液相色谱-串联质谱法测定何首乌中87种农药残留

doi:10.19803/j.1672-8629.20230085

中国药物警戒 ›› 2023, Vol. 20 ›› Issue (6): 601-608.
DOI: 10.19803/j.1672-8629.20230085

• 何首乌质量安全及药效研究专栏 • 上一篇下一篇

液相色谱-串联质谱法测定何首乌中87种农药残留

刘芫汐, 辜冬琳, 汪祺, 姚令文, 王莹^#, 金红宇, 马双成^*

中国食品药品检定研究院中药民族药检定所,北京 102629

收稿日期:2023-02-16 出版日期:2023-06-15 发布日期:2023-06-15
通讯作者: ^* 马双成,男,研究员·博导,中药民族药物质基础与质量安全评价。E-mail：msc@nifdc.org.cn。^#为共同通信作者。
作者简介:刘芫汐,女,本科,中药分析。
基金资助:
国家自然科学基金资助项目（81973476）

Determination of 87 types of pesticide residues in Polygoni Multiflori Radix by LC-MS/MS

LIU Yuanxi, GU Donglin, WANG Qi, YAO Lingwen, WANG Ying^#, JIN Hongyu, MA Shuangcheng^*

Institute for Control of Chinese Traditional Medicine and Ethnic Medicine, National Institutes for Food and Drug Control, Beijing 102629, China

Received:2023-02-16 Online:2023-06-15 Published:2023-06-15

摘要/Abstract

摘要： 目的建立何首乌中87种农药的液相色谱-串联质谱（LC-MS/MS）测定方法,并应用于53批何首乌样品的农药初步筛查,为何首乌安全性研究提供借鉴。方法样品经乙腈高速匀浆提取,采用LC-MS /MS,基质匹配法进行测定。质谱采用动态多反应监测模式（MRM）采集数据。结果 87种农药及其代谢物共计100个指标线性关系良好,相关系数均大于0.99,加标回收率实验中全部指标回收率在70.4%~107.4%之间,RSD均小于11.40%,符合痕量测定的要求。53批何首乌样品中共检出3种农药,分别为多菌灵、啶虫脒和吡唑醚菌酯,残留量均低于0.01 mg·kg^-1。结论此方法检测指标包括LC-MS/MS检测的绝大多数禁用农药,方法灵敏度高、准确性好,可应用于何首乌中农药残留的筛查检测,可为基质类似中药材的农药残留检测方法提供借鉴参考。

关键词: 何首乌, 多菌灵, 啶虫脒, 吡唑醚菌酯, 农药, 液相色谱-串联质谱法, 基质效应, 多反应监测, 安全性

Abstract: Objective To establish a liquid chromatography-tandem mass spectrometry (LC-MS / MS) method for the determination of 87 types of pesticides and their metabolites in Polygonum Multiflori Radix in order to screen pesticides in 53 batches of samples of Polygonum Multiflori Radix, provide reference for safety study of Polygoni Multiflori Radix. Methods The samples were extracted with acetonitrile via high speed homogenate, concentrated and added with analytical protective agents before being determined with LC-MS/MS. The multi reaction monitoring mode (MRM) was used to collect data, and the blank matrix matching-protective agent standard was adopted for quantitative analysis to increase the accuracy and improve the peak shape. Results The calibration curves of all the targets showed good linearity with correlation coefficients of 0.99. The average recovery of the target compounds ranged from 70.4% to 107.4% at three spike levels, with relative standard deviations less than 11.40%, which met the requirements of trace determination. Carbendazim, acetamiprid and pyrazolidate were detected in 53 batches of samples of Polygonum Multiflori Radix, and the residues were all below 0.01 mg·kg^-1. Conclusion The detection indicators of this method involve the vast majority of banned pesticides detected by LC-MS / MS. This method is highly sensitive and accurate so that it can be applied to the screening and detection of pesticide residues in Polygonum Multiflori Radix, which can provide reference for the detection of pesticide residues in similar Chinese herbal medicines.

Key words: Polygoni Multiflori Radix, carbendazim, acetamiprid, pyraclostrobin, pesticide residues, LC-MS/MS, matrix effect, multi-response monitoring mode(MRM), safety

中图分类号:

R917
R994.11

刘芫汐, 辜冬琳, 汪祺, 姚令文, 王莹, 金红宇, 马双成. 液相色谱-串联质谱法测定何首乌中87种农药残留[J]. 中国药物警戒, 2023, 20(6): 601-608.

LIU Yuanxi, GU Donglin, WANG Qi, YAO Lingwen, WANG Ying, JIN Hongyu, MA Shuangcheng. Determination of 87 types of pesticide residues in Polygoni Multiflori Radix by LC-MS/MS[J]. Chinese Journal of Pharmacovigilance, 2023, 20(6): 601-608.

