PDF《固相萃取-气相色谱质谱法测定茶叶中 11 种 农药残留量》

第10 卷第5期食品安全质量检测学报Vol.

10 No.

5 2019 年3月Journal of Food Safety and Quality Mar. ,

2019 *通讯作者: 郭红勤, 主管技师, 主要研究方向为食品安全风险检测.E-mail: [email protected] *Corresponding author: GUO Hong-Qin, Chief Technician, Yongzhou Center for Disease Control and Prevention, No. 159, Station Road, Lengshuitan District, Yongzhou 425000, China. E-mail: [email protected] 固相萃取-气相色谱质谱法测定茶叶中

11 种 农药残留量 郭红勤* , 詹磊(永州市疾病预防控制中心, 永州 425000) 摘要: 目的 建立固相萃取-气相色谱质谱联用法测定茶叶中

11 种农药残留量的分析方法.方法 茶叶样 品中的农药残留经丙酮提取, 无水硫酸镁除水, 采用 Carbon/NH2 固相萃取柱在线净化与富集, DB-17MS 毛细 管柱分离检测, 多离子反应模式, 外标法定量.结果 在20~200 mg/L 的浓度范围,

11 种农药残留均与其对应 的峰面积呈线性关系, 方法的检出限(S/N=3)在0.001~0.018 mg/kg 之间. 以空白样品为基体进行加标回收实验, 所得回收率在 72.0%~93.2%之间, 测定值的相对标准偏差(n=6)在2.35%~6.34%之间. 结论 该方法准确度较 高、稳定性较好、检出限低, 适用于茶叶样品中有机磷、氨基甲酸酯、拟除虫菊酯和杀菌剂等多组分农药残 留量的同时测定. 关键词: 固相萃取;

气相色谱仪质谱联用法;

茶叶;

农药残留 Determination of

11 kinds of pesticide residues in tea by solid phase extraction-gas chromatography-mass spectrometry GUO Hong-Qin* , ZHAN Lei (Yongzhou Municipal Center for Disease Control and Prevention, Yongzhou 425000, China) ABSTRACT: Objective To establish a method for the determination of

11 kinds of pesticide residues in tea by solid phase extraction-gas chromatography-mass spectrometry. Methods The pesticide residues in the tea were extracted with acetone, and the water was removed by anhydrous magnesium sulfate. The carbon/NH2 solid phase extraction column was used for on-line purification and enrichment, DB-17MS capillary column for separation detection, with multi-ion reaction mode, and external standard method for quantity. Results In the concentration range of 20~200 mg/L, the

11 kinds of pesticide residues showed a linear relationship with their corresponding peak areas. The detection limit (S/N=3) of the method was between 0.001 mg/kg and 0.018 mg/kg. The blank sample was used as the matrix to carry out the spike recovery test. The recoveries were between 72.0% and 93.2%, and the relative standard deviations of the measured values (n=6) were between 2.35% and 6.34%. Conclusion This method has high accuracy and stability, and has low detection limit, which is suitable for simultaneous determination of multi-component pesticide residues such as organophosphorus, carbamate, pyrethroid and bactericide in tea samples. KEY WORDS: solid phase extraction;

gas chromatography-mass spectrometry;

tea;

pesticide residues 第5期郭红勤, 等: 固相萃取-气相色谱质谱法测定茶叶中

11 种农药残留量

1347 1 引言随着农业产业化的大力发展, 农产品越来越依赖于 激素、抗生素和农药等外源物质.我国的农药在茶叶、蔬菜、水果[1] 、粮食上的用量一直居高不下, 而这些物质的 不合理使用必将导致农产品农药残留超标, 影响消费者的 食用安全, 严重时还会造成消费者生病、发育畸形, 甚至 会导致中毒死亡.近年来茶叶中农药残留问题越来越受到 人们的关注, 茶叶是我们国家的特产, 随着人民生活水平 的提高, 茶文化的兴起, 喝茶已成为我国传统生活的一部 分[2] .而随着茶叶需求量的增加, 人们越来越重视茶叶安 全问题, 对茶叶的品质也有了更高的要求, 其中茶叶的农 药残留问题一直是人们关注的热点[3-5] . 目前国内茶叶生产 中存在农药用量大、次数多、滥用的现象[6] , 例如,