QuEChERS/UPLC-MS/MS法测定雷公藤及根际土壤中3种农药残留
CSTR:
作者:
作者单位:

1.华中农业大学植物科学技术学院,武汉 430070;2.华润三九(黄石)药业有限公司,黄石 435000;3.国药集团中联药业有限公司,武汉 430070

作者简介:

李凤凤, E-mail:lifengfeng@mail.hzau.edu.cn

通讯作者:

舒少华, E-mail:shushaohua@mail.hzau.edu.cn

中图分类号:

S481+.8

基金项目:

华润三九(黄石)药业有限公司资助项目;“十三五”重点研发计划中药现代化专项(2017YFC1700700)


Determining three pesticide residues content in Tripterygium wilfordii root and its rhizosphere soil with QuEChER/UPLC-MS/MS method
Author:
Affiliation:

1.College of Plant Science and Technology, Huazhong Agricultural University,Wuhan 430070,China;2.China Resources Sanjiu (Huangshi) Pharmaceutical Co.,Ltd,Huangshi 435000,China;3.Sinopharm Zhonglian Pharmaceutical Co.,Ltd,Wuhan 430070,China

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    摘要:

    为建立雷公藤种植过程中常用农药的残留含量检测方法,采用快速样品前处理结合超高效液相色谱-串联质谱法(quick,easy, cheap,effective,rugged and safe/ultra performance liquid chromatography tandem mass spectrometry,QuEChERS/UPLC-MS/MS)测定雷公藤及根际土壤中辛硫磷、氯氰菊酯和乙基多杀菌素的含量。样品中加入适量的水浸润后用乙腈超声提取,N-丙基乙二胺(PSA)吸附净化,利用优化后的UPLC-MS/MS方法进行检测,基质外标法定量。结果显示,3种农药在根样基质中的检出限(LOD)为0.001~0.714 μg/kg,定量限(LOQ)为0.002~2.380 μg/kg;在土壤基质中的检出限(LOD)为0.002~0.810 μg/kg,定量限(LOQ)为0.006~2.410 μg/kg。线性关系、回收率和相对标准偏差均符合农药残留检测的相关规定。结果表明,该方法能满足雷公藤及根际土壤中3种农药残留含量的快速检测要求。

    Abstract:

    QuEChERS pretreatment combined with ultra performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS) method was developed and used to determine pesticide residues including phoxim,cypermethrin and spinetoram in T. wilfordii root and its rhizosphere soil to establish the method for detecting the content of three pesticide residues commonly used in the process of planting Tripterygium wilfordii. The sample was soaked with appropriate amount of water and then extracted by acetonitrile ultrasonic,purified by N-propyl ethylenediamine (PSA) adsorption,detected by optimized UPLC-MS/MS method,and quantified by matrix external standard method. The results showed that the detection limit of pesticides in root like matrix was 0.001-0.714 μg/kg,LOQ was 0.002-2.380 μg/kg。The limit of detection (LOD) of three pesticides in root and soil samples was 0.001-0.714 μg/kg and 0.002-0.810 μg/kg,respectively. The limit of quantitation (LOQ) of three pesticides in root and soil samples was 0.002-2.380 μg/kg and 0.006-2.410 μg/kg,respectively. The linear relationship,recovery rate and relative standard deviation were in line with the relevant provisions of detecting pesticide residue. It is indicated that the method established is simple,rapid,sensitive and accurate,and can meet the requirements of rapidly determining three pesticide residues in Tripterygium wilfordii and rhizosphere related soil.

