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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 an analytical method for 72 pesticide residues in olive oil by on-line gel permeation chromatography-triple quadrupole mass spectrometer (GPC-GC / MS / MS). Methods The pesticide residues in the sample were dissolved in n-hexane and then extracted by acetonitrile. The samples were purified by dispersive solid-phase extraction. The supernatant was collected and filtered through a microporous membrane. The reaction was monitored by on-line GPC-GC / MS / Mode determination, external standard method. Results 72 kinds of pesticides showed a good linearity in the concentration range of 5 ~ 200μg / L, the correlation coefficient r was greater than 0.99, and the lower limit of determination was 0.0045 ~ 1.00μg / L. The spiked recoveries of spiked olive oil samples at 0.01, 0.05 and 0.1 mg / kg were 60.5% -119.5% with relative standard deviations (RSDs) of 3.5% -14.7% . Conclusion The method is simple, rapid and efficient pretreatment, high sensitivity, low reagent costs, fully able to meet the 72 daily needs of olive oil in the detection of pesticide residues.