超高效液相色谱-串联质谱法快速测定不同石斛中8种农药残留量  

Rapid Detection of 8 Pesticide Residues in Different Dendrobii Caulis by Ultra High Performance Liquid Chromatography-Tandem Mass Spectrometry

作　　者：肖苏萍 钟荣荣 高慧 周朗 王继永 李春[4] 刘慧峰 XIAO Su-ping;ZHONG Rong-rong;GAO Hui;ZHOU Lang;WANG Ji-yong;LI Chun;Liu Hui-feng(China National of Traditional Chinese Medicine Co.,Ltd.,Beijing 100195,China;Beijing Analysis Center,Shimadzu (China) Co.,Ltd.,Beijing 100020,China;Jiangxi University of Traditional Chinese Medicine,Nanchang 330004,China;Institute of Chinese Materia Medica,China Academy of Chinese Medical Sciences,Beijing 100700,China;Zai Lab (Suzhou) Co.,Ltd.,Suzhou 215123,China)

机构地区：[1]中国中药有限公司,北京100195 [2]岛津企业管理(中国)有限公司北京分公司,北京100020 [3]江西中医药大学,江西南昌330004 [4]中国中医科学院中药研究所,北京100700 [5]再鼎医药(苏州)有限公司,江苏苏州215123

出　　处：《中国现代中药》2020年第4期603-608,621,共7页Modern Chinese Medicine

基　　金：北京市科技计划项目(Z171100001717028)。

摘　　要：目的:建立一种采用超高效液相色谱-三重四极杆串联质谱对不同石斛中的常见8种农药残留进行快速检测的方法。方法:不同石斛样品采用1%甲酸乙腈提取,无水硫酸镁、氯化钠盐析后无需净化,采用正离子多反应监测(MRM)模式对不同石斛中的8种农药残留进行测定分析,8种农药在给定的范围内线性关系良好(r>0.999),检出限为0.01~0.12μg·L-1,定量限为0.03~0.41μg·L-1,在3个添加水平下的平均回收率为97.3%~111.6%,RSD为4.22%~8.44%。结果:本方法检测灵敏度高、基质干扰小、稳定性好,能获得较高的回收率,可在较短时间内完成1个样品的定性和定量分析,适用于石斛农药残留安全检测与质量控制。结论:利用本方法检测的39批不同石斛样品中,有2批石斛的多菌灵和戊唑醇超出了石斛的农药最大限量理论值,石斛样品总体农药残留安全控制相对较好,但还需加强各种农药的使用。Objective:The 8 pesticide residues in different Dendrobii Caulis were quickly detected by ultra-high performance liquid chromatography-triple quadrupole tandem mass spectrometry.Methods:The Dendrobii Caulis samples were extracted with acetonitrile solution containing1%formic acid,and the extract was salted out with anhydrous magnesium sulfate and sodium chloride salting.The positive and negative ion multi-reaction monitoring(MRM)model was used to determine and analyze 8 pesticide residues in different Dendrobii Caulis,and 8 pesticides had good linear relationship(r>0.999)in a given range,and the detection limit was 0.01-0.12μg·L-1,quantitative limit of 0.03-0.41μg·L-1,the average recovery rate shown in the 3 additional samples of different volumes and same concentration level was between 97.3-111.6%,while RSD value is between 4.22%-8.44%.Results:Among the 39 different Dendrobii Caulis sample groups detected by this method,2 groups had a higher carbendazium and pentazolol content than the theoretical maximum pesticide limit,and the overall result of the pesticide residue safety control of the samples was relatively good,but the use direction is still to be strenthened.Conclusion:This method is of high detection sensitivity,small matrix interference,good stability,and it can obtain high recovery rate,complete the qualitative and quantitative analysis of a sample in a short time,and it is suitable for safety detection and quality control of pesticide residues in Dendrobii Caulis.

关 键 词：超高效液相色谱-串联质谱 农药残留 石斛 

分 类 号：R284[医药卫生—中药学]