离子液体辅助提取刺玫果中木犀草素与金丝桃苷的工艺研究

Study on process of ionic liquid-based ultrasonic-assisted extraction of luteolin, hyperoside from fruit of Rosa davurica Pall.

为给刺玫果的开发利用提供参考依据。采用单因素试验与正交试验相结合的研究方法,以木犀草素、金丝桃苷的峰面积为指标,采用高效液相色谱法,建立了同时测定刺玫果中木犀草素、金丝桃苷含量的方法,探寻并优化了离子液体辅助提取刺玫果中木犀草素、金丝桃苷的工艺条件。检测与分析结果表明:色谱柱为伊利特ODS2 C18(4.6 mm×250 mm,5μm),流动相以乙腈-0.2%磷酸水溶液梯度洗脱,进样量20μL,检测波长360 nm,柱温35℃;木犀草素、金丝桃苷进样质量浓度在0.19~15.20μg·m L-1范围内其线性关系(r=0.997 7)均良好;木犀草素的平均回收率为97.49%,RSD为1.76%;金丝桃苷的平均回收率为101.07%,RSD为1.83%。优化试验结果表明,离子液体辅助提取的最佳工艺条件为:离子液体浓度为0.45 mol·L-1,料液比为1∶25,乙醇的体积分数为70%,提取温度为80℃,提取时间为90 min,超声波功率为180 W;在此优化的提取条件下,木犀草素、金丝桃苷的提取率分别为11.99、25.36μg·g-1,其提取率分别提高了36.87%、49.09%。验证试验结果表明:建立的含量测定方法具有良好的精密度,结果准确可靠;优化的提取方法快速、简单、提取率高。

To provide reference for the development and utilization of Fruit of Rosa davurica Pall. Using a combination of single-factor and orthogonal tests, the peak area of luteolin and hyperoside was used as an indicator, and high- performance liquid chromatography was used to establish simultaneous determination of Fruit of Rosa davurica Pall. The proposed method utilizes a ELITE ODS2 C18 colurrm（4.6 mmx250 mm, 5 μm） with gradient elution of Acetonitrile and 2% Phosphoric acid solution at 35 ℃. An effluent flow rate of 1 mL/min, injection volume 20μL and UV detection at 360 nm was used for the analysis. The described method was linear in the range of 0.19-15.20 μg·m L-1 （r=0.997 7）, with excellent correlation coefficients. The average recoveries of luteolin were 97.49% with RSD of 1.76%. The average recovery of luteolin was 101.07% with RSD of 1.83%. The optimal extraction conditions were as follows： the concentration of ionic liquid was 0.45 mol·L-1, the solid-liquid ratio was 1：25, the volume fraction of ethanol was 70%, the extraction temperature was 80℃, the extraction time was 90 min, the ultrasonic power was 180 W, Under optimized extraction conditions, the extraction rates of luteolin and hyperoside were 11.99μg·m L-1 and 25.36 μg·m L-1, the extraction rate of luteolin was increased by 36.87%, and the extraction rate of hyperoside increased by 49.09%. respectively. Therefore, the proposed analytical method is accurate and specific. The extractive method is fast, simple, high extraction rate.