QuEChERS样品前处理方法联合在线GPC/GC-MS测定水果中15种三唑类农药残留量方法评估  

Evaluation of QuEChERS Method for the Analysis of 15 Triazole Pesticides Residues in Fruits by Online Gel Permeation Chromatography Gas Chromatography-Mass Spectrometry

作　　者：李海飞[1] 聂继云[1] 徐国锋[1] 李静[1] 闫震[1] 李志霞[1] 毋永龙[1] 匡立学[1] 

机构地区：[1]中国农业科学院果树研究所农业部果品质量安全风险评估实验室(兴城)农业部果品及苗木质量监督检验测试中心(兴城),辽宁兴城125100

出　　处：《分析测试学报》2015年第12期1331-1338,共8页Journal of Instrumental Analysis

基　　金：国家农产品质量安全风险评估计划(GJFP2014002;GJFP2015002);中央级科研院所基本科研业务费专项(0032014013);中国农业科学院科技创新工程(CAAS-ASTIP)

摘　　要：比较了3种QuEChERS方法（未加缓冲盐的原创QuEChERS方法、加乙酸盐的AOAC 2007.01方法以及加柠檬酸缓冲盐的CEN 15662方法）提取水果中15种三唑类农药的有效性,考察了乙二胺-N-丙基硅烷（PSA）和C_（18）吸附剂的净化效果,以提取后添加法评估了苹果、梨、桃、葡萄、樱桃、香蕉及橙子中各目标化合物的基质效应。结果表明,3种QuEChERS方法的回收率无明显差异,但原创QuEChERS方法操作简单、成本较低,且有较好的回收率和较低的基质效应。联合使用PSA和C_（18）吸附剂的净化效果优于单独使用PSA或C_（18）的净化效果。15种三唑类农药在7种基质中均存在基质增强效应。采用原创QuEChERS方法结合在线凝胶渗透色谱串联气相色谱-质谱（GPC/GC-MS）,实现了在线净化与分析检测的自动化,缩短了分析时间,弥补了原创QuEChERS方法去除干扰不彻底的缺陷,同时利用PTV大体积进样和进样口程序升温方式提高了检测灵敏度。15种农药在7种基质3个加标水平（20,50,100μg/kg）下的平均回收率为85.7%～120.1%,相对标准偏差（RSD）为0.2%～11.5%,在10～400μg/L范围内线性关系良好,相关系数（r）大于0.998;检出限为0.9～9.5μg/kg。该方法简便快速、准确可靠、经济环保,适用于水果中三唑类农药多残留的快速检测。A comparison was made among three versions of QuEChERS sample preparation methods for the extraction of 15 triazole pesticides in fruits. The three QuEChERS methods were the original method without buffer,the AOAC Official Method 2007. 01 with acetate buffer,and the CEN 15662 Method with citrate buffer. The clean-up effects of primary secondary amine（ PSA） sorbent and C18 sorbent on 15 triazole pesticides were studied. The addition method after extraction was used to evaluate the matrix effects of triazole pesticide in matrix of apple,pear,peach,grape,cherry,banana and orange during gel permeation chromatography coupled to gas chromatography-mass spectrometry（ GPC /GC-MS） analysis. As a result,the QuEChERS method without buffer gave good recoveries for 15 triazole pesticides. The cleaning up effect of PSA plus C18 is superior to that of C18 or PSA sorbent. The matrix effects were intensive in the 7 kinds of fruits. In this article,15 triazole pesticides were extracted by the QuEChERS method without buffer, and analysed by using matrix-matched standard calibration as the external standard method with gas chromatography-mass spectrometry in selective ion monitoring（ SIM） mode. Moreover,a large volume of sample was allowed to be injected using the program of GPC programmed temperature vaporizer of gas chromatography to improve the sensitivity of measurements. The recoveries of 15 residues in 7 matrixes at three spiked levels of 20,50,100 μg / kg ranged from 85. 7% to 120. 1% with relative standard deviations of 0. 2%-11. 5%.The calibration curves were linear（ r 0. 998） in the range of 10-400 μg / L for all the pesticides.The limits of detection（ LOD） for the pesticides in fruits ranged from 0. 9 μg / kg to 9. 5 μg / kg.Based on these results,the analytical method was proved to be highly efficient,robust and sensitive,and was suitable for monitoring 15 triazole pesticides residues in fruits.

关 键 词：QUECHERS 在线凝胶渗透色谱串联气相色谱-质谱 三唑类农药残留 基质效应 水果 

分 类 号：O657.63[理学—分析化学] F767.2[理学—化学]