中国中药杂志

2019, v.44(15) 3287-3296

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金银花配方颗粒中农药多残留筛查研究
Screening of multiple pesticide residues in Jinyinhua Formula Granules

王赵;金红宇;李耀磊;李静;许玮仪;马双成;
WANG Zhao;JIN Hong-yu;LI Yao-lei;LI Jing;XU Wei-yi;MA Shuang-cheng;National Institutes for Food and Drug Control;

摘要(Abstract):

为初步评估市场流通使用的金银花配方颗粒农药残留风险,结合金银花配方颗粒国家药品评价性抽验项目,随机抽取5个企业20批次样品,选择目前对中药材有监测意义的262种农药,总计270个化学单体,对其进行农药多残留筛查。样品采用乙腈为溶媒,高速匀浆法提取,针对拟定的检测指标,分别采用气相串联质谱(GC-MS/MS)和高效液相串联质谱(LCMS/MS),以多反应监测(MRM)模式进行检测,以不少于2组特征离子对进行定性,并针对有检出的农药,以校准曲线法进行定量检测。20批金银花配方颗粒样品中检出农药数量达到20种,平均每批检出农药约9种,但没有禁限用农药检出,且检出农药均处于痕量水平,远低于一般食品标准中的农药残留限量要求。因此,金银花配方颗粒中农药残留安全风险较小。该研究首次建立了金银花配方颗粒中农药多残留筛查方法,方法准确、快速,检测指标针对性强,且通过对筛查结果的分析可为金银花配方颗粒乃至中药配方颗粒中农药安全风险的防控提供理论参考。
To evaluate the pesticide residue risk of Jinyinhua Formula Granules( made from Lonicerae Japonicae Flos) used in the market preliminarily,20 samples of Jinyinhua Formula Granules from 5 manufactures were collected randomly through the national evaluative sampling test program. Totally 262 pesticides( involving 270 chemical monomers) with monitoring significance to traditional Chinese medicinal materials were detected. Samples were extracted by high speed homogenate with acetonitrile as solvent. And their residues were analyzed by GC-MS/MS and LC-MS/MS in MRM mode. No less than 2 groups of characteristic ion pairs were adopted for qualitative detection,and the calibration curve method was used for quantitative detection. The results showed that 20 pesticides were detected in 20 batches of Jinyinhua Formula Granules,with an average of about 9 pesticides detected in every batch,but no restricted pesticide was detected. The detected pesticides were all at the trace level,which was far lower than the limit of the general food standard. Therefore,the safety risk was low in Jinyinhua Formula Granules. In this study,a screening method for pesticide residues in Jinyinhua Formula Granules was established for the first time. The method was accurate and rapid,and the detection indicators were highly targeted. The results could provide theoretical reference for the prevention and control of pesticide safety risks in Jinyinhua Formula Granules and even traditional Chinese medicine formula granules.

关键词(KeyWords): 金银花;配方颗粒;农药多残留;气相色谱串联质谱法;液相色谱串联质谱法;安全风险
Lonicerae Japonicae Flos;formula granules;multiple pesticide residues;gas chromatography tandem mass spectrometry;liquid chromatography tandem mass spectrometry;safety risks

Abstract:

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基金项目(Foundation): 国家药典委员会药品医疗器械审评审批制度改革项目(ZG2016-2-01)

作者(Author): 王赵;金红宇;李耀磊;李静;许玮仪;马双成;
WANG Zhao;JIN Hong-yu;LI Yao-lei;LI Jing;XU Wei-yi;MA Shuang-cheng;National Institutes for Food and Drug Control;

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