表面活性剂结合QuEChERS-气相色谱-串联质谱法同时测定大豆油中有机氯农药、多氯联苯及多环芳烃

Simultaneous Determination of OCPs, PCBs and PAHs in Soybean Oil Using Surfactant-Based QuEChERS Method Coupled with GC-MS/MS

  • 摘要: 建立了气相色谱-串联质谱(GC-MS/MS)同时测定大豆油中34种有机氯农药(OCPs)、12种多氯联苯(PCBs)及6种多环芳烃(PAHs)残留量的检测方法。首先使用表面活性剂作为乳化剂制备相对稳定的油/水乳状液,采用乙腈-二甲苯(9∶1,V/V)为提取剂,以QuEChERS前处理方法对其提取2次后净化,随后进行GC-MS/MS检测。对8种表面活性剂及添加浓度进行优化,结果表明,表面活性剂的添加可显著提高大豆油中OCPs、PCBs及PAHs的提取率,最佳添加方案为大豆油∶水∶Tween60=1∶3∶0.01 (m/m/m)。该方法在1/2.5/5/10~400 μg/L浓度范围内的线性关系良好,相关系数R2为0.993 8~0.999 7。在5~100 μg/kg添加浓度水平内,相对标准偏差为1.59%~20.50%,34种OCPs在大豆油中的添加回收率为64.35%~120.63%,12种PCBs的添加回收率为49.65%~97.76%,6种PAHs的添加回收率为74.05%~101.52%。该方法操作简单、油脂去除效果良好,灵敏度、精密度及回收率均可满足国内外相关标准中大豆油中残留限量的要求。

     

    Abstract: A method of gas chromatography-tandem mass spectrometry (GC-MS/MS) was developed for determination of 34 kinds of organochlorine pesticides (OCPs), 12 kinds of polychlorinated biphenyls (PCBs) and 6 kinds of polycyclic aromatic hydrocarbons (PAHs) in soybean oil.Firstly, 1 g soybean oil and 3 g purified water were emulsified with surfactant, then extracted with 5 mL acetonitrile-xylene mixture (9∶1, V/V) by QuEChERS method, and detected by GC-MS/MS. The optimal experiments of adding surfactants about species and concentrations showed that the adding of surfactants can significantly increase the extraction efficiency of OCPs, PCBs, PAHs in soybean oil, and the appropriate surfactant is Tween 60. The calibration curves show a good linearity for all the congeners, and the relative coefficient is 0.993 8-0.999 7. The relative standard deviations (RSDs) are in the range of 1.59%-20.50%, and the spiked recoveries of OCPs range from 64.35% to 120.63%, that of PCBs are in the range of 49.65%-97.76%, and PAHs range from 74.05% to 101.52%. The developed analytical method is quick and easy maneuverability with satisfactory effect on the removing of oil, which is suitable for the determination of OCPs, PCBs, PAHs in soybean oil.

     

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