超高效液相色谱质谱联用法测定蔬菜中 氨基甲酸酯农药及其代谢物研究

Determination of carbamate pesticides and metabolite residues in vegetables by ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  氨基甲酸酯农药  代谢物  超高效液相色谱质谱联用法  蔬菜

英文关键词:carbamate pesticides  metabolite  ultra performance liquid chromatography-tandem mass spectrometry  vegetables

中文摘要:

      目的 建立以QuEChERS法进行样品前处理, 以超高效液相色谱质谱联用法分析蔬菜中氨基甲酸酯类农药的多残留检测技术, 以适应食品安全风险监测工作需要。方法 采用QuEChERS法进行样品前处理, 采用超高效液相色谱串联三重四极杆联用技术, 以CH3CN:0.1%甲酸含5 mmol/L甲酸铵(每升中加入10 mg无水乙酸钠)为流动相, 流速0.3 mL/min, 以ACCUIITY BEH C18 (2.1 mm ×100 mm, i.d. 1.7 μm) 为分析柱, 柱温35 ℃, 三重四杆质谱仪ESI源, 正离子模式, 多反应监测方式测定蔬菜中6种氨基甲酸酯类农药。结果 本方法检出限为0.01 mg/kg, 在线性范围2.5~200 ng/mL内有良好线性关系, 线性相关系数(r)分别为: 灭多威0.9997、涕灭威0.9993、克百威0.9994、涕灭威亚砜0.9979、3-羟克百威0.9994、涕灭威砜0.9995, 回收率62.3%~114.0%, 相对标准偏差2.53%~12.0%。结论 本方法样品制备速度快, 操作简便, 适用于蔬菜样品中氨基甲酸酯类农药多残留检测。

英文摘要:

      Objective On the basis of QuEChERS method for the sample pretreatment, to establish a simultaneous determination method of carbamate pesticides and metabolite residues in vegetables by ultra performance liquid chromatography-tandem mass spectrometry, in order to meet the needs of food safety monitoring. Methods The samples were extracted by ultra performance liquid chromatography and triple quadrupole technique, after the pretreatment with QuEChERS method. The mobile phase was CH3CN and 0.1% formic acid containing 5 mmol/L ammonium formate (10 mg anhydrous sodium acetate per liter of solution). The flow rate was 0.3 mL/min. An Accuity BEN C18 (2.1 mm ×100 mm, i.d. 1.7 μm) was used as the analysis column and the column temperature was 35 ℃. Six kinds of carbamate pesticides and metabolite residues in vegetables were measured by the triple quadrupole mass spectrometry, which was used under the source of ESI, positive ion multiple reaction mode (MRM) and multiple reaction detection method. Results The detection limit was 0.01 mg/kg. The method linear range was 2.5~200 ng/mL. Excellent linearities were obtained with the correlation coefficient (r): methomyl 0.9997, aldicarb 0.9993, carbofuran 0.9994, aldicarb sulfoxide 0.9979, 3-hydroxycarbofuran 0.9994, and aldicarb sulfone 0.9995, respectively. The average recoveries were 62.3%~114.0% and the relative standard deviations were in the range of 2.53%~12.0%. Conclusion The developed method is highly efficient, easy to operate and suitable for monitoring the 6 kinds of carbamate pesticides and metabolite residues in vegetables.