[关键词]
[摘要]
目的 优化枇杷叶Eriobotryae Folium蜜炙炮制工艺,建立生品与炮制品的质量差异评价体系,为枇杷叶饮片的标准化生产与质量控制提供科学依据。方法 通过单因素实验考察蜜水比、料液比、闷润时间、炒制温度及炒制时间5个因素的影响,采用层次分析法(analytic hierarchy process,AHP)结合客观权重赋权法(criteria importance through intercriteria correlation,CRITIC)确定山楂酸、科罗索酸、齐墩果酸、熊果酸、新绿原酸、绿原酸、隐绿原酸、金丝桃苷的综合权重,利用Box-Behnken设计-响应面法(Box-Behnken design coupled with response surface methodology,BBD-RSM)优化关键工艺参数(蜜水比、炒制温度、炒制时间),得到枇杷叶蜜炙的最佳炮制工艺;利用UPLC/HPLC建立枇杷叶生品与蜜炙品的指纹图谱,通过相似度分析、层次聚类分析(hierarchical cluster analysis,HCA)、主成分分析(principal component analysis,PCA)及正交偏最小二乘-判别分析(orthogonal partial least squares-discriminant analysis,OPLS-DA)比较其成分差异,并进行色度值与指标成分的相关性分析。结果 优化得到蜜炙枇杷叶的最佳工艺参数为蜜水比1∶1.06、料液比2.0∶1、闷润时间2.5 h、炒制温度157.9 ℃、炒制时间11.1 min。建立的枇杷叶三萜酸类成分的指纹图谱中,生品共确定12个共有峰,炮制品共确定了9个共有峰,指认了其中的4个峰,分别为山楂酸(6号峰)、科罗索酸(7号峰)、齐墩果酸(11号峰)、熊果酸(12号峰),在蜜炙品中含量均有所增加;建立的有机酸类成分指纹图谱中,生品共确定11个共有峰,炮制品共确定12个共有峰,指认了其中的4个峰,新绿原酸(1号峰)、绿原酸(3号峰)、隐绿原酸(4号峰)、金丝桃苷(11号峰),在蜜炙品中含量均有下降趋势。枇杷叶饮片色度值(L*、a*、b*)与三萜酸类成分、有机酸类成分及黄酮醇类成分含量呈显著相关性。结论 建立的AHP-CRITIC权重结合BBD-RSM的优化方法,可综合考量多重指标的综合贡献,得到的蜜炙枇杷叶炮制工艺稳定可行;结合指纹图谱与化学计量学手段,精准表征了枇杷叶蜜炙前后的质量差异,为枇杷叶饮片质量的稳定可靠提供了安全保障。
[Key word]
[Abstract]
Objective To optimize the honey-frying process of Pipaye (Eriobotryae Folium, EF) and establish a quality differentiation system between raw and processed products, providing scientific evidence for standardized production and quality control of honey-fried EF. Methods The effects of five factors-honey-to-water ratio, solid-to-liquid ratio, moistening time, stir-frying temperature, and stir-frying duration were investigated through single-factor experiments. The comprehensive weights of maslinic acid, corosolic acid, oleanolic acid, ursolic acid, neochlorogenic acid, chlorogenic acid, cryptochlorogenic acid, and hyperoside were determined using the analytic hierarchy process (AHP) combined with the criteria importance through intercriteria correlation (CRITIC) objective weighting method. Key process parameters (honey-to-water ratio, stir-frying temperature, and stir-frying duration) were optimized via Box-Behnken design coupled with response surface methodology (BBD-RSM) to establish the optimal honey-processing conditions for EF. Ultra-performance liquid chromatography/high-performance liquid chromatography (UPLC/HPLC) was employed to develop fingerprint profiles of raw and honey-processed EF. Component differences were compared using similarity analysis, hierarchical cluster analysis (HCA), principal component analysis (PCA), and orthogonal partial least squares-discriminant analysis (OPLS-DA). Additionally, correlation analysis between colorimetric values and indicator components was conducted. Results The optimized honey-processing parameters for EF were determined as follows: honey-to-water ratio of 1:1.06, solid-to-liquid ratio of 2.0:1, moistening time of 2.5 h, stir-frying temperature of 157.9 ℃, and stir-frying duration of 11.1 min. In the established fingerprint profile of triterpenic acids in EF, 12 common peaks were identified in the raw products, while nine common peaks were identified in the processed products. Among these, four peaks were assigned as maslinic acid (peak 6), corosolic acid (peak 7), oleanolic acid (peak 11), and ursolic acid (peak 12), all of which showed increased content after honey-processing. In the fingerprint profile of organic acids, 11 common peaks were identified in the raw products, and 12 common peaks were found in the processed products. Four of these peaks were identified as neochlorogenic acid (peak 1), chlorogenic acid (peak 3), cryptochlorogenic acid (peak 4), and hyperoside (peak 11)-all of which decreased in content after honey-processing. The colorimetric values (L*, a*, b*) of the honey-processed loquat slices showed a significant positive correlation with the content of triterpenic acids, and a significant negative correlation with the content of organic acids and flavonol glycosides. Conclusion The AHP-CRITIC weighting method combined with BBD-RSM can effectively balance multiple indicators. The honey-frying process for EF is stable and feasible. Integrating fingerprints with chemometric methods precisely characterizes quality changes before and after processing, offering evidence for enhanced quality control standards.
[中图分类号]
R283.6
[基金项目]
国家自然科学基金项目(81874345);沈阳市中青年科技创新人才支持计划项目(RC200174);2022年辽宁省自然科学基金资助面上项目(2022-MS-223);国家中医药管理局重点实验室研究领域的中医临床疗效提升项目(2100222179);朱月信全国老药工传承工作室项目