QuEChERS结合高效液相色谱三重四极杆串联质谱法测定花椒中191种农药残留  

QuEChERS combined with high performance liquid chromatography-triple quadrupole tandem mass spectrometry for the determination of 191 pesticide residues in Zanthoxylum bungeanum Maxim.

作　　者：扈斌 谢瑜杰 蒋康丽 吴兴强[1] 仝凯旋 范春林[1] 王明林[2] 吕美玲[3] 陈辉[1] HU Bin;XIE Yujie;JIANG Kangli;WU Xingqiang;Tong Kaixuan;FAN Chunlin;WANG Minglin;LV Meiling;CHEN Hili(Chinese Academy of Inspection and Quarantine,Beijing 100176;College of Food Science and Engineering,Shandong Agricultural University,Taian 271018;Agilent Technologies(China)Co.,Ltd.,Beijing 100102)

机构地区：[1]中国检验检疫科学研究院,北京100176 [2]山东农业大学食品科学与工程学院,泰安271018 [3]安捷伦科技(中国)有限公司,北京100102

出　　处：《分析试验室》2021年第10期1154-1165,共12页Chinese Journal of Analysis Laboratory

基　　金：国家重点研发计划(2017YFF0211304);中国检科院基本科研业务费项目(2020JK009)资助。

摘　　要：建立了QuEChERS法结合液相色谱-三重四极杆串联质谱法检测花椒中191种农药残留的方法。花椒样品加水浸润后,使用全自动样品制备系统经1%(V/V)乙酸乙腈提取,乙二胺-N-丙基硅烷化硅胶(PSA)、十八烷基硅烷键合硅胶(C18)、ENVI-Carb和Z-Sep+填料净化,ZORBAX SB-C18(100 mm×2.1 mm,3.5μm)色谱柱分离,以0.1%(V/V)甲酸水溶液(含5 mmol/L乙酸铵)-乙腈为流动相进行梯度洗脱,应用高效液相色谱三重四极杆串联质谱(LC-MS/MS)在电喷雾电离正离子模式扫描,在动态多反应监测(DMRM)模式下检测,基质匹配外标法定量分析,实现了花椒样品中191种农药的定量和定性分析。实验表明,191种目标农药在各自线性范围内线性关系良好,线性相关系数(R2)均大于0.995,检出限(LOD)范围为1~5μg/kg,定量限(LOQ)范围为2~20μg/kg,在1倍、2倍和10倍定量限(LOQ)添加水平下,191种农药的回收率范围分别为70.9%~107.6%、70.5%~116.5%和70.9%~119.0%,各添加水平相对标准偏差(RSDs)均<14%。将该方法应用于实际花椒样品的检测中,所有批次均检测出农药残留,适用于花椒中多种农药残留的快速筛查与检测。A method for the determination of 191 pesticide residues in Zanthoxylum bungeanum Maxim. was established by using QuEChERS device combined with high performance liquid chromatography-triple quadrupole tandem mass spectrometry( LC-MS/MS). The samples were extracted by 1%( V/V) acetonitrile acetate using an automatic sample preparation system,purified with primary secondary amine( PSA),octadecylsilane( C18),ENVI-Carb and Z-SEP+. The pesticides were separated on a ZORBAX SB-C18 chromatographic column( 100 mm × 2. 1 mm,3. 5 μm) by gradient elution using 0. 1%( V/V) aqueous acid solution( containing5 mmol/L ammonium acetate)-acetonitrile as mobile phase,analyzed by electrospray LC-MS/MS scanning in positive ionized mode,and detected in the dynamic multiple reaction monitoring( DMRM) mode. The matrix matching external calibration was used for quantitative analysis. The experimental results showed that 191 target pesticides exhibited good linear relationships within their corresponding linear ranges,and the linear correlation coefficients( R2) were greater than 0. 995. The limits of detection( LODs) were in the range of 1-5 μg/kg and the limits of quantification( LOQs) were in the range of 2-20 μg/kg. The recoveries of 191 pesticides were 70. 9%-107. 6%,70. 5%-116. 5% and 70. 9%-119. 0% when spiked at 1,2 and 10 LOQ levels,respectively,with the relative standard deviations( RSDs) less than 14%. The proposed method was applied for the analysis of real samples,and the pesticide residues were detected in all samples,showing the developed method was suitable for the rapid screening and detection of various pesticide residues in Zanthoxylum bungeanum Maxim..

关 键 词：花椒 自动QuEChERS 高效液相色谱串联质谱法 农药残留 

分 类 号：O657.63[理学—分析化学] TS255.7[理学—化学]