快速滤过型净化法应用于气相色谱—串联质谱检测大豆中农药残留  

Detection of Pesticide Residues in Soybean by Multi-Plug Filtration Cleanup Combined with Gas Chromatography-Tandem Mass Spectrometry

作　　者：张鹏 彭菲 刘玮琦 刘贺 马玲 刘本纬 刘振伟 刘宁 ZHANG Peng;PENG Fei;LIU Weiqi;LIU He;MA Ling;LIU Benwei;LIU Zhenwei;LIU Ning(Manzhouli Customs Technology Center,Manzhouli 021400,China)

机构地区：[1]满洲里海关技术中心,内蒙古满洲里021400

出　　处：《大豆科学》2023年第4期466-472,共7页Soybean Science

基　　金：海关总署科研项目(2022HK029)。

摘　　要：为研究快速滤过型净化法(m-PFC)对大豆基质中14种常见农药残留气相色谱-串联质谱(GC-MS/MS)同时检测的适用性,本研究选取两种快速滤过型净化柱(m-PFC柱)作为净化手段,利用气相色谱-串联质谱进行检测分析,以外标法作为定性定量依据对14种农药进行测定,通过对基质效应、净化效果、回收率、多次滤过效果等方面进行评价。结果显示:多数农药在大豆基质中的基质效应影响无法忽略,14种农药在0.005~0.5 mg·mL^(-1)范围内线性关系良好,回收率为85%~110%,RSD为4.3%~10.2%,m-PFC柱2(150 mg无水硫酸镁,25 mg MWCNTs,25 mg C18,25 mg PSA)的净化效果更好,两次滤过次数的净化效果、检测准确度、重复性更佳。本方法可对大豆中14种农药进行快速测定,操作简单,效率高,亦具备一定的普适性,可以作为大豆中其他农药残留检测的参考方法。This study developed a method for the simultaneous determination of 14 pesticide residues in soybeans using Gas Chromatography-tandem Mass Spectrometry(GC-MS/MS)by multi-Plug Filtration Cleanup(m-PFC)method.Two multi-Plug Filtration Cleanup columns(m-PFC columns)were selected as the cleanup means,and fourteen pesticides were determined by GC-MS/MS with external standards as the qualitative and quantitative basis,and evaluated by matrix effect,cleanup effect,recovery and multiple filtration effect.The results showed that the effect of matrix effect in soybean matrix was not ignorable for most pesticides.The fourteen pesticides showed good linearity in the range of 0.005-0.5 mg mL^(-1) with recoveries between 85%-110%and RSDs between 4.3%-10.2%.m-PFC column 2(150 mg anhydrous MgS04,25 mg MWCNTs,25 mg Cis,and 25 mg PSA)gave better purification results.The two filtrations gave better clean-up,assay accuracy and reproducibility.It can be used as a reference method for the determination of other pesticide residues in soybean.

关 键 词：农药残留 m-PFC 净化 气相色谱-串联质谱 大豆 检测 

分 类 号：O657.63[理学—分析化学] TS214.2[理学—化学]