在线凝胶渗透色谱-三重四极杆气质联用法同时测定橄榄油中72种农药残留

Determination of 72 pesticide residues in olive oil by online gel permeation chromatography gas chromatography-tandem mass spectrometry

目的采用在线凝胶渗透色谱-三重四极杆气质联用仪（GPC-GC/MS/MS）建立了橄榄油中72种农药残留的分析方法。方法样品中的农药残留用正己烷溶解后用乙腈溶液振荡提取,经分散固相萃取法净化处理,取上清液并用微孔滤膜过滤,采用在线GPC-GC/MS/MS在多反应监测模式下进行测定,外标法定量。结果 72种农药组分在5~200μg/L质量浓度范围内呈良好线性关系,相关系数r大于0.99,测定低限为0.0045~1.00μg/L。对空白橄榄油样品进行3个浓度水平0.01、0.05和0.1 mg/kg的加标回收试验,各农药的加标回收率为60.5%？119.5%,相对标准偏差（RSD）为3.5%？14.7%。结论本方法具有前处理简便、快速高效、灵敏度高、试剂成本低等特点,完全能够满足橄榄油中72种农药残留的日常检测需要。

Objective To establish a method for the simultaneous determination of 72 pesticide residues in olive oil by online gel permeation chromatography gas chromatography-tandem mass spectrometry （GPC-GC/MS/MS） method. Methods The samples were extracted with acetonitrile and n-hexane, cleaned up using dispersive solid phase extraction （DSPE）, and then filtrated by micro filtration membrane. The extractions were detected by online GPC-GC/MS/MS under the multi reaction monitoring （MRM） mode and quantified by the external standard method. Results The correlation coefficients （r） of 72 pesticides were greater than 0.99 in the concentration range of 5-200 ~tg/L. The limits of quantitation （LOQ） were varied from 0.0045 to 1.00 ~tg/L. It was found that the average recoveries ranged from 60.5% to 119.5%, and the relative standard deviations （RSD） were in the range of 3.5% to 14.7% at three spiked levels 0.01, 0.05 and 0.1 mg/kg. Conclusion The method is simple, fast, efficient, sensitive and cheap. It can meet the detection needs of the 72 pesticide residues in olive oil.