[关键词]
[摘要]
目的 建立心痛泰颗粒的HPLC指纹图谱,为其质量评价提供依据。方法 采用Phenomenext Luna C18柱(250 mm×4.6 mm,5μm)色谱柱,以0.1%甲酸溶液-甲醇为流动相,检测波长为280 nm,体积流量为1.0 mL/min;柱温为30℃。测定10批心痛泰颗粒样品,应用中药色谱指纹图谱相似度评价系统(2012版)建立心痛泰颗粒指纹图谱共有模式图,并计算相似度,再通过对照品色谱图对共有峰进行指认。结果 通过10批样品的测定,建立心痛泰颗粒HPLC指纹图谱,相似度均在0.95以上,共标定26个共有色谱峰,共有峰全部归属到各药材,其中3个共有峰(21、22、26号峰)为丹参专属,8个共有峰(4~10、16号峰)为葛根专属,7个共有峰(13、15、17~20、23号峰)为枳壳专属,12号峰为川芎专属,14号峰为甘草专属,1号峰为三七与甘草共有,2号峰为三七、木香与山楂共有,3号峰为川芎与木香共有,11号峰为葛根与郁金共有,24号峰为川芎与枳壳共有,25号峰为郁金与枳壳共有,并通过对照品色谱图对共有峰进行指认,7、12、22、26号峰分别为葛根素、阿魏酸、丹酚酸B、丹参酮IIA。结论 10批样品相似度结果表明该颗粒制备工艺方法稳定可行,同时建立的HPLC指纹图谱方法稳定可靠,可以用于衡量心痛泰颗粒生产过程的稳定性和成品质量的可控性。
[Key word]
[Abstract]
Objective To establish an HPLC method for fingerprint analysis of Xintongtai Granules (XG) for its quality control. Methods The chromatographic behaviors were obtained by a Phenomenext Luna C18 column (250 mm×4.6 mm, 5 μm) with gradient elution using 0.1% formic acid solution-methanol as the mobile phase. The detection wavelength was 280 nm, the volume flow rate was 1.0 mL/min, and the column temperature was 30℃. The samples of 10 batches of XG were determined, and the chromatographic fingerprint similarity evaluation system of Chinese medicine (2012 edition) was used to establish the common pattern of XG fingerprints, and the similarity was calculated. Then the common peaks were identified by the reference chromatogram. Results HPLC fingerprints of XG were established by the determination of 10 batches of samples. The similarity was above 0.95. A total of 26 common peaks were calibrated. Three mutual peaks (No. 21, 22, 26 peaks) were from Salviae Miltiorrhizae Radix et Rhizoma, eight mutual peaks (No. 4-10, 16 peaks) were from Puerariae Lobatae Radix, seven mutual peaks (No. 13, 15, 17-20, 23 peaks) were from Aurantii Fructus, No. 12 peak was from Chuanxiong Rhizoma, No. 14 peaks was from Glycyrrhizae Radix et Rhizoma, No. 1 peak was shared by Notoginseng Radix et Rhizoma and Glycyrrhizae Radix et Rhizoma, No. 2 peaks was shared by Notoginseng Radix et Rhizoma, Aucklandiae Radix, and Crataegi Fructus, No. 3 peaks was shared by Chuanxiong Rhizoma and Aucklandiae Radix, No. 11 peaks was shared by Puerariae Lobatae Radix and Curcumae Radix, the No. 24 peaks was shared by Chuanxiong Rhizoma and Aurantii Fructus, and No. 25 peaks was shared by Curcumae Radix and Aurantii Fructus. The common peaks were all assigned to each medicinal material and identified by reference chromatograms:No. 7, 12, 22, and 26 peaks were puerarin, ferulic acid, salvianolic acid B, and tanshinone IIA. Conclusion The similarity results of 10 batches of samples indicate that the particle preparation process is stable and feasible, and the established HPLC fingerprint method is stable and reliable. It can be used to measure the stability of XG production process and the controllability of finished product quality.
[中图分类号]
[基金项目]
国家自然科学基金资助项目(81673955);湖南省自然科学基金资助项目(2017JJ2206);湖南中医药大学中药学一流学科建设项目(4901-0200002006);湖南省大学生创新创业训练计划项目(S201910541009)