利用多壁碳纳米管的QuEChERS技术结合液相色谱-质谱法测定食用菌农药残留量

Determination of Pesticide Residues in Edible Fungi by QuEChERS Technique with Multi-Walled Carbon Nanotubes Coupled to Liquid Chromatography Mass Spectrometry

为建立一种食用菌常见农药的分析方法,样品经乙腈提取,采用QuEChERS方法前处理,经碳纳米管净化,用高效液相色谱-质谱仪检测。碳纳米管用量为5 mg、25 mg、50 mg,试验结果表明5 mg的用量效果较好。正离子模式下,61种农药标准品在水-甲醇(均含有10 mmol·L^(-1)乙酸铵和0.01%乙酸)流动相中具有较好的响应;各化合物在0.01 mg·L^(-1)~0.40 mg·L^(-1)范围内线性良好,相关系数r均大于0.99。3个浓度水平加标回收试验的回收率为70.17%~101.85%,相对标准偏差为1.09%~10.00%。结果表明,该方法操作简单、分析准确,满足食用菌中常见农药的检测要求。

In order to establish a method for determination of pesticide residues in edible fungi,the target pesticides in edible fungi were extracted by a modified QuEChERS method with acetonitrile as the solvent,followed by cleanup with multi-walled carbon nanotubes(MWCNTs).The target pesticides were determined by HPLC-MS.The experimental results of carbon nanotube dosage(5 mg,25 mg,50 mg)showed that the dosage of 5 mg is better.In the positive ion mode,the 61 pesticide residues responded well in the mobile phase of water-methanol(containing 10 mmol·L^(-1) ammonium acetate and 0.01%acetic acid).Each compound had good linearity in the range of 0.01 mg·L^(-1)-0.40 mg·L^(-1),and the correlation coefficients r were greater than 0.99.The recoveries of the 3 concentration levels of the standard addition recovery experiment were 70.65%-101.85%,and the relative standard deviations were 1.09%-10.00%.The method is simple and accurate,and can meet the detection requirement of common pesticides in edible fungi.