芝麻油中芝麻素、芝麻林素和细辛素 检测方法优化Optimization of detection methods for sesamin, sesamolin and asarinin in sesame oil

Abstract

采用有机溶剂甲醇提取、HPLC同时分析芝麻油中芝麻素、芝麻林素和细辛素含量。为提高分析质量与准确性，优化甲醇提取溶剂用量和超声辅助提取的时间，并对检测方法进行方法学考察。结果表明：最佳提取条件为甲醇用量10 mL（芝麻油0.1 g），超声时间2 min;芝麻素、芝麻林素和细辛素线性范围分别为4～100 mg/L、4～100 mg/L和1～40 mg/L，线性关系良好，相关系数分别为0999 5、0.999 6和0.999 2；芝麻素、芝麻林素和细辛素的检出限分别为0.03、0.02 mg/g和0.02 mg/g，定量限分别为0.06、0.06 mg/g和0.04 mg/g，加标回收率分别为87.17%～92.59%、9271%～102.24%和95.66%～108.93%，加标回收率的相对标准偏差均小于5%，方法的稳定性、准确性和精密度均符合检测要求。该方法操作简单、耗时短(完成一次分析只需30 min)、成本低、稳定性高，能有效应用于芝麻油中3种木脂素组分的分析检测。The content of sesamin, sesamolin and asarinin in sesame oil was simultaneously analyzed by organic solvent methanol extraction and HPLC method. In order to improve the analysis quality and accuracy, the dosage of methanol extraction solvent and the time of ultrasound-assisted extraction were optimal, and the detection method was investigated. The results showed that the optimal extraction conditions were methanol dosage 10 mL（0.1 g sesame oil）, ultrasonic time 2 min. The sesamin, sesamolin and asarinin had good linearity within the ranges of 4-100 mg/L, 4-100 mg/L and 1-40 mg/L, respectively, and their correlation coefficients were 0.999 5, 0.999 6 and 0.999 2, respectively. The LOD of sesamin, sesamolin and asarinin were 0.03, 0.02 mg/g and 0.02 mg/g, respectively, and their LOQ were 0.06, 0.06 mg/g and 0.04 mg/g, respectively. The recoveries of sesamin, sesamolin and asarinin were 87.17%-92.59%, 92.71%-102.24% and 95.66%-10893%, respectively, with RSD all less than 5%. The stability, accuracy and precision of the method met the testing requirements. In conclusion, the method has advantages of simple operation, short time-consuming (only 30 min to complete an analysis), low cost, high stability, etc., and can be effectively applied to the analysis and detection of three lignan components in sesame oil.

Keywords

• 高效液相色谱；芝麻油；芝麻素；芝麻林素；细辛素
• hplc; sesame oil; sesamin; sesamolin; asarinin