摘要
目的:建立基于标准汤剂的番泻叶(狭叶番泻)配方颗粒的质量标准。方法:建立15批番泻叶(狭叶番泻)标准汤剂和10批不同厂家番泻叶(狭叶番泻)配方颗粒的高效液相色谱法(HPLC)特征图谱,并进行相似度评价、层次聚类分析(HCA)及主成分分析(PCA)。针对特征图谱中的共有峰建立双标线性校正法(LCTRS)、一测多评法(QAMS),测定饮片、标准汤剂与配方颗粒中主要成分的含量,计算从饮片到标准汤剂及配方颗粒的转移率。结果:15批番泻叶(狭叶番泻)标准汤剂和10批番泻叶(狭叶番泻)配方颗粒特征图谱相似度均>0.95,共确定8个特征峰,并指认山柰酚-3,7-O-二葡萄糖苷、芹菜素-6,8-二-C-葡萄糖苷、槲皮素-3-O-龙胆二糖苷、番泻苷B、番泻苷A 5个成分。HCA、PCA结果表明,不同批次标准汤剂成分有一定差异性,但未表现出产地聚集性。15批番泻叶(狭叶番泻)标准汤剂出膏率26.54%~45.38%,山柰酚-3,7-O-二葡萄糖苷、芹菜素-6,8-二-C-葡萄糖苷、槲皮素-3-O-龙胆二糖苷、番泻苷B、番泻苷A质量分数分别为12.16~19.26、2.57~4.94、3.27~5.11、6.75~11.39、4.69~7.79 mg·g^(-1),这5个成分从饮片到标准汤剂的转移率分别为45.41%~79.02%、29.12%~55.07%、40.52%~67.90%、24.72%~49.12%、27.54%~49.34%。番泻叶(狭叶番泻)配方颗粒样品C8~C10的出膏率38.10%~39.50%,上述5个成分从饮片到配方颗粒的转移率分别为72.85%~73.58%、53.43%~53.94%、40.19%~40.74%、24.62%~25.00%、28.65%~29.11%,与饮片到标准汤剂的转移率基本一致。结论:LCTRS的预测精度更高,适用色谱柱较多,明显优于相对保留时间法。基于标准汤剂建立的番泻叶(狭叶番泻)配方颗粒质量控制标准合理可靠,不同厂家样品各项指标均在基于标准汤剂规定的范围内,可为该配方颗粒的质量控制及工艺研究提供参考。
Objective:To establish the quality standards for Sennae Folium(Cassia angustifolia)dispensing granules based on standard decoctions.Methods:High performance liquid chromatography(HPLC)specific chromatograms were established for 15 batches of Sennae Folium(C.angustifolia)standard decoctions and 10 of Sennae Folium(C.angustifolia)dispensing granules from different manufacturers,and the similarity evaluation,hierarchical cluster analysis(HCA)and principal component analysis(PCA)were performed.Linear calibration with two reference substances(LCTRS)and quantitative analysis of multi-components by single-marker(QAMS)were established for the common peaks in the specific chromatograms to determine the contents of main components in the decoction pieces,standard decoctions and dispensing granules,and to calculate their transfer rates from decoction pieces to standard decoctions and dispensing granules.Results:The similarities of specific chromatograms of 15 batches of Sennae Folium(C.angustifolia)standard decoctions and 10 batches of Sennae Folium(C.angustifolia)dispensing granules were all greater than 0.95,and a total of 8 characteristic peaks were calibrated,and five of them were identified,including kaempferol-3,7-O-diglucoside,apigenin-6,8-di-C-glucoside,quercetin-3-O-gentianoside,sennoside B and sennoside A.HCA and PCA results showed that there were certain differences in the composition of different batches of standard decoctions,but no clustering was observed in the production area.As the standard decoctions,the extract rate of 15 batches of samples was 26.54%-45.38%,the contents of kaempferol-3,7-O-diglucoside,apigenin-6,8-di-C-glucoside,quercetin-3-O-gentianoside,sennoside B and sennoside A were 12.16-19.26,2.57-4.94,3.27-5.11,6.75-11.39,4.69-7.79 mg·g^(-1),and their transfer rates from decoction pieces to standard decoctions were 45.41%-79.02%,29.12%-55.07%,40.52%-67.90%,24.72%-49.12%,27.54%-49.34%,respectively.The extract rates of Sennae Folium(C.angustifolia)dispensing granules(C8-C10)were 38.10%-39.50%,the transfer rates of the above five components from decoction pieces to dispensing granules were 72.85%-73.58%,53.43%-53.94%,40.19%-40.74%,24.62%-25.00%,28.65%-29.11%,respectively,which were generally consistent with the transfer rates from decoction pieces to standard decoctions.Conclusion:Compared with the relative retention time method,LCTRS has higher prediction accuracy and is more suitable for chromatographic columns.The established quality control standard of Sennae Folium(C.angustifolia)dispensing granules based on standard decoction is reasonable and reliable,and all indicators of samples from different manufacturers are within the range specified based on the standard decoction,which can provide reference for the quality control and process research of this dispensing granules.
作者
李金鑫
董雪
段帅
曹桂云
张京华
栾永福
林永强
董晓弟
孟兆青
LI Jinxin;DONG Xue;DUAN Shuai;CAO Guiyun;ZHANG Jinghua;LUAN Yongfu;LIN Yongqiang;DONG Xiaodi;MENG Zhaoqing(Shandong Technical Innovation Center for Traditional Chinese Medicine Treatment of Respiratory Diseases,Shandong Hongjitang Pharmaceutical Group Co.Ltd.,Jinan 250103,China;Shandong Institute for Food and Drug Control,Jinan 250101,China)
出处
《中国实验方剂学杂志》
北大核心
2025年第9期192-200,共9页
Chinese Journal of Experimental Traditional Medical Formulae
基金
山东省重点研发计划重大科技创新工程项目(2021CXGC010511)
泉城“5150”引才倍增计划项目(2021年)。
关键词
番泻叶
标准汤剂
配方颗粒
双标线性校正法(LCTRS)
一测多评法(QAMS)
特征图谱
质量控制
高效液相色谱法(HPLC)
Sennae Folium
standard decoction
dispensing granules
linear calibration with two reference substances(LCTRS)
quantitative analysis of multi-components by single-marker(QAMS)
specific chromatograms
quality control
high performance liquid chromatography(HPLC)
