液相色谱-串联质谱法同时测定蜂王浆中15种高风险农药残留

Simultaneous determination of 15 kinds of high risk pesticide residues in royal jelly by liquid chromatography-tandem mass spectrometry

目的 建立液相色谱-串联质谱法(liquid chromatography-tandem mass spectrometry,LC-MS/MS)测定蜂王浆中苯菌灵、乙基硫菌灵、多菌灵等15种高风险农药残留的检测方法。方法 样品经提取净化后,以0.1%甲酸水溶液与甲醇为流动相进行梯度洗脱,采用电喷雾离子源正离子方式扫描,在多反应监测(multiple reaction monitoring, MRM)模式下检测。结果 实验验证15种农药在一定的浓度范围内,具有良好线性关系,相关系数为0.9915~0.9999,回收率范围为65.3%~113.5%,精密度为0.56%~9.11%,检出限为0.01 mg/kg,定量限为0.10 mg/kg。结论 该方法操作简单、准确可靠、灵敏度高,可同时完成蜂王浆中15种农药残留的检测。

Objective To establish a liquid chromatography-tandem mass spectrometry(LC-MS/MS) method for the determination of 15 kinds of high risk pesticide residues in royal jelly such as benomyl, thiophanate-ethyl and carbendazim, etc. Methods After extraction and purification, the samples were subjected to gradient elution with 0.1% formic acid aqueous solution and methanol as the mobile phase, and then scanned by using electrospray ion source positive ion method, and detected in multiple reaction monitoring(MRM) mode. Results The experiments verified that the 15 kinds of pesticides had good linear relationship within a certain concentration range, with the correlation coefficient of 0.9915-0.9999, recoveries range of 65.3%-113.5%, precision of 0.56%-9.11%, limit of detection was 0.01 mg/kg and limit of quantitation was 0.10 mg/kg. Conclusion This method is simple, accurate,reliable and sensitive, and can be used for the simultaneous detection of 15 kinds of pesticide residues in royal jelly.