正相高效液相色谱法同时测定芝麻油中生育酚、芝麻素及芝麻林素含量

Simultaneous determination of tocopherol,sesamin and sesamolin in sesame oil by normal phase-high performance liquid chromatography

建立了正相高效液相色谱法同时测定芝麻油中生育酚(α-、β-、γ-、δ-生育酚)、芝麻素及芝麻林素含量的方法。样品经正庚烷溶解后,在二醇基硅胶色谱柱上以四氢呋喃-正庚烷溶液洗脱、荧光检测器分析。结果表明:芝麻素及芝麻林素荧光特性良好,样品分析在20 min内完成;方法学评价结果显示生育酚在1.0~5.0μg/m L、芝麻素及芝麻林素在0.1~5.0μg/m L范围内线性关系良好,相关系数R^2均大于0.99;生育酚、芝麻素以及芝麻林素的检出限为0.29~0.74 mg/kg,定量限为0.91~2.10 mg/kg;6种化合物加标回收率为83.47%~104.57%,相对标准偏差为0.38%~6.55%。采用该方法分析了12个芝麻香油、冷榨芝麻油、浸出成品芝麻油中生育酚、芝麻素以及芝麻林素含量,发现芝麻油中生育酚以γ型为主,芝麻素、芝麻林素含量较高。该方法简单、灵敏度高、重复性好,可用于芝麻油中生育酚、芝麻素及芝麻林素含量的同时检测。

A method was developed for simultaneous determination of tocopherol, sesamin and sesamolin in sesame oil by normal phase - high performance liquid chromatography. The sample was dissolved by n - heptane, and eluted by tetrahydrofuran - n - heptane in a DIOL column, and detected by fluorescence detector. The results showed that sesamin and sesamolin presented good fluorescent characteristics and the analysis was carried out within 20 min. The evaluation of methodology indicated that tocopherol showed a good linearity in the range of 1.0 - 5.0 μg/mL while sesamin and sesamolin of 0. 1 - 5.0 μg/mL with correlation coefficients （R2） above 0.99. The limits of detections （LODs） and the limits of quantifications （LOQs） of tocopherol, sesamin and sesamolin were 0.29 -0.74 mg/kg and 0.91 -2.10 mg/kg, respectively. The average recoveries of six analytes were 83.47% - 104.57%, and the relative standard deviations （RSDs） were 0.38% -6.55%. Twelve samples including fragrant sesame oil, cold pressed sesame oil and extracted sesame oil were analyzed by this method. The results showed that main tocopherol in the sesame oil was γ＇ type and the contents of sesamin and sesamolin were high. The method could be used to simultaneously determine tocopherol, sesamin and sesamolin due to its simple operation, high sensitivity and good reproduction.