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目的采用高效液相色谱-四级杆/静电场轨道阱高分辨质谱建立分散固相萃取法(dispersive solid phase extraction,d-SPE)快速分析植物油中16种邻苯二甲酸酯(Phthalate esters,PAEs)的检测方法。方法样品采用正己烷饱和的乙腈提取,经N-丙基乙二胺(primary secondary amine,PSA)和Nano Carb填料分散固相萃取净化,以BEH phenyl色谱柱为分析柱,0.1%甲酸乙腈及0.1%甲酸水溶液作为流动相进行梯度洗脱分离。采用正离子采集模式对植物油样品进行快速筛查,并对16种PAEs进行定量测定。结果 16种PAEs在2~500μg/L范围内呈良好的线性关系,回归系数(r)大于0.995,该方法的定量限为8~10μg/kg。在不同加标水平下的平均回收率为77.9%~115.6%,相对标准偏差为0.3%~8.9%。结论本方法简单、灵敏、准确,适用于植物油中PAEs的快速筛查和定量测定。
OBJECTIVE To develop a dispersive solid phase extraction (d-SPE) method for the rapid analysis of 16 phthalate esters in vegetable oils by high performance liquid chromatography-quadrupole / electrostatic field orbit-well high resolution mass spectrometry PAEs) detection methods. Methods The sample was extracted with acetonitrile saturated with n-hexane, purified by solid-phase extraction (SPE) with primary secondary amine (PSA) and Nano Carb filler. The analytical column was BEH phenyl, 0.1% formic acid and 0.1 % Formic acid aqueous solution as a mobile phase gradient elution. The samples of vegetable oil were screened by positive ion mode and the quantification of 16 kinds of PAEs was carried out. Results The 16 PAEs showed a good linear relationship in the range of 2 ~ 500 μg / L with the regression coefficient (r) greater than 0.995. The limit of quantification for this method was 8 ~ 10 μg / kg. The average recoveries at different spiked levels ranged from 77.9% to 115.6% with relative standard deviations of 0.3% to 8.9%. Conclusion The method is simple, sensitive and accurate and is suitable for rapid screening and quantitative determination of PAEs in vegetable oils.