摘要
为了建立简便、准确、快速测定油脂中的甘油三酯氧化聚合物(triacylglycerol polymers,TGP)的方法,用正向硅胶柱串联凝胶柱(双柱法),经高效液相色谱-蒸发光散射检测器分离检测油脂中的非极性部分、甘油三酯氧化寡聚物、甘油三酯氧化二聚物(oxidized dimeric triacylglycerols,TGD)、甘油三酯氧化单体、甘油二酯(diacylglycerls,DG)、脂肪酸等极性组分;以DG作为外标,结合外标法和面积归一化法定量油脂中TGP各组分的含量。结果表明:优化的测定条件为石油醚(A)和四氢呋喃(B)为流动相;梯度洗脱程序为0 min、5%B,20 min、15%B,30 min、30%B,35 min、5%B;流速0.7 mL/min;测定时间50 min;该条件下上述各组分分离效果良好。双柱法测定TGP的相关性良好,相关系数(R2)为0.9995,TGD检出限为156 mg/L,定量限为267 mg/L。双柱法对加标DG的回收率在95%~99%之间,相对标准偏差均小于2%;且检测油脂中TGP的重复性良好,相对标准偏差均小于3%。此方法能够在1 h内定量油脂中TGP的含量,操作简便、定量准确、节约试材。
This study aimed to establish a simple,rapid and accurate analytical method for the determination of oxidized triacylglycerol polymers(TGP)in oils and fats.Non-polar components(Non-PC)and polar components(PC),including oxidized triacylglycerol oligomers(TGO),oxidized triacylglycerol dimers(TGD),oxidized triacylglycerol monomers(ox-TGM),diacylglycerls(DG)and free fatty acids(FFA),were separated by high performance liquid chromatography with two sequential columns(silica gel column connected to Phenogel column)and detected by an evaporative light scattering detector.The peak area normalization method was used to quantitate TGP using DG as external standard.The eluent used was a gradient mixture of petroleum ether(A)and tetrahydrofuran(B).Elution was performed at a solvent flow rate of 0.7 mL/min in the following linear gradient mode:0 min,5%B;20 min,15%B;30 min,30%B;and 35 min,5%B,and the analytical time was 50 min.The results showed that good separation of the above compounds was achieved.The method exhibited a good linearity with a correlation coefficient(R2)of 0.9995.The limit of detection(LOD)of TGD was 156 mg/L,and the limit of quantitation(LOQ)was 267 mg/L.The recoveries of DG spiked samples were between 95%and 99%with relative standard deviation(RSD)of less than 2%.Moreover,the method presented good repeatability with RSD of less than 3%.This method could allow accurate quantification of TGP in oils and fats within 1 h with simple operation and without using extra experimental materials.
作者
邓琪
袁仲安
黄雪松
DENG Qi;YUAN Zhong’an;HUANG Xuesong(College of Science and Engineering,Jinan University,Guangzhou 510632,China)
出处
《食品科学》
EI
CAS
CSCD
北大核心
2020年第2期321-326,共6页
Food Science
基金
广东省科技计划项目(2017A050506030)
公益性行业(农业)科研专项(201303077)
关键词
三酰甘油氧化聚合物
极性组分
双柱法
高效液相色谱
oxidized triacylglycerol polymer
polar component
two sequential columns
high performance liquid chromatography
作者简介
第一作者:邓琪(1995-)(ORCID:0000-0003-4984-6050),女,硕士研究生,研究方向为食用油脂,E-mail:781943730@qq.com;通信作者:黄雪松(1957-)(ORCID:0000-0002-4164-1897),男,教授,博士,研究方向为功能性食品,E-mail:thxs@jnu.edu.cn。
