色谱-串联质谱法快速检测平贝母中52种禁用农药残留  

Rapid detection of 52 banned pesticide residues in Fritillaria ussuriensis by chromatography-tandem mass spectrometry

作　　者：刘欣宇 王艳[1] 陈大忠[1] LIU Xinyu;WANG Yan;CHEN Dazhong(Heilongjiang University of Chinese Medicine,Harbin 150000,China)

机构地区：[1]黑龙江中医药大学,哈尔滨150000

出　　处：《化学分析计量》2024年第6期21-28,共8页Chemical Analysis And Meterage

基　　金：黑龙江应用技术研究与开发计划项目(GA19C107)。

摘　　要：建立超高效液相色谱-串联质谱联用及气相色谱-串联质谱联用法测定平贝母中52种禁用农药残留。基于QuEChERS原则的固相萃取法对平贝母样品进行处理,超高效液相色谱-串联质谱联用法采用电喷雾离子源,正离子模式下多反应监测,采用外标法定量;气相色谱-串联质谱联用法采用电子轰击离子源。52种农药的质量浓度在一定范围内与响应值线性关系良好,相关系数均大于0.990,定量限为0.02~0.1 mg/kg。样品平均回收率为75%~120%,测定结果的相对标准偏差为均小于15%。该方法快速、准确检测出平贝母禁用农药残留量,可用用于平贝母质量评价,为平贝母质量安全提供实验依据。Ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)and gas chromatography-tandem mass spectrometry(GC-MS/MS)method were established for the determination of 52 banned pesticide residues in Fritillaria ussuriensis.The solid phase extraction method based on the principle of QuEChERS was used to process the Fritillaria ussuriensis samples.The UPLC-MS/MS method used electrospray ion source,multiple reaction monitoring in positive ion mode,and external standard method for quantification.GC-MS/MS method used electron bombardment ion source.The mass concentration of 52 pesticides had a good linear relationship with the response value in a certain range,the correlation coefficients were all greater than 0.990,and the quantitative limits were 0.02-0.1 mg/kg.The average recovery of the samples was 75%-120%,and the relative standard deviation of the determination results was less than 15%.The method can quickly and accurately detect the banned pesticide residues in Fritillaria ussuriensis,and it can be used for the quality evaluation of Fritillaria ussuriensis,and provide experimental basis for the quality and safety of Fritillaria ussuriensis.

关 键 词：液相色谱-串联质谱法 气相色谱-串联质谱法 平贝母 禁用农药残留 

分 类 号：O657[理学—分析化学]