QuEChERS-液相色谱-串联质谱法测定中草药中22种三唑类农药残留 Translated title: QuEChERS-liquid chromatography-tandem mass spectrometry for determination of 22 triazole pesticide residues in Chinese herbal medicines – ScienceOpen
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      QuEChERS-液相色谱-串联质谱法测定中草药中22种三唑类农药残留 Translated title: QuEChERS-liquid chromatography-tandem mass spectrometry for determination of 22 triazole pesticide residues in Chinese herbal medicines

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          Abstract

          建立了“浙八味”中草药中22种三唑类杀菌剂农药残留的简便、快速和精准分析方法。以白术为代表性基质,对QuEChERS前处理方法进行改良,样品经乙腈萃取后,选取10 mg羧基化多壁碳纳米管和20 mg C18组合作为净化吸附剂,并采用液相色谱-串联质谱进行分析;对建立的方法进行了系统考察,糠菌唑、氟环唑和乙环唑的线性范围为2.5~200 μg/L,其余农药的线性范围为1~200 μg/L,相关系数( R)均大于0.99;在10、20、100和200 μg/kg的添加水平下平均回收率为77.0~115%,相对标准偏差(RSD)均低于9.4%;本方法的检出限为1~2.5 μg/kg,定量限为10~20 μg/kg;通过添加回收试验验证该方法对“浙八味”其他中草药的适用性,目标农药在不同基质中的平均回收率为76.4%~123%, RSD均低于12.2%。利用该方法检测了市售30份“浙八味”中草药中三唑类农药残留,结果显示,浙贝母和杭白菊中有三唑类农药检出,其中浙贝母中均检出苯醚甲环唑,含量为41.4~110 μg/kg,杭白菊中检出苯醚甲环唑、腈菌唑、三唑醇和丙环唑,含量为16.1~250 μg/kg。所建立的方法操作简便快速,方法灵敏度高,重复性好,可满足“浙八味”中三唑类杀菌剂准确定量分析的要求。

          Translated abstract

          Eight well-known herbals in Zhejiang Province, Zhebawei, are commonly used as traditional Chinese herbal medicines owing to their rich active ingredients. However, the unavoidable use of pesticides during agricultural production has led to pesticide residue problems in these herbs. In this study, a simple, rapid, and accurate method was established to determine 22 triazole pesticide residues in Zhebawei. An improved QuEChERS method was used for sample pretreatment, and Rhizoma Atractylodis Macrocephalae was used as a representative sample. The sample was extracted with acetonitrile to eliminate some polar and nonpolar compounds, pigments, and other impurities, and the purification effects of multiwalled carbon nanotubes (MWCNTs), amino-modified multiwalled carbon nanotubes (MWCNTs-NH 2), carboxylated multiwalled carbon nanotubes (MWCNTs-COOH), crosslinked polyvinylpyrrolidone (PVPP), zirconium dioxide (ZrO 2), 3-( N, N-diethylamino)-propyltrimethoxysilane (PSA), octadecyl (C18), and graphitized carbon black (GCB) were compared. MWCNTs-COOH and C18 were selected as the purification adsorbents, and their dosages were systematically optimized. The combination of 10 mg of MWCNTs-COOH and 20 mg of C18 was eventually selected as the purification adsorbents. Liquid chromatography-tandem mass spectrometry (LC-MS/MS) was used for analysis, and box graphs were plotted to present the dispersion of each group of recoveries, thus enabling the identification of the data outliers, dispersion distribution, and data symmetry. The established method was systematically verified and showed good linearity over the concentration range of 1-200 μg/L (except for bromuconazole, epoxiconazole, and etaconazole) with correlation coefficients >0.99. The average recoveries of the 22 pesticides at spiked levels of 10, 20, 100, and 200 μg/kg were in the range of 77.0%-115% with relative standard deviations (RSDs) <9.4%. The limits of detection and quantification were 1-2.5 μg/kg and 10-20 μg/kg, respectively. The applicability of the developed method to other herbals was investigated at 100 μg/kg, and the average recoveries of the target pesticides in different matrices ranged from 76.4% to 123% with RSDs <12.2%. Finally, the method established was used to detect triazole pesticide residues in 30 actual Zhebawei samples. The results showed that triazole pesticides were present in Bulbus Fritillariae Thunbergii and Dendranthema Morifolium. Difenoconazole was detected in Bulbus Fritillariae Thunbergii at contents ranging from 41.4 μg/kg to 110 μg/kg, while difenoconazole, myclobutanil, triadimenol and propiconazole were detected in Dendranthema Morifolium at contents ranging from 16.1 μg/kg to 250 μg/kg. The established method can meet the requirements for the accurate quantitative analysis of triazole fungicides in Zhebawei.

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          Author and article information

          Contributors
          Journal
          Se Pu
          Se Pu
          Chinese Journal of Chromatography
          Editorial board of Chinese Journal of Chromatography (No. 457, Zhongshan Road, Shahekou District, Dalian City, Liaoning Province(116023) )
          1000-8713
          1872-2059
          8 April 2023
          : 41
          : 4
          : 330-338
          Affiliations
          [1] 省部共建农产品质量安全危害因子与风险防控国家重点实验室, 浙江省农业科学院农产品质量安全与营养研究所, 浙江 杭州 310021 State Key Laboratory for Managing Biotic and Chemical Threats to the Quality and Safety of Agro-products, Institute of Agro-product Safety and Nutrition, Zhejiang Academy of Agricultural Sciences, Hangzhou 310021, China
          Author notes
          *Tel:(0571)86419076,E-mail: qipeipei@ 123456zaas.ac.cn .
          [#]

          共同第一作者.

          Article
          10.3724/SP.J.1123.2022.08005
          10071351
          37005920
          bf2b81d5-b32d-4856-952f-65aa1820b126
          Copyright @ 2023

          本文是开放获取文章,遵循CC BY 4.0协议

          This is an open access article distributed under the terms of the Creative Commons Attribution License, which permits unrestricted use, distribution, and reproduction in any medium, provided the original author and source are credited.

          History
          : 8 August 2022
          Funding
          Funded by: 浙江省重点研发计划项目
          Funded by: Key Research and Development Program of Zhejiang Province
          Award ID: 2020C02023
          Categories
          Articles
          O658
          a

          液相色谱-串联质谱法,三唑类农药残留,浙八味,中草药,羧基化多壁碳纳米管,liquid chromatography-tandem mass spectrometry (lc-ms/ms),triazole pesticide residues,zhebawei,chinese herbal medicines,carboxylated multi-wall carbon nanotubes

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