液相色谱-串联质谱法定量检测油脂中16种多环芳烃

Quantitative determination of 16 polycyclic aromatic hydrocarbons in fats and oils by liquid chromatography-mass spectrometry.

中文关键词:  固相萃取  多环芳烃  高效液相色谱-三重四极杆质谱  油脂  菜籽油

英文关键词:solid-phase extraction  polycyclic aromatic hydrocarbons  high-performance liquid chromatography tandem mass spectrometry  oils and fats  rapeseed oil

中文摘要:

      目的 为保障食用油安全性评价和质量，提高检测效率和易用性，建立同时测定食用油中16种多环芳烃（Polycyclic aromatic hydrocarbons，PAHs ）含量的方法。方法 油脂经乙腈提取处理后，采用柱纯化技术对PAHs进行富集，通过液相色谱-串联质谱进行检测。重点优化离子源的选择、色谱柱的优化、提取溶剂和提取溶剂体积以及洗脱溶液的选择等。确定最优前处理方法为: 5 mL乙腈提取，PAH固相萃取柱净化并用15 mL乙酸乙酯:二氯甲烷（υ:υ=1: 1）洗脱。最优检测条件为:使用APCI电离源在正离子模式下进行离子化，使用Eclipse PAH液相色谱柱进行分离。结果 16种PAHs在0.1~500.0 ?g/L的质量浓度范围内呈现良好的线性关系，检出限在0.04~1.72 μg/kg,定量限在0.14~17.01 ?g/kg，加标回收率有最优值为75.71%~117.6%，日内相对标准偏差为0.09%~8.00%，日间相对标准偏差为0.10%~8.18%。结论 该方法可准确提取并检测出16种PAHs，提高食用油中PAHs的检测效率，为食用油的安全性评价提供了方法支撑。

英文摘要:

      Objective To ensure the safety assessment and quality of edible oil, a method for simultaneously determining 16 kinds of polycyclic aromatic hydrocarbons (polycyclic aromatic hydrocarbons PAHs) in edible oil was established. Methods After being extracted with acetonitrile, PAHs were enriched using column purification technology, and analyzed by liquid chromatography-tandem mass spectrometry (LC-MS/MS). We optimized the following conditions including purification conditions, the ion sources, as well aschromatographicseparation.PAHs were extracted with acetonitrile, then purified with a PAH solid-phase extraction (SPE) column, followed by being eluted with the mixture of ethyl acetate and dichloromethane (υ:υ=1:1). They were separated with an Eclipse PAH liquid chromatography column, and analyzed using an APCI ion source in positive ion mode. Results The 16 PAHs showed a good linearity ranging from 0.1-500.0 μg/L. The limit of detection was determined from 0.04-1.72 μg/kg, while the limit of quantification was from 0.14-17.01 μg/kg. The recovery rates of the spiked samples were between 75.71%-117.6%. The intraday relative standard deviations were between 0.09%-8%, and the interday relative standard deviations were between 0.1% and 8.18%. Conclusion The established method is rapid and efficient, capable of accurately extracting and detecting 16 types of PAHs, making it suitable for the rapid detection of PAHs in edible oils.