QuEChERS-HPLC-MS/MS同时检测红薯中11种地下杀虫剂残留  

Determination of Eleven Types of Underground Pesticides in Sweet Potatoes by QuEChERS and HPLC-MS/MS

作　　者：刘红[1] 李传勇[2] 曾志杰[2] 陈其煌[2] 黄和勇 陈琼[2] 曹敏杰[1] 刘光明[1] 

机构地区：[1]集美大学食品与生物工程学院,福建厦门361021 [2]厦门市农产品质量安全检验测试中心,福建厦门361009

出　　处：《厦门大学学报（自然科学版）》2015年第6期802-811,共10页Journal of Xiamen University：Natural Science

基　　金：国家自然科学基金(31171660)

摘　　要：利用QuEChERS前处理结合高效液相色谱-串联质谱（HPLC-MS/MS）,建立同时检测红薯中11种地下杀虫剂的痕量残留分析方法.通过优化确定了乙腈提取、乙二胺-N-丙基硅烷（PSA）为净化剂的QuEChERS前处理方法;采用水（含0.1%甲酸,5%乙腈）和乙腈（含0.1%甲酸,5%水）梯度洗脱,Venusil MP C18色谱柱分离,电喷雾电离正离子（ESI＋）模式、多反应监测方式（MRM）测定,以及空白基质外标法定量.结果显示,11种地下杀虫剂的保留时间≤10min,在各自的范围内线性关系良好,R2〉0.999 0;方法的检出限（LOD）为0.007-4.000μg/kg,定量限（LOQ）为0.023-13.333μg/kg;空白红薯分别添加5,10,20和50μg/kg 4个含量水平,11种地下杀虫剂的平均回收率为81.7%-117.2%,相对标准偏差（RSD）为1.4%-8.3%.结果表明,本研究建立的QuEChERS-HPLC-MS/MS方法简单、快速,灵敏度、准确度符合要求,适用于红薯中多种地下杀虫剂痕量残留的同时检测.In this study a method has been developed for simultaneous and multiresidue analysis of 11 types of trace level under- ground pesticides in sweet potatoes by QuEChERS and high-performance liquid chromatography tandem mass spectrometry（HPLC- MS/MS）. Sample pretreatment conditions and HPLC-MS/MS conditions were optimized. From sweet potatoes acetonitrile was directly extracted,and pesticides were purified using primary secondary amine （PSA） with QuEChERS method. 0.1% HAc Acetonitrile-water （5：95,by volume） and 0.1% H Ac acetonitrile-water （95：5, by volume） were chose to be mobile with gradient elution, and then they were analyzed using HPLC-MS/MS in multiple reaction monitoring （MRM） modes via positive electrospray ionization （ESI＋ ） with an Venusil MP C18 column （3 μm,2.1 mm×100 mm） as the analytical column,and the quantization was carried out by the external standard method with the blank matrix. The chromatographic peaks of 11 types of underground pesticides were flowed out within 10 minutes. Data demonstrated that the linear correlation coefficients for 11 types of pesticides were not less than 0. 999 0 in their linear scope with good linearity. The limit of detection （LOD） ranged from 0. 007 to 4. 000 μg/kg,and the limit of quantization （LOQ） was in the range of 0. 023 to 13. 333 μg/kg. The recoveries of 11 types of underground pesticides in sweet potato matri- ces at four spiked levels of 5,10,20,and 50 μg/kg ranged from 81.7 % to 117.2%, and the relative standard deviations were in the range of 1.4% to 8.3 %. The results showed that the method is simple,rapid, and characterized with acceptable sensitivity and accuracy to meet the requirements of the pesticide residue analysis.

关 键 词：QUECHERS HPLC-MS/MS 红薯 地下杀虫剂残留 同时检测 

分 类 号：O657.63[理学—分析化学]