超高效液相色谱-四极杆/静电场轨道阱高分辨质谱快速检测三七农药残留

High Resolution Mass Spectrometry Method for Screening Pesticide Residues in Panax Notoginseng

目的:利用超高效液相色谱–四级杆/静电场轨道阱高分辨质谱建立三七中农药多残留的检测方法,快速筛查三七中的多种农药残留。方法:建立66种农药的高分辨质谱数据库,样品采用乙腈提取,QuECHERS净化,在Full MS-dd MS^(2)正离子扫描模式下对三七中的66种目标化合物进行检测,然后与数据库中目标化合物信息进行比对,用基质匹配外标法定量。结果:66种农药在0.005~0.5 mg/L质量浓度范围内线性关系良好,相关系数均大于0.99,加标回收率在71.7%~110.3%之间,相对标准偏差为1.2%~6.8%。结论:该方法根据高分辨质谱库进行检索并使用多种特征碎片离子进行确证,具有简便、快速、高效等优点,适用于三七中农药多残留的快速筛查和测定。

Objective:To quickly screen multiple pesticide residues in Panax notoginseng,a method has been established for the determination of pesticide residues in Panax notoginseng by ultra performance liquid chromatography-quadrupole/electrostatic field orbitrap high resolution mass spectrometry(UPLC-Orbitrap HRMS).Methods:A high-resolution mass spectrometry database for 66 pesticides was estab-lished,and the samples were extracted by acetonitrile and purified by QuECHERS.In the Full MS-dd MS^(2) positive ion scanning mode,the target 66 kinds of pesticides in Panax notoginseng were detected,and then compared with database,the matrix-matched external standard method was used for quantification.Results:The 66 pesticide residues shows good linear relations in the ranges of 0.005~0.5 mg/L with good linear cor-relations(R^(2)>0.99).The average recoveries are in the range of 71.7%~110.3%,with relative standard devi-ations(RSDs)of 1.2%~6.8%.Conclusion:This method can realize quick screening according to an accur-ate mass database,and characteristic product ion,with the characteristics of simplicity,speed,and high effi-ciency,which can be used for rapid screening of pesticide residues in Panax notoginseng.