HPLC测定芝麻油中木脂素类化合物含量研究

Determination of Lignans in Sesame Oil by HPLC

建立了HPLC同时测定芝麻油中芝麻素、芝麻林素、芝麻酚和芝麻素酚4种木脂素化合物含量的方法。首先确定了HPLC法分离和测定这4种物质的色谱条件,色谱柱为ODS-C18(250 mm×4.6 mm,5μm);检测波长:芝麻素和芝麻林素为287 nm,芝麻酚和芝麻素酚为293 nm;柱温30℃;流速0.8 mL/min,流动相为甲醇(A)和水(B)进行梯度洗脱,梯度为0 min(A,60%)→6 min(A,60%)→9 min(A,75%)→24min(A,70%)→27 min(A,60%)→32 min(A,60%)。同时比较筛选了皂化法、氧化铝柱层析法和薄层层析法3种去除脂肪类成分的前处理方法,确定薄层层析法为最有效的前处理方法。

A HPLC method for simultaneously determining contents of lignans,including sesamin,sesamolin,sesamol and sesaminol,in sesame oil has been developed.Separation and content determination of the four lignans were achieved by using ODS-C18 column（250 mm × 4.6 mm,5 μm） and by a gradient elution using（A） methanol and（B） water as the mobile phase of 0 min（A,60%）→6 min（A,60%）→9 min（A,75%） →24 min（A,70%） →27 min（A,60%） →32 min（A,60%）.The flow rate was 0.8 mL/min and column temperature was 30 ℃.The wavelength was 287 nm for sesamin and sesamolin,and 293 nm for sesamol and sesaminol.Three pretreatment methods have been compared for the removal of triglyceride from sesame oil,namely saponification,alumina column chromatography and thin layer chromatography,and results showed that thin layer chromatography was the best.