QuEChERS-HPLC-MS/MS法同时测定果蔬中21种农药残留  

Determination of 21 sorts of pesticide residues in fruits and vegetables by QuEChERS-HPLC-MS/MS

作　　者：黄何何[1,2] 郑向华[2] 董健[1] 罗佳[1] 严丽娟[2] 王连珠[2] 徐敦明[2] 

机构地区：[1]福建农林大学植物保护学院,福建福州350002 [2]厦门出入境检验检疫局,福建厦门361026

出　　处：《福建农林大学学报（自然科学版）》2013年第4期423-428,共6页Journal of Fujian Agriculture and Forestry University:Natural Science Edition

基　　金：福建省自然科学基金(2011J05029;2011J01386)

摘　　要：建立果蔬21种农药残留的QuEChERS-高效液相色谱—串联质谱(HPLC-MS/MS)同时检测方法.样品经QuEChERS方法提取和净化,以Agilent Extend-C18色谱柱(2.1×100 mm,3.5μm)进行分离,采用电喷雾电离、正离子多反应检测模式检测,外标法定量.21种农药的浓度为0.005-0.500 mg·L-1时,相关系数均>0.9956;磺酰唑草酮和炔草酸检出限(S/N≥3)为4μg·kg-1,定量限(S/N≥10)为12.0μg·kg-1,其它待测物的检出限均为2μg·kg-1,定量限为5μg·kg-1;平均回收率为67.7%-105.1%,相对标准偏差为2.8%-13.2%(n=6).An effective multi-residual method for the trace determination of 21 sorts of pesticide residues in fruits and vegetables was developed by HPLC-MS/MS. Target pesticides in samples were extracted by acetonitrile, purified by developed QuEChERS method, then analyzed using H_PLC-MS/MS under multiple reaction monitoring （MRM） mode with positive electmspray ionization, and Agi- lent Extend-C18 column （2.1 × 100 mm, 3.5 μm） was used as the analytical column. The results showed the 21 pesticides were lin- ear in the range of 0.005 -0.500 mg . L-1 with R2 〉 0.9956. The limits of detection （LODs） and the limits of quantification （LO- Qs） of Sulfentrazone and Clodinafop acid both were 4μg .kg-1 , 12 μg. kg-1, respectively, the others all were 2 μg . kg-1 , 5 μg . kg-1, respectively. The recoveries ranged from 67.7% to 105.1%, with the relative standard deviations （RSDs, n =6） of 2.8% - 13.2%.

关 键 词：QUECHERS 农药多残留 高效液相色谱-串联质谱 果蔬 

分 类 号：O658[理学—分析化学]