基于高效液相色谱法定性定量跟踪的大黄结合型与游离型蒽醌分离及纯化初步研究  

Preliminary study on the separation and purification of combined and free anthraquinones in Rhei Radix et Rhizoma based on HPLC qualitative and quantitative tracking

作　　者：郁文刘 张月月 窦志华 YU Wen-liu;Zhang Yue-yue;DOU Zhi-hua(School of Pharmacy,Nantong University,Jiangsu Nantong 226006,China;Department of Pharmacy,Nantong Third Hospital Affiliated to Nantong University,Jiangsu Nantong 226006,China)

机构地区：[1]南通大学药学院,江苏南通226006 [2]南通大学附属南通第三医院药学部,江苏南通226006

出　　处：《中国医院药学杂志》2022年第19期1995-2001,共7页Chinese Journal of Hospital Pharmacy

基　　金：江苏省重点研发计划(社会发展)项目(编号:BE2018674);江苏省中医药科技计划项目(编号:YB201836)。

摘　　要：目的:考察大黄中结合型与游离型蒽醌分离及纯化方法。方法:采用高效液相色谱(HPLC)法对大黄药材中8个结合型蒽醌及5个游离型蒽醌含量进行测定,采用Triple-Q-TOF/MS技术对大黄药材色谱图中主要色谱峰成分进行鉴定,95%乙醇提取大黄药材中的蒽醌类成分,提取液回收乙醇后加水沉淀,分离为结合型蒽醌和游离型蒽醌2个部位,分别采用碱性醇沉法和氯仿-酸水双相萃取法对结合型蒽醌和游离型蒽醌进行初步纯化,并结合HPLC-DAD法在280 nm和430 nm 2个波长下进行定性定量跟踪。结果:大黄药材中检测到的43个主要成分全部转移到了提取液中,经纯化处理后,结合型蒽醌部位杂质明显减少,游离型部位纯度从19.98%提高到92.97%。结论:考察的方法可用于大黄结合型与游离型蒽醌初步分离及纯化。OBJECTIVE To investigate the separation and purification methods for combined and free anthraquinones in Rhei Radix et Rhizoma.METHODS HPLC was used to determine the contents of eight combined anthraquinones and five free anthraquinones in Rhei Radix et Rhizoma.The components of main chromatographic peaks in the chromatogram of Rhei Radix et Rhizoma were identified by Triple-Q-TOF/MS.Anthraquinones in Rhei Radix et Rhizoma were extracted by 95%ethanol.After recovering ethanol and adding water,the extract was centrifuged and separated into two parts of combined and free anthraquinones.Combined anthraquinones and free anthraquinones were purified by the methods of alkaline alcohol precipitation and chloroform acid water two-phase extraction,respectively,and qualitatively and quantitatively detected at 280 nm and 430 nm by HPLC-DAD.RESULTS All the 43 components detected in Rhei Radix et Rhizoma were transferred to the extract.After purification,the impurities in combined anthraquinones were significantly reduced,and the purity of free anthraquinones was increased from 19.98%to 92.97%.CONCLUSION The investigated method can be used for the preliminary separation and purification of combined and free anthraquinones in Rhei Radix et Rhizoma.

关 键 词：大黄 蒽醌 结合型蒽醌 蒽醌苷 游离型蒽醌 分离 

分 类 号：R927.2[医药卫生—药学]