GC-MS/MS法同时测定蜂王浆中8种高风险农药残留

Simultaneous Determination of 8 High-risk Pesticide Residues in Royal Jelly by GC-MS/MS

建立气相色谱-三重四极杆质谱联用法同时测定蜂王浆中双甲脒、双甲脒2,4-DMA、氯苯胺灵、克螨特、毒死蜱、三唑醇、蝇毒磷、氟胺氰菊酯8种高风险农药残留的检测方法。样品经提取净化后,使用Agilent19091S-431 HP-5ms,15 m×250μm×0.25μm色谱柱2根,在EI源和动态多反应监测dMRM模式下采集数据,以外标法定量。结果表明,该方法在0.02~0.25μg/mL具有良好线性关系,相关系数R^(2)为0.9917~0.9990;检出限为0.003 mg/kg;定量限为0.009 mg/kg。方法采用在0.01,0.05和0.10 mg/kg这3个浓度进行加标回收试验,回收率范围为80.7%~109.2%;精密度S_(RSD)为0.89%~9.74%(n=6)。该方法操作简单、准确可靠、灵敏度高,可同时完成蜂王浆中8种农药残留的检测。

A method for the simultaneous determination of 8 high-risk pesticide residues of amitraz,amitraz 2,4-dma,chlorpropham,propargite,chlorpyrifos,triadimenol,coumaphos and fluvalinate in royal jelly by gas chromatography triple quadrupole mass spectrometry was established.After extraction and purification,Agilent 19091s-431 HP-5 ms and 15 m×250μm×0.25μm chromatographic columns used,the data were collected in EI source and dynamic multi reaction monitoring d MRM mode and quantified by external standard method.The results showed that this method had a good linear relationship in the range of 0.02-0.25μg/mL,and the correlation coefficient R^(2) was 0.9917-0.9990.The detection limit was 0.003 mg/kg and the limit of quantization was 0.009 mg/kg.The standard addition recovery test was carried out at the concentrations of 0.01,0.05 and 0.10 mg/kg with the recovery ranged from 80.7% to 109.2%.The precision S_(RSD) was 0.89%-9.74%(n=6).This method was simple,accurate,reliable and sensitive,which could detect 8 pesticide residues in royal jelly at the same time.