基于HPLC指纹图谱与含量测定的新保肾片生产过程质量控制研究

Quality Control of Xinbaoshen Tablets Based on HPLC Fingerprints and Content Determination

目的建立新保肾片生产过程中饮片、中间品、成品的高效液相色谱指纹图谱,并对5种游离型蒽醌类化合物进行含量测定,分析化学成分群变化情况,以期为生产过程的质量控制提供依据。方法采用高效液相色谱法,色谱柱为Waters Symmetry C18(4.6 mm×250 mm,5μm),甲醇-0.1%磷酸梯度洗脱,检测波长:260 nm,体积流量为0.8 ml·min-1,柱温:30℃,建立大黄饮片-中间品-新保肾片成品的特征图谱,并对其进行相关性分析。同时采用HPLC法测定3类样品中芦荟大黄素、大黄酸、大黄素、大黄酚和大黄素甲醚的含量,分析生产过程中有效成分变化情况。结果建立了大黄饮片-中间品-新保肾片的多成分HPLC特征图谱,10批大黄相似度为0.929~0.988,共标定了24个共有峰,并指认出其中芦荟大黄素、大黄酸、大黄素、大黄酚和大黄素甲醚5个成分。10批中间品相似度为0.976~1.000,10批新保肾片相似度为0.988~0.997,相似度均较高,且5种成分含量测定结果无显著性差异。结论新保肾片生产过程较为稳定,所建方法简单、可靠,可为新保肾片工艺研究、过程质量控制提供参考。

Objective To establish the HPLC fingerprints of raw materials,intermediate products and finished products in the process of producing Xinbaoshen tablets,determine the contents of five free anthraquinone compounds,and analyze the changes of chemical components so as to provide data for quality control during production.Methods The fingerprints were established on the Waters Symmetry C18(4.6 mm×250 mm,5μm)column at 30℃,with a gradient mobile phase composed of methanol-0.1%phosphoric acid solution.The flow rate was 0.8 ml·min-1 while the detection wavelength was 260 nm.The similarity of fingerprints was evaluated by the“Similarity Evaluation System for Chromatographic Fingerprints of TCM”(2012 edition)software.Correlations between them were analyzed.The contents of aloe emodin,rhein,emodin,chrysophanol and emodin methyl ether in three types of samples were determined by HPLC,and the variations of these effective components in the process of production were analyzed.Results The multi-component HPLC specific chromatograms of Rhubarb,intermediate products,and Xinbaoshen tablets were established.The similarity of ten batches of Rhubarb ranged from 0.929 to 0.988.Twenty-four common peaks were marked,and the five components were identified as aloe emodin,rhein,emodin,chrysophanol and emodin methyl ether.The similarity of ten batches of intermediate products and Xinbaoshen tablets ranged from 0.976 to 1.000 and from 0.988 to 0.997 respectively,suggesting the production process was stable.There was no significant difference in the contents of the five components between intermediate products and Xinbaoshen tablets.Conclusion The production process of Xinbaoshen tablets is stable,and the established method is simple and reliable,which can provide reference for the process research and quality control of Xinbaoshen tablets.