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  

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

作　　者：常晨阳 王晓 单娇 李晓明 CHANG Chen-yang;WANG Xiao;SHAN Jiao;LI Xiao-ming(Technology Center of Jinan Customs District,Jinan 250002,China;Liaocheng Customs,Liaocheng 252000,Shandong,China;Zaozhuang Customs,Zaozhuang 277000,Shandong,China;Huangdao Customs,Qingdao 266000,Shandong,China)

机构地区：[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

出　　处：《湖北农业科学》2024年第9期180-184,共5页Hubei Agricultural Sciences

基　　金：海关总署科研项目(2020HK200)。

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,1.9μm),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5~150μg/L浓度范围内线性关系良好,相关系数(R^(2))均>0.9990,LOD为0.10~1.43μg/L,LOQ为0.29~4.76μg/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。To establish a QuEChERS high-performance liquid chromatography tandem mass spectrometry method for simultaneous de-termination 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,1.9μm).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 relation-ship among the 10 types of carbamate pesticides within the concentration range of 5~150μg/L,and the correlation coefficients(R^(2))were all greater than 0.9990,the LOD was 0.10-1.43μg/L,the LOQ was 0.29-4.76μg/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.

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 

分 类 号：O657.7[理学—分析化学]