湖北农业科学 ›› 2024, Vol. 63 ›› Issue (9): 180-184.doi: 10.14088/j.cnki.issn0439-8114.2024.09.030

• 检测分析 • 上一篇    下一篇

QuEChERS法结合高效液相色谱-串联质谱法检测啤酒中10种氨基甲酸酯类农药残留

常晨阳1,2, 王晓3, 单娇4, 李晓明1   

  1. 1.济南海关技术中心,济南 250002;
    2.聊城海关,山东 聊城 252000;
    3.枣庄海关,山东 枣庄 277000;
    4.黄岛海关,山东 青岛 266000
  • 收稿日期:2022-11-18 出版日期:2024-09-25 发布日期:2024-09-30
  • 通讯作者: 李晓明(1982-),男,山东莱西人,高级工程师,主要从事品安全分析与质量体系研究,(电子信箱)isotope@yeah.net。
  • 作者简介:常晨阳(1988-),女,山东东阿人,高级工程师,硕士,主要从事食品安全分析与检测研究,(电话)0635-6023678(电子信箱)changcy2015@139.com。
  • 基金资助:
    海关总署科研项目(2020HK200)

QuEChERS method combined with high performance liquid chromatography tandem mass spectrometry for detecting residues of 10 carbamate pesticides in beer

CHANG Chen-yang1,2, WANG Xiao3, SHAN Jiao4, LI Xiao-ming1   

  1. 1. Technology Center of Jinan Customs District,Jinan 250002, China;
    2. Liaocheng Customs, Liaocheng 252000, Shandong, China;
    3. Zaozhuang Customs,Zaozhuang 277000, Shandong, China;
    4. Huangdao Customs, Qingdao 266000, Shandong, China
  • Received:2022-11-18 Published:2024-09-25 Online:2024-09-30

摘要: 为建立QuEChERS-高效液相色谱-串联质谱法同时测定啤酒中10种氨基甲酸酯类农药残留,啤酒样品通过乙腈提取,1.5 g氯化钠盐析分层,净化剂为30 mg PSA+15 mg GCB+885 mg无水硫酸镁,流动相A为0.01%甲酸水溶液+2 mmol/L甲酸铵溶液、流动相B为甲醇,色谱柱为Shim-pack GIST-HP C18-AQ(100 mm×2.1 mm,1.9 μm),在多反应监测模式(MRM)下进行分析,外标法定量。结果表明,10种氨基甲酸酯类农药在5~150 μg/L浓度范围内线性关系良好,相关系数(R2)均>0.999 0,LOD为0.10~1.43 μg/L,LOQ为0.29~4.76 μg/L, 样品的加标回收率为85.9%~118.0%,RSD为1.4%~8.8%(n=6)。该方法定量准确、操作简单、分析快速,适用于啤酒中多种氨基甲酸酯类农药残留的快速筛查与定量分析。

关键词: 啤酒, QuEChERS法, 高效液相色谱-串联质谱法, 氨基甲酸酯类农药, 残留

Abstract: To establish a QuEChERS high-performance liquid chromatography tandem mass spectrometry method for simultaneous determination of 10 carbamate pesticide residues in beer,beer samples were extracted with acetonitrile, and 1.5 g of sodium chloride was used for salting out. The purification agent was 30 mg PSA+15 mg GCB+885 mg anhydrous magnesium sulfate, mobile phase A was 0.01% formic acid aqueous solution+2 mmol/L ammonium formate solution, mobile phase B was methanol, and the chromatographic column was Shim pack GIST-HP C18-AQ (100 mm × 2.1 mm, 1.9 μm). The analysis was carried out in multiple reaction monitoring mode (MRM) and the external standard method was used for quantification. The results showed that there was a good linear relationship among the 10 types of carbamate pesticides within the concentration range of 5~150 μg/L, and the correlation coefficients (R2) were all greater than 0.999 0,the LOD was 0.10-1.43 μg/L, the LOQ was 0.29-4.76 μg/L, the spiked recovery rate of the sample was 85.9%~118.0%, and the RSD was 1.4%~8.8% (n=6). This method was accurate in quantification, simple in operation, and fast in analysis, and was suitable for rapid screening and quantitative analysis of various carbamate pesticide residues in beer.

Key words: beer, QuEChERS method, high performance liquid chromatography tandem mass spectrometry, carbamate pesticides, residues

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