发现,烯酰吗啉、霜脲氰和唑嘧菌胺在0.001~1.000μg·mL^(-1)范围内线性关系良好,相关系数均大于0.999。目标物在蔬菜中的定量限均为0.005 mg·kg^(-1)。样品添加回收试验中,烯酰吗啉的平均回收率为87.3%~105.6%,相对标准偏差为1.5%~11%(n=5);霜脲氰的平均回收率为85.4%~113.4%(n=5),相对标准偏差为0.5%~10.9%(n=5);唑嘧菌胺的平均回收率为80.9%~108.4%,相对标准偏差为2.8%~10.2%(n=5)。该方法快速简便,定量准确,可满足多种蔬菜中烯酰吗啉、霜脲氰和唑嘧菌胺残留检测要求。

In order to establish an analytical method for simultaneous detection of dimethomorph, cymoxanil and ametoctradin residues in vegetables, the samples were extracted with acetonitrile, purified by octadecylsilane(C18) dispersed solid phase extraction, separated by HSS T3 chromatographic column, gradient eluted with methanol and 0.1% formic acid water as mobile phase, detected by positive and negative ion segmented scanning and multi-reaction detection mode(MRM), and quantified by matrix matching standard solution external standard method. The results showed that dimethomorph, cymoxanil and ametoctradin had good linear relationships in the range of 0.001~1.000 μg·mL^(-1), and the correlation coefficients were all greater than 0.999. The quantitative limit of the target substance in vegetables was 0.005 mg·kg^(-1). In sample addition recovery test, the average recovery rates of dimethomorph were 87.3%~105.6%, and the relative standard deviations were 1.5%~11%(n=5). The average recovery rates of cymoxanil were 85.4%~113.4%(n = 5), and the relative standard deviations were 0.5%~10.9%(n=5). The average recovery rates of ametoctradin were 80.9%~108.4%, and the relative standard deviations were 2.8%~10.2%(n=5). The present method was rapid, simple and accurate, and it met the requirements of residue detection of dimethomorph, cymoxanil and ametoctradin in various vegetables.