结合逐步敲入策略与制剂工艺过程的肾宝片复杂成分辨识

Identification of complex components of Shenbao Pian based on stepwise knockin strategy and preparation process

目的结合肾宝片处方22味药材组成及其制剂工艺过程,阐明肾宝片提取物(浸膏)的化学成分,为肾宝片质量控制提供依据。方法采用UPLC分别建立浸膏1与浸膏2的指纹图谱,将浸膏1、2成分与全浸膏对应,按照浸膏1、2逐步敲入的方式,验证全浸膏中的成分,并利用UPLC-Q-TOF-MS快速鉴定各浸膏中的成分。结果基于UPLC重点分析表征了全浸膏中朝藿定A、B、C及淫羊藿苷、松果菊苷、毛蕊花糖苷、补骨脂素、异补骨脂素等21个成分;利用UPLC-QTOF-MS从浸膏1中共鉴定了朝藿定A、人参皂苷Rg1、人参皂苷Ro等17个化合物,浸膏2中鉴定了松果菊苷、毛蕊花糖苷、甘草苷、大黄素等58个化合物,从全浸膏中共鉴定了宝藿苷I、人参皂苷Rb1、甘草酸、毛蕊花糖苷等82个化合物,涵盖了处方中22味药材,主要组分包括淫羊藿黄酮组分、人参皂苷组分、制何首乌蒽醌组分、黄芪皂苷组分、肉苁蓉苯乙醇苷组分与补骨脂香豆素组分。结论基于UPLC-Q-TOF-MS对肾宝片的化学成分进行了较为全面的分析,为其物质基础及制剂工艺过程的质量控制提供了实验依据。

Objective To elucidate chemical constituents and provide references for the quality control of the extract of Shenbao Pian based on the composition of 22 kinds of herbs from Shenbao Pian and its preparation process. Methods The fingerprints of extractum 1 and extractum 2 were established separately by UPLC. The components in the total extractum were compared and verified according to the stepwise knock-in of extractum 1 and extractum 2. Meanwhile, UPLC-Q-TOF-MS was used to rapidly identify the compounds in the extract of Shenbao Pian. Results A total of 21 chemical constituents(epimedin A, epimedin B, epimedin C, icariin, echinacoside, verbascoside, psoralen, isopsoralen, and etc) from the total extractum were characterized based on UPLC. A total of 17 compounds(epimedin A, ginsenoside Rg1, ginsenoside Ro, and etc) in extractum 1, 58 compounds(echinacoside, verbascoside, liquiritin, emodin, and etc) in extractum 2 and 82 chemical constituents(baohuoside I, ginsenoside Rb1, glycyrrhizic acid, verbascoside, and etc) in total extractum were identified using UPLC-Q-TOF-MS, covering 22 herbs in the prescription, including Yinyanghuo(Epimedii Folium) flavonoid composition, ginsenosides composition, Zhiheshouwu(Polygoni Multiflori Radix Praeparata) anthraquinone composition, Huangqi(Astragali Radix) saponin composition, Roucongrong(Cistanches Herba) phenylethanolide composition and Buguzhi(Psoraleae Fructus) coumarin composition. Conclusion This study introduces a comprehensive analysis method for chemical ingredients in Shenbao Pian, and provide experimental foundation for the substance basis research and quality control.