分散固相萃取-同位素稀释高分辨质谱法测定 植物油中16种邻苯二甲酸酯

Determination of 16 phthalate esters in vegetable oils by dispersive solid phase extraction-high resolution mass spectrometry with isotope dilution technique

中文关键词:  邻苯二甲酸酯  分散固相萃取  高分辨质谱法  植物油

英文关键词:phthalate esters  dispersive solid phase extraction  high-resolution mass spectrometry  vegetable oils

中文摘要:

      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2~500 μg/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8~10 μg/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。

英文摘要:

      Objective To establish a dispersive solid phase extraction (d-SPE)/high-resolution benchtop Q exactive mass spectrometry (HRMS) method for the rapid analysis of 16 phthalate esters (PAEs). Methods The samples were extracted with acetonitrile saturated with hexane, and cleaned up by d-SPE with the N-propyl ethlene diamine (PSA) and Nano Carb as the sorbents. The chromatographic analysis was per-formed on a BEH phenyl column with 0.1% formic acid in acetonitrile and 0.1% formic acid solution as the mobile phase and a gradient elution program was used. The PAEs were analyzed in positive mode by Q exactive high-resolution mass spectrometry, which were applied in rapid analysis of PAEs for vegetable oils. 16 PAEs analytes were screened qualitatively in the vegetable oil samples and then quantified by isotope dilution technique. Results All the target 16 PAEs showed a good linearity in the range of 2~500 μg/L , and the aver- age recovery rates of the spiked vegetable oil samples were in the range of 77.9%~115.6% with the RSD in the range of 0.3%-8.9%. The limit of quantification (LOQ) for 16 PAEs in vegetable oil were between 8 μg/kg and 10 μg/kg. Conclusion The method was simple, sensitive and accurate, and was suitable for the rapid analysis of 16 PAEs in vegetable oils.