凝胶渗透色谱-高效液相色谱-串联质谱法测定 食品中邻苯二甲酸酯类化合物的含量

Determination of phthalates in food by gel permeation chromatography-high performance liquid chromatography-tandem mass spectrometry

中文关键词:  邻苯二甲酸酯  高效液相谱-串联质谱  凝胶渗透色谱

英文关键词:phthalates  high performance liquid chromatography-tandem mass spectrometry  gel permeation chromatography

中文摘要:

      目的 建立同时测定食品中6种邻苯二甲酸酯类化合物含量的高效液相色谱-串联质谱方法(HPLC-MS/MS)。方法 以Agilent ZORBAX SB-C18色谱柱为分析柱, 以甲醇-0.1%甲酸水为流动相, 采用梯度洗脱模式, 流速为0.35 mL/min; 质谱离子源的工作模式为正离子电离模式(ESI+), 采用多反应监测离子模式(MRM)进行定量检测; 样品用有机溶剂提取, 凝胶渗透色谱净化。结果 食品中邻苯二甲酸丁苄酯等6种增塑剂在线性范围内线性关系良好(r2＞0.999), 定量限为0.04~0.2 μg/kg, 检测限为0.01~0.04 μg/kg。方法的加标回收率为81.9%~103.9%, 相对标准偏差均小于7.2%。结论 本文所建立的方法简单, 灵敏度高, 适用于食品中的6种邻苯二甲酸酯类增塑剂的分析检测。

英文摘要:

      Objective To establish a method for the simultaneous determination of 6 kinds of phthalates in food by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). Methods The samples were separated by an Agilent ZORBAX SB-C18 column with a mobile phase of methanol-0.1% formic acid/water in gradient elution mode at the flow rate of 0.35 mL/min. The mass spectrometry worked in the positive ion mode, and multiple reaction monitoring (MRM) was adopted for the quantification of the analytes. Samples were purified by gel permeation chromatography (GPC) after extraction with organic solvents. Results A good linearity for 6 kinds of phthalates was achieved, with all correlation coefficients more than 0.999. Average recoveries of 6 analytes at three spiked level were ranged from 81.9% to 103.9%, with RSDs less than 7.2%. The limits of quantification and detection of the method was 0.04~0.2 μg/kg and 0.01~0.04 μg/kg, respectively. Conclusion The established method is sensitive and simple, and suitable for the determination of 6 kinds of phthalates in food.