GC-MS/MS法快速测定党参等中药中3种拟除虫菊酯类农药残留的方法学研究  

Determination of 3 pyrethroid residues in 5 kinds of traditional Chinese medicines including codonopsis by GC-MS/MS

作　　者：张乐 于生兰[1] 秦枫[1] 徐加兵 高岭梅 杨海峰[1] 谢恺舟[3] 仇雅静 ZHANG Le;YU Shenglan;QIN Feng;XU Jiabing;GAO Lingmei;YANG Haifeng;XIE Kaizhou;QIU Yajing(Jiangsu Key Laboratory of Veterinary Biopharmaceutical High Technology Research/Jiangsu Agri-Animal Husbandry Vocational College,Taizhou 225300,China;Taizhou Drug Inspection Institute,Taizhou 225300,China;College of Animal Science and Technology,Yangzhou University,Yangzhou 225009,China)

机构地区：[1]江苏农牧科技职业学院/江苏省兽用生物制药高技术研究重点实验室,江苏泰州225300 [2]泰州市药品检验院,江苏泰州225300 [3]扬州大学动物科技学院,江苏扬州225009

出　　处：《扬州大学学报（农业与生命科学版）》2023年第1期132-138,共7页Journal of Yangzhou University：Agricultural and Life Science Edition

基　　金：国家现代农业产业技术体系专项(CARS-41);江苏省高等学校自然科学基金面上项目(19KJB360005);江苏省大学生创新创业项目(202112806066H);江苏农牧科技职业学院动物药品科技创新团队项目(NSF2021TC02)。

摘　　要：通过对比气相色谱法(GC)和气相色谱-串联质谱(GC-MS/MS)联用2种检测技术,建立党参、黄芪等5种中药中常见的联苯菊酯、甲氰菊酯和氯氟氰菊酯3种拟除虫菊酯类农药残留量的检测方法。结果表明:在与GC-MS/MS法同一样品浓度下,采用配置ECD检测器的GC法检测信号强度较弱,无法在较低浓度下进行农药残留量的定量分析;而通过GC-MS/MS法,以联苯菊酯、甲氰菊酯和氯氟氰菊酯含量测定为研究目标,通过MRM模式在线检测,优化GC-MS/MS检测条件,具有较好的信号强度,可采用外标法进行含量测定。线性范围在1.95~21.79 ng·g^(-1)之间,线性关系良好,最低检出限为0.25~0.50 ng·g^(-1),定量限为0.84~1.67 ng·g^(-1),决定系数R2为0.987 5~0.998 1, 5种中药的加标回收率为87.45%~92.82%,精密度为3.08%~4.78%,相对标准偏差为5.53%~6.41%。综上,GC-MS/MS方法具有灵敏度高、操作快捷、定性定量准确,可用于5种药食同源中药中3种拟除虫菊酯类农药残留的检测。In order to establish a method for the determination of pyrethroid pesticide residues such as bifenthrin, fenpropathrin and cypermethrin in five traditional Chinese medicines such as Codonopsis pilosula and Astragalus propinquus, two detection techniques were compared by gas chromatography(GC) and gas chromatography tandem mass spectrometry(GC-MS/MS). The results showed that the detection signal intensity of GC equipped with ECD detector was weak at the same sample concentration as that of GC-MS/MS, so it was impossible to quantitatively analyze pesticide residues at low concentration. Through the GC-MS/MS method, taking the content determination of bifenthrin, fenpropathrin and cypermethrin as the research goal, through the online detection of MRM mode, the detection conditions of GC-MS/MS were optimized, which had good signal strength, and the external standard method can be used for the content determination. The linear range was 1.95-21.79 ng·g^(-1). The linear relationship was good. The minimum detection limit was 0.25-0.50 ng·g^(-1), the quantitative limit was 0.84-1.67 ng·g^(-1), and the correlation coefficient R~2 was 0.987 5-0.998 1. The spiked recoveries of the five traditional Chinese medicines were 87.45%-92.82%, the precision was 3.08%-4.78%,and the relative standard deviation was 5.53%-6.41%.In conclusion,GC-MS/MS method has high sensitivity,fast operation and accurate qualitative and quantitative.It can be applied to the detection of three pyrethroid pesticide residues in five traditional Chinese medicines with homologous food and medicine.

关 键 词：中草药 气相色谱-串联质谱联用技术 拟除虫菊酯类农药 农药残留检测 

分 类 号：S567.9[农业科学—中草药栽培]