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中国农学通报

中国农学通报 ›› 2021, Vol. 37 ›› Issue (35): 104-109.doi: 10.11924/j.issn.1000-6850.casb2021-0035

• 食品·营养·检测·安全 • 上一篇    下一篇

加味逍遥片中福美双和代森锰锌残留量气相色谱法的建立

屈浩然1,2(), 卢建秋2, 孙巍3, 王莹1(), 金红宇1(), 马双成1   

  1. 1中国食品药品检定研究院,北京 100050
    2北京中医药大学,北京 100029
    3天士力医药集团股份有限公司,天津 300410
  • 收稿日期:2021-01-12 修回日期:2021-05-18 出版日期:2021-12-15 发布日期:2022-01-07
  • 通讯作者: 王莹,金红宇
  • 作者简介:屈浩然,女,1993年出生,硕士,主要从事中药质量控制研究。通信地址：100050 北京市东城区天坛西里2号 中国食品药品检定研究院,E-mail： 18801377581@163.com。
  • 基金资助:
    国家科技重大专项“重大新药创制”(2018ZX09303-024)

Determination of Thiram and Mancozeb Residues in Jiawei Xiaoyao Tablets by Gas Chromatography

Qu Haoran1,2(), Lu Jianqiu2, Sun Wei3, Wang Ying1(), Jin Hongyu1(), Ma Shuangcheng1   

  1. 1National Institutes for Food and Drug Control, Beijing 100050
    2Beijing University of Chinese Medicine, Beijing 100029
    3Tasly Pharmaceutical Group Co., Ltd., Tianjin 300410
  • Received:2021-01-12 Revised:2021-05-18 Online:2021-12-15 Published:2022-01-07
  • Contact: Wang Ying,Jin Hongyu

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摘要：

为了探究样品中二硫代氨基甲酸酯类农药污染情况及其在加工过程中的转移情况,本研究通过优化样品前处理条件及色谱条件后,建立了测定加味逍遥片中代森锰锌及福美双的残留量的气相色谱-火焰光度(GC-FPD)法。二硫代氨基甲酸酯类农药在含氯化亚锡的盐酸介质中反应生成CS2,采用顶空进样法精密度不佳,且顶空气体中存在高浓度HCl气体会造成气相色谱进样部件腐蚀,故本研究将顶空进样改为溶液进样,使用异辛烷对检测指标进行提取。实验证明此方法在0.02~2.0 μg/mL浓度范围内线性关系良好,相关系数R值大于0.99。在5、20、100 μg/kg三水平进行加样回收率考察,代森锰锌及福美双平均回收率在99%~115%之间,RSD均小于2.0%,符合痕量农药残留的检测要求。对加味逍遥片及其处方中药材、提取物共计36批次进行检测,结果表明样品中CS2残留量符合欧洲药典及中国食品安全标准中相关残留限量规定。本研究建立的加味逍遥片中代森锰锌及福美双的GC检测方法,其灵敏度高,准确、可靠,可用于加味逍遥片及生产中间提取物的农药残留监控。

关键词: 代森锰锌, 福美双, 加味逍遥片, 气相色谱, 农药转移

Abstract:

To investigate the contamination of dithiocarbamate pesticides in the samples and their transfer during the processing, through optimizing pretreatment conditions and chromatographic conditions, this study established a gas chromatography-flame photometry (GC-FPD) method to determine thiram and mancozeb residual quantity in Jiawei Xiaoyao tablets. Dithiocarbamate pesticides reacted to form CS2 in hydrochloric acid medium containing stannous chloride. The precision of headspace injection method was not good, and the presence of high concentration of HCl in headspace gas would cause corrosion of gas chromatography injection components. Therefore, in this study, headspace injection was changed to solution injection, and isooctane was used to extract the detection indexes. The linear range of this method was 0.02-2.0 μg/mL, and the R of correlation coefficient was greater than 0.99. The average recoveries of mancozeb and thiram were 99%-115% at the level of 5, 20, 100 μg/kg, and the RSD of them was less than 2.0%, both met the detection requirements of trace pesticide residues. A total of 36 batches of Jiawei Xiaoyao tablets, and its Chinese herbal medicines and extracts were detected. The results showed that the residues of CS2 in the samples met the relevant residue limits of European Pharmacopoeia and Chinese Food Safety Standards. In this study, a GC method for the determination of mancozeb and thiram in Jiawei Xiaoyao tablets was established, which is sensitive, accurate and reliable, and could be used for the monitoring of pesticide residues in Jiawei Xiaoyao tablets and its intermediates.

Key words: mancozeb, thiram, Jiawei Xiaoyao tablets, gas chromatography, transfer of pesticides

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