经典名方桃核承气汤的UPLC指纹图谱及多指标成分含量测定研究

UPLC fingerprint and multi-index component content determination of classical herbal prescription Taohe Chengqi Decoction

目的通过建立UPLC指纹图谱及多指标成分含量测定方法,构建经典名方桃核承气汤(Taohe Chengqi Decoction,TCD)的质量体系,研究TCD基准样品量值传递规律。方法遵照古籍记载并结合工艺考察,制备不同产地的15批次TCD基准样品,采用UPLC法建立基准样品指纹图谱,使用中药色谱指纹图谱相似度评价软件(2012版)进行相似度评价,结合UPLC-Q-Exactive Orbitrap-MS技术全面分析基准样品化学成分,同时测定样品中指标成分(苦杏仁苷、桂皮醛、肉桂酸、甘草酸、游离型蒽醌、总蒽醌、结合蒽醌)的含量。结果建立了15批TCD基准样品的UPLC指纹图谱,与对照指纹图谱比较相似度≥0.90,通过对照品确认、高分辨质谱数据分析及文献比对,共鉴定出80个化学成分,共归属26个指纹峰,鉴定了17个色谱峰。15批TCD基准样品中苦杏仁苷、桂皮醛、肉桂酸、甘草酸、游离型蒽醌、总蒽醌、结合蒽醌的质量分数分别为0.29%~0.58%、0.011%~0.032%、0.05%~0.13%、0.48%~1.04%、0.20%~0.30%、0.42%~0.66%、0.19%~0.37%,饮片到基准样品的转移率分别为31.49%~60.78%、0.43%~2.67%、51.61%~76.99%、26.79%~49.88%、16.01%~32.65%、9.66%~19.07%、6.97%~19.48%;出膏率为19.55%~22.92%,传递率为80.98%~99.34%。结论所建立的UPLC指纹图谱及多指标成分含量测定分析方法快速简便,结合基准样品的量值传递过程分析,可为后续制剂的开发和质量控制提供理论依据。

Objective The quality system of classical herbal prescription Taohe Chengqi Decoction(桃核承气汤,TCD)was established by establishing UPLC fingerprint and multi-index component content determination method,and the quantitative value transfer law of the benchmark samples of TCD was studied.Methods According to the records of ancient books and combined with technological investigation,15 batches of benchmark samples of TCD from different areas were prepared.The fingerprint of the benchmark sample was established by UPLC method,and the similarity was evaluated by“Similarity Evaluation Software of Chromatographic Fingerprint of Traditional Chinese Medicine”(version 2012).Combined with UPLC-Q-ExactiveOrbitrap-MS technology,the chemical components of the benchmark samples were analyzed comprehensively,and the contents of index components(amygdalin,cinnamaldehyde,cinnamic acid,glycyrrhizic acid,free anthraquinone,total anthraquinone and bound anthraquinone)in the samples were determined at the same time.Results The UPLC fingerprints of 15 batches of TCD benchmark samples were established,and the similarity between them and the control fingerprints was≥0.90.A total of 80 chemical constituents were identified,belonging to 26 fingerprint peaks of which 17 chromatographic peaks were identified through the confirmation of the reference substance,the analysis of high resolution mass spectrometry data and the comparison of literature.The mass fraction ranges of amygdalin,cinnamaldehyde,cinnamic acid,glycyrrhizic acid,free anthraquinone,total anthraquinone and bound anthraquinone were 0.29%-0.58%,0.011%-0.032%,0.05%-0.13%,0.48%-1.04%,0.20%-0.30%,0.42%-0.66%,0.19%-0.37%.The transfer rate of index component from the decoction pieces to the substance benchmaerk was in the range of amygdalin 31.49%-60.78%,cinnamaldehyde 0.43%-2.67%,cinnamic acid 51.61%-76.99%,glycyrrhizic acid 26.79%-49.88%,free anthraquinone 16.01%-32.65%,total anthraquinone 9.66%-19.07%,bound anthraquinone 6.97%-19.48%.The extract rate was in the range from 19.55%-22.92%,and the transmission rate was in the range from 80.98%-99.34%.Conclusion The established UPLC fingerprint and the determination and analysis method of multi-index component content are rapid and simple,combined with the quantitative value transfer process analysis of the benchmark sample,which can provide a theoretical basis for the development and quality control of follow-up preparations.