核磁共振法监控山茶油甘油解的方法研究

Method of monitoring glycerolysis of oil-tea camellia seed oil by NMR

对核磁共振法监控山茶油甘油解的方法进行了研究。通过查找核磁共振谱图中山茶油甘油一酯(MAG)、甘油二酯(DAG)及甘油三酯(TAG)的特征指标,建立了其特征指标与含量的定量关系,从而实现了山茶油甘油解反应程度的有效监控。对1H NMR谱分析得到甘油一酯的特征峰化学位移(δ)为3.92,1,2-甘油二酯的特征峰化学位移(δ)为5.09,1,3-甘油二酯的特征峰化学位移(δ)为4.09,甘油三酯的特征峰化学位移(δ)为5.27,其相对峰面积分别为88.69、42.11、27.26、和36.74,进而推导出未知样甘油酯含量的计算方法。通过对比,发现核磁共振法和柱层析法监控山茶油甘油解反应的测定结果无显著性差异,核磁共振法所得到的结果可靠,可以用于山茶油甘油解反应过程的监控。

The method of monitoring glycerolysis of oil-tea camellia seed oil by nuclear magnetic resonance(NMR)was studied.The characteristic indexes of monoacylglycerols(MAG),diacylglycerols(DAG)and triacylglycerols(TAG)were searched from NMR spectrum,and the quantitative relationship between the characteristic index and content was established so as to effectively monitor the reaction degree of glycerolysis of oil-tea camellia seed oil.The chemical shifts of the characteristic peaks of monoacylglycerols,1,2-diacylglycerols,1,3-diacylglycerols and triacylglycerols were δ3.92,δ5.09,δ4.09 and δ5.27,and their relative peak areas were 88.69,42.11,27.26 and 36.74,respectively.Then the calculation method of glyceride content in unknown samples was deduced.It was found that there was no significant difference between the results of NMR and column chromatography in monitoring glycerolysis of oil-tea camellia seed oil by comparison.The results obtained by NMR were reliable and NMR could be used for monitoring the glycerolysis of oil-tea camellia seed oil.