QuEChERS-气相色谱串联质谱法快速测定供港蔬菜中118种农药残留  

Determination of 118 pesticide residues in vegetables from Hong Kong’s regulation by modified-QuEChERS combined with gas chromatography-tandem mass spectrometry

作　　者：司露露 梁杨琳 李湧 吕春秋 覃金兰 邓佳宁 汪文龙 SI Lu-lu;LIANG Yang-lin;LI Yong;LV Chun-qiu;QIN Jin-lan;DENG Jia-ning;WANG Wen-long(Technical Center of Nanning Customs District,Nanning 530021,China;Hezhou Customs,Hezhou 542800,China)

机构地区：[1]南宁海关技术中心,广西南宁530021 [2]贺州海关,广西贺州542800

出　　处：《化学研究与应用》2020年第11期2034-2043,共10页Chemical Research and Application

基　　金：广西重点研发计划基金项目(桂科AB17292071)资助;南宁海关科技计划基金项目(2018GXCIQ009)资助。

摘　　要：建立了QuEChERS法结合气相色谱串联质谱(GC-MS/MS)高通量快速检测供港蔬菜中118种香港规例农药残留的方法。以1%(v/v)乙酸乙腈为提取溶剂,高速匀浆提取,净化后添加内标校正回收率,基质匹配标准曲线进行定量。GC-MS/MS检测的118种农药在0.01~0.20 mg·L^-1范围内线性关系良好,相关系数均在0.995以上。所有的农药定量限均小于0.01 mg·kg^-1,各个浓度水平加标回收率为70.1%~116.7%,其中回收率在90%~110%之间的化合物占87%,重复性试验的相对标准偏差(RSD)为0.6%~17.7%(n=6)。本方法重现性和稳定性良好,定量限满足港澳以及世界各地对农残检测的要求,适用于监管供港蔬菜的农药残留。A throughput and rapid method for the determination of 118 pesticide residues in vegetables supplied to Hong Kong was developed by modified-QuEChERS combined with gas chromatography-tandem mass spectrometry(GC-MS/MS).Pesticide residues from the Hong Kong’s regulation were extract by 1%(v/v)acetonitrile acetate.Then after high-speed homogeneous extraction and purification,internal standard,triphenyl phosphate was added to correct the recovery and the analytes were quantified using matrix-matched standard calibrations as the external standard.The standardcurves of 118 pesticides detected by GC-MS/MS were linear in the range of 0.01~0.20 mg·L^-1,with correlation coefficients were higher than 0.995.The method quantitative limit was less than 0.01 mg·kg^-1 to all the pesticides,and the recoveries were in the rage of 70.1%~116.7%with relative standard deviations(RSD,n=6)were 0.6%~17.7%.87%of the recoveries of all target compounds were between 90%and 110%.This method is suitable for supervising pesticide residues in vegetables supplied to Hong Kong with its advantages of good reproducibility and stability,its quantitative limit meets the requirements for pesticide residue detection in Hong Kong,Macao and around the world.

关 键 词：QUECHERS 气相色谱串联质谱 供港蔬菜 农药残留 香港《规例》 

分 类 号：O657.71[理学—分析化学]