自动QuEChERS结合液相色谱-串联质谱法测定香叶中的212种农药残留  

Detection of 212 kinds of pesticide residues in Laurus nobilis by automatic QuEChERS combined with liquid chromatography-tandem mass spectrometry

作　　者：扈斌 蒋康丽 连思雨 崔宗岩 范春林[2] 王明林[1] 陈辉[2] 连玉晶[1] 吕美玲[4] 王雯雯[4] HU Bin;JIANG Kang-Li;LIAN Si-Yu;CUI Zong-Yan;FAN Chun-Lin;WANG Ming-Lin;CHEN Hui;LIAN Yu-Jing;LV Mei-Ling;WANG Wen-Wen(College of Food Science and Engineering,Shandong Agricultural University,Taian 271018,China;Chinese Academy of Inspection and Quarantine,Beijing 100176,China;Technology Center of Qinhuangdao Customs,Qinhuangdao 066004,China;Agilent Technologies(China)Limited,Beijing 100102,China)

机构地区：[1]山东农业大学食品科学与工程学院,泰安271018 [2]中国检验检疫科学研究院农产品安全研究中心,北京100176 [3]秦皇岛海关技术中心,秦皇岛066004 [4]安捷伦科技(中国)有限公司,北京100102

出　　处：《食品安全质量检测学报》2022年第4期1114-1122,共9页Journal of Food Safety and Quality

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

摘　　要：目的 建立自动QuEChERS结合液相色谱-三重四极杆串联质谱法测定香叶中212种农药残留。方法 香叶样品用乙腈提取,使用300 mg十八烷基硅烷键合硅胶(C_(18))+75 mg Nano-Carb、4.0 g无水硫酸镁和1.0g氯化钠进行净化,经自动样品制备系统进行制备后,应用液相色谱-三重四极杆串联质谱法进行检测,在电喷雾电离正离子模式下扫描,动态多反应监测(dynamic multiple reaction monitoring, DMRM)模式下检测,基质匹配外标法定量分析。结果 212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(γ^(2))均大于0.995,检出限(limits of detection, LODs)范围为1-5μg/kg,定量限(limits of quantitation, LOQs)范围为2-20μg/kg,在10、50和100μg/kg的添加水平,212种农药的平均回收率范围分别为70.35%-112.49%、70.30%-107.02%和72.39%-95.87%,相对标准偏差均小于14.1%。结论 该方法快速、准确、灵敏度高,能够应用于香叶中多农药残留的高通量定性筛查和准确定量,并可扩展到其他香辛料多农药残留检测中。Objective To establish a method for the detection of 212 kinds of pesticide residues in Laurus nobilis by automatic QuEChERS method combined with liquid chromatography-triple quadrupole tandem mass spectrometry.Methods Laurus nobilis samples were extracted by acetonitrile, purified with 300 mg C_(18)+75 mg Nano-Carb, 4.0 mg anhydrous magnesium sulfate and 1.0 g sodium chloride. Then the samples were prepared by automatic extraction equipment, detected by liquid chromatography-triple quadrupole tandem mass spectrometry, scanned in electrospray ionized ion mode, and quantified by matrix matching external standard method with the dynamic multiple reaction monitoring(DMRM) mode. Results Two hundred and twelve kinds of target pesticides exhibited great linear relationships within their respective linear ranges, and linear correlation coefficients(γ^(2)) were all 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, at 10, 50 and 100 μg/kg addition levels, the recoveries of 212 kinds of pesticides were 70.4%-112.5%,70.3%-107.0% and 72.4%-95.9%, respectively, the relative standard deviations(RSDs) were all less than 14.1%.Conclusion This method is fast, accurate and sensitive, can be applied to the high-throughput qualitative screening and accurate quantification of multi-pesticide residues in Laurus nobilis, and can be extended to the high-throughput screening of multi-pesticide residues in other spices.

关 键 词：自动QuEChERS 香叶 农药残留 液相色谱-三重四极杆串联质谱法 

分 类 号：TS264.3[轻工技术与工程—发酵工程] O657.63[轻工技术与工程—食品科学与工程]