QuEChERS结合PTV-GC-MS/MS测定进口植物油籽及原油中109种农药  

The Residues of 109 Kinds of Pesticides in Oil Seeds and Crude Oil were Determined by QuEChERS Combines PTV-GC-MS/MS

作　　者：杨丽 王珂 魏哲文 房芳 徐新龙 刘海丽 吕新明 李兰 YANG Li;WANG Ke;WEI Zhewen;FANG Fang;XU Xinlong;LIU Haili;LV Xinming;LI Lan(Alashankou Customs Technology Center,Alashankou,Xinjiang 833418,China;Urumqi Customs Technology Center,Urumqi,Xinjiang 830000,China)

机构地区：[1]阿拉山口海关技术中心,新疆阿拉山口833418 [2]乌鲁木齐海关技术中心,新疆乌鲁木齐830000

出　　处：《农产品加工》2024年第21期86-94,99,共10页Farm Products Processing

基　　金：新疆维吾尔自治区自然科学基金项目(2021D01B14)。

摘　　要：利用优化后的QuEChERS前处理条件和PTV大体积进样技术,结合气相色谱三重四极杆串接质谱仪(GC-MS/MS)建立了一种进口植物油籽及植物原油中109种农药残留的快速检测方法。取试样2.00 g,用环己烷-乙酸乙酯(1∶1,V/V)萃取,经十八烷基键合硅胶、石墨化炭黑、N-丙基乙二胺吸附剂组合净化,采用PTV大体积进样,结合GC-MS/MS分析测试,以基质标准曲线校正与定量。结果表明,109种农药在0.005~0.500μg/mL内,线性相关系数良好,均达到0.99以上,在3个添加水平下的平均回收率为65.15%~118.50%,相对标准偏差(RSD)为0.60%~16.00%(n=6),各组分检出限(LOD)为0.002~0.010 mg/kg。该方法前处理过程简单,成功减少了基质和农药重叠信号的干扰,检测过程准确、高效,满足农残检测中的相关要求。该方法适用于植物油籽及植物原油中多种农药的残留检测,为口岸一线快速筛查及确证提供技术支撑。In this article,a rapid analytical technique for the detection of 109 pesticide residues in imported plant oil seeds and vegetable crude oil was established by using the optimized QuEChERS pretreatment conditions and PTV mass sampling technology,combined with GC-MS/MS.A 2.00 g sample was treated with a mixture of cyclohexane-ethyl acetate(1∶1,V/V)and then purified with a combination of C18,GCB and PSA.The sample was injected by PTV in large volume and tested by GC-MS/MS.The standard solution was used to calibrate it with matrix matching,and the quantification was done through the external standard method.The findings showed that strong linear correlations ranging from 0.005~0.500μg/mL for the 109 pesticides.The average recovery rates fell within the range of 65.15%~118.50%,with a variation of 0.60%~16.00%(n=6).The LOD of each component was 0.002~0.010 mg/kg.A pretreatment process of simplicity,which effectively eliminates the interference of matrix and pesticide overlapping peaks,along with an accurate and efficient detection process,as well as sensitivity and accuracy that met agricultural residue detection requirements.This method was suitable for the detection of pesticide residues in plant oilseeds and plant crude oil,and provided research methodology support for the rapid screening and confirmation of port.

关 键 词：QUECHERS PTV进样 气相色谱三重四极杆串接质谱仪 植物油籽 植物原油 农药残留 

分 类 号：O658[理学—分析化学]