湖北农业科学 ›› 2019, Vol. 58 ›› Issue (23): 176-181.doi: 10.14088/j.cnki.issn0439-8114.2019.23.044

• 检测分析 • 上一篇    下一篇

QuEChERS法与传统固相萃取法对比检测茶叶中25种农药残留

卢森华1, 梁爽2, 黎强1, 陈宇1, 庞小莲1, 钟盈盈1, 唐明华1   

  1. 1.玉林市食品药品检验检测中心,广西 玉林 537000;
    2.广西中医药大学药学院,南宁 530001
  • 收稿日期:2019-01-07 出版日期:2019-12-10 发布日期:2019-12-18
  • 通讯作者: 黎 强(1974-),男,副主任药师,主要从事食品药品分析与实验室质量管理工作,电子信箱)527099595@qq.com。
  • 作者简介:卢森华(1985-),男,广西北流人,主管药师,硕士,主要从事食品药品检验与实验室质量管理工作,(电话)18077585685(电子信箱)185143773@qq.com
  • 基金资助:
    广西高校中青年教师基础能力提升项目(P18037); 玉林市科学研究与技术开发计划项目(玉市科201934034)

Determination of 25 pesticide residues in tea by QuEChERS and SPE

LU Sen-hua1, LIANG Shuang2, LI Qiang1, CHEN Yu1, PANG Xiao-lian1, ZHONG Ying-ying1, TANG Ming-hua1   

  1. 1.Yulin Center for Food and Drug Control,Yulin 537000,Guangxi,China;
    2.Guangxi University of Chinese Medicine,Nanning 530001,China
  • Received:2019-01-07 Online:2019-12-10 Published:2019-12-18

摘要: 通过对比QuEChERS法与传统固相萃取(SPE)法,建立了气相色谱-串联质谱法检测茶叶中25种农药高通量定量检测方法。试验考察了QuEChERS法和SPE法中影响提取和净化效果的各个因素,同时对二者的基质效应进行了分析。QuEChERS法中25种农药在33.33~333.3 ng/mL线性关系良好,相关系数均大于0.990,方法的检出限为0.04~3.00 μg/kg,回收率为74.99%~104.71%,RSD为0.4%~9.0%;SPE法中25种农药在25.0~300.0 ng/mL线性关系良好,相关系数均大于0.990,方法的检出限为0.004~0.300 μg/kg,回收率为62.90%~104.04%,RSD为0.2%~6.4%。2种方法的灵敏度和精密度差异不显著,均符合农药残留分析要求,但SPE法较QuEChERS法基质效应小、净化相对彻底,QuEChERS法较SPE法操作简单、检测快速。2种方法均能对茶叶样品进行农药高通量定量检测,确保在食品安全国家标准设定的MRL水平上对茶叶中的农药残留进行检测。

关键词: 固相萃取, QuEChERS, 茶叶, 气相色谱-串联质谱, 农药残留

Abstract: A high-throughput quantitative method for the determination of 25 pesticides in tea by GC-MS/MS was established by comparing the QuEChERS method with the traditional SPE method. The factors influencing the extraction and purification effect of QuEChERS and SPE were investigated, and the matrix effect of them was analyzed. The linear relationship of 25 pesticides in the concentration range of 33.33~333.3 ng/mL was good, the correlation coefficient was>0.990, the detection limit of the method was 0.04~3.00 μg/kg, the recovery was 74.99%~104.71%, and the corresponding RSD was 0.4%~9.0%; the linear relationship of 25 pesticides in SPE was good in the concentration range of 25.0~300.0 ng/mL, the correlation coefficient was>0.990, the detection limit of the method was 0.004~0.300 μg/kg. The recovery was 62.90%~104.04%, and the corresponding RSD was 0.2%~6.4%. There was no significant difference in sensitivity and precision between the two methods, which met the requirements of pesticide residue analysis. However, the matrix effect of SPE method is smaller than that of QuEChERS method, and the purification is relatively thorough. Compared with SPE method, QuEChERS method is simpler in operation and faster in detection. Both of the two methods can be used for high-throughput quantitative detection of pesticides in tea samples to ensure reliable control of pesticide residues in tea at the MRL level set by the national food safety standard.

Key words: SPE, QuEChERS, tea, GC-MS/MS, pesticide residues

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