[关键词]
[摘要]
本文研究了超高效液相色谱-三重四极杆质谱联用仪(UPLC-MS/MS)在检测食用植物油中缩水甘油酯(GEs)含量的应用。通过提高前处理上样量,增加了目标物的分析浓度,满足对GEs含量更低的样品的检测要求;优化了流动相梯度洗脱程序,避免了流动相对色谱柱造成损耗,并减少有机溶剂的使用,且整个流动相梯度洗脱程序只需15.2 min,更加高效;通过子离子模式优化了5种GEs的定量离子对和碰撞能,采用多反应监测模式(MRM)进行定量使得5种GEs的检测更具特异性。本方法中5种GEs的检出限在0.0045~0.023 mg/kg之间,平均回收率在96.16%~107.02%之间,相对标准偏差(RSD)为1.98%~5.74%。这说明,此方法可操作性强,具有较高的灵敏度和准确度,重现性好,能够满足实际食用植物油样品中微量GEs的高效准确定量检测。
[Key word]
[Abstract]
This study investigated the application of ultra-performance liquid chromatography-triple quadrupole mass spectrometry (UPLC-MS/MS) in the analysis of glycidyl esters (GEs) in edible vegetable oils. By increasing the loading quantity of sample for pretreatment, the analytical concentration of the target substance was increased while satisfying the detection requirements for samples with lower GE contents. The elution procedure for the mobile phase was optimized to avoid mobile phase-induced loss of stationary phase and reduce the use of organic solvents. As a result, the total elution time was only 15.2 min, which made the analysis more efficient. After the quantitative ion pairs and collision energies were optimized in daughter ion mode, the multiple reaction monitoring mode (MRM) was adopted to quantify the five GEs in more specific way. The minimum detection limit of the five GEs ranged from 0.0045 to 0.023 mg/kg, and the average recovery rate was 96.16%~107.02% with the relative standard deviation as 1.98%~5.74%. Accordingly, this method has strong operability, high sensitivity and good reproducibility, and can meet the requirements for efficient, accurate and quantitative analysis of GEs in actual edible vegetable oils.
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[基金项目]
国家重点研发计划项目(2017YFC1600405-2;2016YFD0400401-5);国家自然科学基金资助项目(31771895;31471677)