    参考文献
    [1] LI X X,DU F Y,LIU H X,et al.Investigation of the active components in Tripterygium wilfordii leading to its acute hepatotoxicty and nephrotoxicity[J].Journal of ethnopharmacology,2015,162:238-243.
    [2] 简应权,张金霞,王文章,等.雷公藤主要虫害综合防治技术[J].现代农业科技,2018(9):153-154.JIAN Y Q,ZHANG J X,WANG W Z,et al.Integrated control techniques of main pests of Tripterygium wilfordii[J].Modern agricultural science and technology,2018(9):153-154(in Chinese).
    [3] ELERSEK T, FILIPIC M. Organophosphorus pesicides-mechanisma of their toxicity[M]//STOYTCHEVA M. Pesticides:the impacts of pesticides exposure. Oxford, UK: Blackwell Pub Professional,2011: 243-268.
    [4] 李增鑫,李亮,朱坤淼,等.华中地区稻纵卷叶螟对7种杀虫剂的敏感性监测[J].华中农业大学学报,2021,40(2):130-141.LI Z X,LI L,ZHU K M,et al.Susceptibility monitoring of Cnaphalocrocis medinalis Guenée to seven insecticides in central China[J].Journal of Huazhong Agricultural University, 2021,40(2): 130-141(in Chinese with English abstract).
    [5] 姜波,彭楠,武迪,等.拟除虫菊酯类农药引起脑组织氧化应激反应的研究进展[J].毒理学杂志,2020,34(6):511-513.JIANG B,PENG N,WU D,et al.Research progress of pyrethroid pesticides induced oxidative stress in brain tissue[J].Journal of toxicology,2020,34(6):511-513(in Chinese).
    [6] 王珂慧,郭超,刘艳丽,等.多杀菌素类杀虫剂的应用及其抗性研究进展[J].世界农药,2022,44(2):18-24.WANG K H,GUO C,LIU Y L,et al.Research progress on application and resistance of spinosyn insecticides[J].World pesticide,2022,44(2):18-24(in Chinese with English abstract).
    [7] 任理雪,邓高琼,龙婉君,等.中药材中常见农药残留及其研究进展[J].中国中药杂志,2022,47(11):2899-2908.REN L X,DENG G Q,LONG W J,et al.Research progress on common pesticide residues in Chinese medicinal materials[J].China journal of Chinese materia medica,2022,47(11):2899-2908(in Chinese with English abstract).
    [8] 王迪,俞佳,詹固,等.液质联用技术在中药研究中的应用进展[J].中华中医药学刊,2022,40(2):68-71.WANG D,YU J,ZHAN G,et al.Advances in application of liquid chromatography-mass spectrometry technology in study of traditional Chinese medicine[J].Chinese archives of traditional Chinese medicine,2022,40(2):68-71(in Chinese with English abstract).
    [9] ANASTASSIADES M,LEHOTAY S J,?TAJNBAHER D,et al.Fast and easy multiresidue method employing acetonitrile extraction/partitioning and “dispersive solid-phase extraction” for the determination of pesticide residues in produce[J].Journal of aoac international,2019,86(2):412-431.
    [10] LEHOTAY S J,KOK A D,HIEMSTRA M,et al.Validation of a fast and easy method for the determination of residues from 229 pesticides in fruits and vegetables using gas and liquid chromatography and mass spectrometric detection[J].Journal of aoac international,2019,88(2):595-614.
    [11] PERESTRELO R,SILVA P,PORTO-FIGUEIRA P,et al.QuEChERS-fundamentals,relevant improvements,applications and future trends[J].Analytica chimica acta,2019,1070:1-28.
    [12] KOESUKWIWAT U,LEHOTAY S J,MASTOVSKA K,et al.Extension of the QuEChERS method for pesticide residues in cereals to flaxseeds,peanuts,and doughs[J].Journal of agricultural and food chemistry,2010,58(10):5950-5958.
    [13] MASTOVSKA K,DORWEILER K J,LEHOTAY S J,et al.Pesticide multiresidue analysis in cereal grains using modified QuEChERS method combined with automated direct sample introduction GC-TOFMS and UPLC-MS/MS techniques[J].Journal of agricultural and food chemistry,2010,58(10):5959-5972.
    [14] LIU Y Q,LI X Y,ZHOU C,et al.Toxicity of nine insecticides on four natural enemies of Spodoptera exigua[J/OL].Scientific reports,2016,6:390601[2022-09-16].https://doi.org/10.1038/s41598-022-20779-3.
    [15] 张治科,李少南,张蓉,等.辛硫磷在宁夏甘草及对应根际土壤中的残留及消解动态[J].西北农业学报,2010,19(2):52-56.ZHANG Z K,LI S N,ZHANG R,et al.Residues and degradation dynamics of phoxim in Glycyrrhiza uralensis and rhizospheric soil in Ningxia[J].Acta agriculturae boreali-occidentalis sinica,2010,19(2):52-56(in Chinese with English abstract).
    [16] 杨红兵,鲁立良,王自军.枸杞中拟除虫菊酯农药残留量的检测研究[J].时珍国医国药,2008,19(4):846-847.YANG H B,LU L L,WANG Z J.Studies on the determination of pyrethroids in Fructus lycii[J].Lishizhen medicine and materia medica research,2008,19(4):846-847(in Chinese with English abstract).
    [17] 牛艳,杨静,冶海雄,等.枸杞中乙基多杀菌素及其代谢物的检测方法[J].农药,2019,58(11):828-830.NIU Y,YANG J,YE H X,et al.Detection method of spinetoram and its metabolites in Lycium fruit[J].Agrochemicals,2019,58(11):828-830(in Chinese with English abstract).
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李凤凤,张毅鹏,龚达林,刘三波,黄麒元,梅之南,王学奎,舒少华. QuEChERS/UPLC-MS/MS法测定雷公藤及根际土壤中3种农药残留[J].华中农业大学学报,2023,42(1):205-211

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  • 收稿日期:2022-09-16
  • 在线发布日期: 2023-02-22
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