加速溶剂萃取法提取小米多酚及其组分分析

Extraction of millet polyphenols by accelerated solvent extraction and analysis of components of millet polyphenols

中文关键词:  小米多酚  加速溶剂萃取  响应面法  多酚组成  滋味

英文关键词:millet polyphenol  accelerated solvent extraction  response surface method  polyphenol composition  relish

中文摘要:

      目的 采用加速溶剂萃取方法构建快速高效的小米多酚提取方法, 并探究小米多酚类化合物的组成及滋味成分。方法 采用加速溶剂萃取方法, 以小米粉为原料, 基于加速溶剂萃取仪, 分析乙醇体积分数、萃取温度和萃取时间对提取的小米多酚含量的影响, 并对提取工艺参数进行响应面优化, 通过超高效液相色谱-三重四极杆/线性离子阱质谱法(ultra performance liquid chromatography-triple quadrupole/linear ion trap mass spectrometry, UPLC-QTRAP-MS/MS)对所得小米多酚的组成及滋味成分进行分析。结果 加速溶剂萃取法提取小米多酚的最优工艺参数为: 乙醇体积分数为59%、萃取时间10 min、萃取温度60℃, 此条件下小米多酚含量达(2.90±0.01) mg/g。UPLC-QTRAP-MS/MS从小米中共鉴定出822种多酚类化合物, 其中黄酮类化合物最多, 占总多酚类化合物的47.20%; 其次为酚酸类化合物, 占42.09%。将822种多酚类化合物与滋味库进行对比, 发现其中能够呈现滋味的有16种, 分别是2-甲氧基-4-甲基苯酚、水杨酸、苯甲酸、苯甲酰胺、芥子酸、熊果苷、咖啡酸、没食子酸、苯醋酸乙酯、查尔酮、水飞蓟素、白杨素、杨梅素、槲皮素、6-甲基香豆素、双香豆素。结论 以加速溶剂萃取法结合响应面分析提取小米多酚的方法是可行的, 该方法简便省时, 是小米提取多酚的有效途径。本研究系统地定性了小米多酚的组成成分及其种类, 明确了部分多酚类化合物的滋味, 为小米多酚的组成及小米滋味的研究提供一定的理论依据。

英文摘要:

      Objective To construct a fast and efficient extraction method for polyphenols from millet by accelerated solvent extraction method, and study the composition and flavor components of millet polyphenols. Methods The effects of ethanol volume fraction, extraction temperature and extraction time on the polyphenol content of millet were analyzed by an accelerated solvent extraction instrument using millet flour as raw material. The extraction process was optimized by response surface method, and the composition and taste of the obtained millet polyphenols were analyzed by ultra performance liquid chromatography-triple quadrupole/linear ion trap mass spectrometry (UPLC-QTRAP-MS/MS). Results The optimal extraction process of millet polyphenols by accelerated solvent extraction was as follows: Ethanol volume fraction was 59%, extraction time was 10 min, extraction temperature was 60℃, and the maximum content of millet polyphenols was (2.90±0.01) mg/g under these conditions. After UPLC-QTRAP-MS/MS detection, 822 kinds of polyphenols were identified in rice flour, among which flavonoids were the most, accounting for 47.20% of the total polyphenols. The second was phenolic acid compounds, accounting for 42.09%. By comparing 822 kinds of polyphenols with the taste library, 16 kinds of polyphenols were found to present taste, which were 2-methoxy-4-methylphenol, salicylic acid, benzoic acid, benzamide, sinapic acid, arbutin, caffeic acid, gallic acid, ethyl phenylacetate, chalcone, silibinin, chrysin, myricetin, quercetin, 6-methylcoumarin, and dicumarol. Conclusion The accelerated solvent extraction method combined with response surface analysis is feasible. The method is simple and time-saving. It is an effective way to extract polyphenols from millet. This study has systematically characterized the components and types of millet polyphenols, and clarified the taste of some polyphenols, and provides a certain theoretical basis for the study of the composition and taste of millet polyphenols.