虞淼, 姚芳, 张寒, 王娇, 齐沛沛, 王新全. 液相色谱-串联质谱法测定中药材浙八味中30种有机磷农药残留[J]. 农药学学报, 2022, 24(3): 591-600. DOI: 10.16801/j.issn.1008-7303.2021.0184
    引用本文: 虞淼, 姚芳, 张寒, 王娇, 齐沛沛, 王新全. 液相色谱-串联质谱法测定中药材浙八味中30种有机磷农药残留[J]. 农药学学报, 2022, 24(3): 591-600. DOI: 10.16801/j.issn.1008-7303.2021.0184
    YU Miao, YAO Fang, ZHANG Han, WANG Jiao, QI Peipei, WANG Xinquan. Determination of 30 organophosphorus pesticides in eight traditional Chinese medicine in Zhejiang (Zhebawei) by liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Pesticide Science, 2022, 24(3): 591-600. DOI: 10.16801/j.issn.1008-7303.2021.0184
    Citation: YU Miao, YAO Fang, ZHANG Han, WANG Jiao, QI Peipei, WANG Xinquan. Determination of 30 organophosphorus pesticides in eight traditional Chinese medicine in Zhejiang (Zhebawei) by liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Pesticide Science, 2022, 24(3): 591-600. DOI: 10.16801/j.issn.1008-7303.2021.0184

    液相色谱-串联质谱法测定中药材浙八味中30种有机磷农药残留

    Determination of 30 organophosphorus pesticides in eight traditional Chinese medicine in Zhejiang (Zhebawei) by liquid chromatography-tandem mass spectrometry

    • 摘要: 建立了中药材浙八味中30种有机磷 (OPPs)农药残留的检测方法。针对中草药基质复杂、净化难度大的问题,采用纳米材料二氧化锆 (nano-ZrO2)和介孔分子筛 (MCM-41)作为分散固相萃取 (d-SPE)净化吸附剂,以延胡索为代表基质对净化过程进行优化,采用液相色谱-串联质谱 (LC-MS/MS)进行分析。结果表明:以30 mg nano-ZrO2和50 mg MCM-41为净化吸附剂时,延胡索基质中,除苯腈磷、敌百虫 (0.002~0.25 mg/L)和敌敌畏 (0.005~0.25 mg/L)外,其余27种农药在0.001~0.25 mg/L范围内线性关系良好,相关系数 (r)均大于0.99。方法定量限 (LOQ)除敌敌畏 (0.05 mg/kg)外,均为0.01 mg/kg。8种基质在0.05 mg/kg添加水平下,除倍硫磷和敌敌畏外,其余28种农药平均回收率范围为64 %~125 %,相对标准偏差 (RSDs)在0.05%~11%之间。该方法简单、快速、准确、重现性好,并且在浙八味中有较好的适用性,弥补了浙八味中有机磷农药残留检测技术缺乏的空白。

       

      Abstract: A method for simultaneous determination of 30 organophosphorus pesticides in eight traditional Chinese medicine of Zhejiang (called Zhebawei) was established. Considering the complexity of Chinese herbal medicine and difficulty in purification, nano-ZrO2 and mesoporous molecular sieve MCM-41 were selected as dispersive solid phase extraction (d-SPE) cleanup adsorbents. The cleanup process was systematically optimized with Rhizoma Corydalis as the representative matrix, and combined with liquid chromatography-tandem mass spectrometry (LC-MS/MS) analysis. The results showed that using 30 mg nano-ZrO2 and 50 mg MCM-41 as d-SPE cleanup adsorbents, the linearity for the pesticides was good in the concentration range of 0.001-0.25 mg/L and the correlation coefficient (r) was greater than 0.99, except for cyanofenphos, trichlorphon (0.002-0.25 mg/L) and dichlorvos (0.005-0.25 mg/L). The limit of quantitation (LOQ) was 0.01 mg/kg except for dichlorvos (0.05 mg/kg). Except for fenthion and dichlorvos, the average recoveries of the 28 pesticides in the samples ranged from 64% to 125% at spiking level of 0.05 mg/kg, and the relative standard deviations (RSDs) ranged from 0.05% to 11%. The method is simple, rapid, accurate and reproducible, and has good applicability in the Zhebawei of Zhejiang, which makes up for the lack of detection technology of organophosphorus pesticide residues in the Zhebawei of Zhejiang.

       

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