参考文献

[1] Chinese Pharmacopoeia Commission.Pharmacopoeia of the People’s Republic of China, Volume I (中华人民共和国药典一部)[M]. Beijing: China Medical Science Press, 2020.
[2] WANG Z, ZHONG LY, XIE Y, et al.Research progress on Polygoni Multiflori Radix based on “raw and cooked with different uses” and prediction analysis on quality marker (Q-Marker)[J]. Chinese Traditional and Herbal Drugs(中草药), 2022, 53(3): 882-897.
[3] WAN XF, WANG S, KANG CZ, et al.Chinese medicinal materials industry during the 14th Five-Year Planperiod: trends and development suggestions[J]. China Journal of Chinese Materia Medica(中国中药杂志), 2022, 47(5): 1144-1152.
[4] LI H, CAO S, WANG X, et al.Quality evaluation of heshouwu, a Taoist medicine in Wudang[J]. Experimental and Therapeutic Medicine 2016, 12(4): 2317-2323.
[5] LIANG QP, LIANG YY, GUO JX, et al.Determination of organochlorine pesticide residues in Heshouwu and Zhizi by GC-ECD[J]. Journal of North Pharmacy(北方药学), 2013, 10(8): 8-9.
[6] ZHANG L, LI J, WANG Y, et al.Simultaneous determination of 26 organophosphorus pesticide residues in Radix Polygoni Multiflori Preparata by GC-FPD[J]. Journal of North Pharmacy(北方药学), 2012, 9(12): 2-3.
[7] ZHOU HB, FANG ZJ, YANG LW, et al.Determination of residues of organochlorinated pesticides in polygonum multiflorum by GC-MS with solid-phase extraction[J]. China Pharmacy(中国药房), 2010, 289(19): 1777-1778.
[8] WANG Y, LIU YX, FAN J, et al.Determination of residues of 100 pesticides in Polygoni Multiflori Radix by GC-MS/MS[J]. Mod Chin Med(中国现代中药), 2022, 24(10): 1886-1892.
[9] WANG Y, JIN HY, LI YL, et al.Risk Assessment of exogenous harmful residues in Polygonum multiflorum Thunb. and its correlation with liver injury[J]. Chinese Pharmaceutical Affairs(中国药事), 2022, 36(10): 1134-1146.
[10] Chinese Pharmacopoeia Commission.Pharmacopoeia of the People’s Republic of China, Volume IV (中华人民共和国药典四部)[M]. Beijing: China Medical Science Press, 2020.
[11] National food safety standard—Maximum residue limits for pesticides in food(GB 2763 食品安全国家标准食品中农药最大残留限量)[S]National food safety standard—Maximum residue limits for pesticides in food(GB 2763 食品安全国家标准食品中农药最大残留限量)[S]. Beijing: China Agriculture Press, 2021.
[12] CHEN J, DING WL, CHENG HZ. Medicinal Plant Protection(药用植物保护学)[M]. Beijing: Publishing House of Electronics Industry, 2019.
[13] ZHAO Y.Cultivation and pest control technology of Polygonum multiflorum Thunb.[J]. Scientific breeding(科学种养), 2015(6): 18-21.
[14] XIONG Y, LI C, REN J, et al.Determination of pesticide residues in citri r eticulatae pericarpium by SPE-GC-MS/MS[J]. China Pharmacist(中国药师), 2022, 25(3): 537-543.
[15] ZHAO SM, MENG YL, HAN HL, et al.SPE-GC/MS /MS method for determination 5 triazole pesticide residues in dendrobium officinale[J]. Journal of Guangdong Pharmaceutical University(广东药科大学学报), 2020, 36(2): 210-214.
[16] XIONG Y, LI C, REN J, et al.Determination of 109 pesticide residues in Gynostemma pentaphyllum by SPE-LC-MS/MS and SPE-GC-MS/MS[J]. Central South Pharmacy(中南药学), 2020,18(12): 2044-2049.
[17] YANG JB, WANG Q,WANG XT, et al.Difference analysis of chemical composition of Polygoni Multiflori Radix and Polygoni Multiflori Radix Preparata based on plant metabonomics[J]. Chinese Journal of Pharmacovigilance(中国药物警戒), 2022, 19(6): 5.
[18] CORTESE M, GIGLIOBIANCO MR, MAGNONI F, et al.Compensate for or minimize matrix effects? Strategies for overcoming matrix effects in liquid chromatography-mass spectrometry technique: a tutorial review[J]. Molecules, 2020, 25(13): 3047.

液相色谱-串联质谱法测定何首乌中87种农药残留

Determination of 87 types of pesticide residues in Polygoni Multiflori Radix by LC-MS/MS

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