气相色谱-负化学源-质谱法测定乌龙茶中拟除虫菊酯和有机氯农药多残留
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(1.广东省疾病预防控制中心,广东 广州 511430;2.华南农业大学资源环境学院, 广东 广州 510642;3.国家食品安全风险评估中心,北京 100021)

作者简介:

朱盼 女 助理研究员 研究方向为食品安全 E-mail:529134125@qq.com

通讯作者:

吴永宁 男 研究员 研究方向为食品安全E-mailwuyongning@ cfsa.net.cn

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基金项目:

广东省自然科学基金(2020A1515010655);广东省医学科研基金(A2017035,C2020010)


Determination of pyrethroids and organochlorine pesticides in oolong tea by gas chromatography-negative chemical ionization-mass spectrometry
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(1.Guangdong Provincial Center for Disease Control and Prevention, Guangdong Guangzhou 511430, China;2.The College of Natural Resources and Environment, South China Agricultural University, Guangdong Guangzhou 510642, China;3.National Center for Food Safety Risk Assessment, Beijing 100021, China)

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    摘要:

    目的 建立一种基于液液萃取-固相萃取-气相色谱-负化学源-质谱(GC-NCI-MS)测定乌龙茶中多组分拟除虫菊酯和有机氯类杀虫剂的分析方法。方法 茶叶样品粉碎过筛后,经沸水浸泡、丙酮-正己烷液液萃取、Carb-NH2固相萃取柱进化后,用GC-NCI-MS方法进行定性、定量分析。结果 18种拟除虫菊酯和9种有机氯类杀虫剂分别在0.006~1.00 μg/mL和0.006~0.50 μg/mL浓度范围内具有良好的线性关系,相关系数(r)均大于0.996,加标回收率为60.1% ~119.8%,相对标准偏差为1.5%~10.4%(n=6),方法检出限和定量限分别为0.5~4.8 μg/kg和1.7~16.0 μg/kg。结论 该方法快速、准确,能满足乌龙茶样品中18种拟除虫菊酯和9种有机氯类杀虫剂残留的快速检测分析要求。

    Abstract:

    Objective To establish a method for the determination of several kinds of pyrethroids and organochlorine pesticides in Chinese oolong tea samples based on liquid-liquid extraction-solid phase extraction-gas chromatography-negative chemical ionization-mass spectrometry (GC-NCI-MS).Methods Oolong tea samples were crushed and screened, soaked in boiling water, extracted with acetone-n-hexane, purified by Carb-NH2 column, and then identified and quantified by GC-NCI-MS.Results All the 18 kinds of pyrethroids and 9 kinds of organochlorine pesticides showed good linear relationships in range of 0.006-1.00 μg/mL and 0.006-0.50 μg/mL respectively, and the correlation coefficients were above 0.996. The recoveries at different spiked levels for all target compounds in blank matrices were 60.1%-119.8%, and the relative standard deviation (RSD) were 1.5%-10.4% (n=6). The limits of detection and quantification of the method were 0.5-4.8 μg/kg and 1.7-16.0 μg/kg, respectively.Conclusion The method was suitable for rapid screening and analysis of 18 pyrethroids and 9 organochlorine pesticides in Chinese oolong tea with the advantage of accuracy, rapidity and high sensitivity.

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朱盼,万欢,吕芬,姚敬,龙朝阳,黄伟雄,吴永宁.气相色谱-负化学源-质谱法测定乌龙茶中拟除虫菊酯和有机氯农药多残留[J].中国食品卫生杂志,2021,33(4):415-422.

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  • 收稿日期:2021-01-12
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  • 在线发布日期: 2021-07-21
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