近红外测定丹参提取浓缩过程中的丹参酮类的含量  

Process Quality Control of Tanshinones in Salvia miltiorrhizawithin the extraction and concentration of Fufangdanshen Tabletsby Near Infrared Spectroscopy

作　　者：张偲偲 王德勤[1] 朱晶晶[2] 李楚源[1] 王智民[2] 匡艳辉[1] ZHANG Si-si;WANG De-qin;ZHU Jing-jing;LI Chu-yuan;WANG Zhi-min;KUANG Yan-hui(Guangzhou Baiyun Mountain and Hutchison Whampoa Ltd.,Guangzhou 510515,China;Institute of Chinese Materia Medica,China Academy of Chinese Medical Sciences,Beijing)

机构地区：[1]广州白云山和记黄埔中药有限公司,广州510515 [2]中国中医科学院中药研究所,北京100700

出　　处：《人参研究》2021年第3期15-20,共6页Ginseng Research

基　　金：广东省重点领域研发计划项目:中成药大品种复方丹参片上市后再评价研究,项目编号:2020B1111110002;国家发改委、国家中医药管理局中药标准化项目:复方丹参片标准化研究,项目编号:ZYBZH-C-GD-05。

摘　　要：目的利用近红外技术(NIR)研究复方丹参片中丹参的提取浓缩过程中丹参酮类成分的监测模型,实现生产过程中的在线质量监控。方法利用NIR光谱扫描在线监测检测技术,以丹参的提取浓缩过程中的样品为研究对象,关联UPLC检测技术和化学计量学的数据处理方法,建立二氢丹参酮、隐丹参酮、丹参酮Ⅰ和丹参酮ⅡA的NIR模型。结果二氢丹参酮的最佳波段分别为12489.3-7498.3cm^(-1)和6102~5446.3 cm^(-1),决定系数(R2)=98.47,相对分析误差(RPD)为8.09,内部交叉均方差分别为(RMSECV)=5.21;隐丹参酮的最佳波段为6102~5446.3 cm^(-1),RMSECV=23.9,R2=97.41,RPD为6.22;丹参酮Ⅰ的最佳波段为6102~5446.3 cm^(-1),RMSECV=13.8,R2=98.21,RPD为7.48和丹参酮ⅡA的最佳波段为7502.1~5446.3 cm^(-1),RMSECV=112,R2=98.13,RPD为7.31,验证集样品的验证结果的相对误差均在5%以内。结论建立的二氢丹参酮、隐丹参酮、丹参酮Ⅰ和丹参酮ⅡA的模型预测性良好,可用于丹参的提取浓缩的实时监控和质量控制。Objective To establish the monitoring models of tanshinonesin Salvia miltiorrhiza(SM)in the extraction and concentration processes by near-infrared spectroscopy(NIRs)and to realize on-line quality controls in the manufacturingprocesses of Fufangdanshen(FFDS)Tablets,in which the composition include salviaemiltiorrhizae radix et rhizoma,notoginseng radix et rhizome and borneolumsyntheticum.Methods Based on the NIRs data collected from the extraction and concentration of SM,the analytical method and dependency modelfor dihydrotanshinone,cryptotanshinone,tanshinoneⅠand tanshinoneⅡA were established by UPLC,stoichiometry and NIRs,respectively.Results The best wavebands of dihydrotanshinonewere within 12489.3-7498.3 cm^(-1) and 6102-5446.3 cm^(-1),the determination coefficient,the root-mean-squares error of cross-validation(RMSECV)and regression point displacement(RPD)were 98.47,5.21 and 8.09,respectively.The best wavebands ofcryptotanshinonewere within6102-5446.3 cm^(-1).The determination coefficient,the RMSECVand RPD were97.41,23.9 and 6.22,respectively.The best waveband of tanshinoneⅠwere within 6102~5446.3 cm^(-1).The determination coefficient,RMSECVand RPDwere 98.21,13.8 and 7.48,respectively.The best waveband of tanshinoneⅡAwere within 7502.1-5446.3 cm^(-1).The determination coefficient,RMSECV and RPD were 98.13,112 and 7.48,respectively.When this model was used for validation of these four constituents,their relative errors were2.63%,3.35%,0.69%and 2.51%,respectively.The relative standard deviationof the established modelswere within 5%.Conclusion The models with good predictability can be applied to the real time monitoring and process quality control of dihydrotanshinone,cryptotanshinone,tanshinoneⅠand tanshinoneⅡA in the production of FFDS Tablets.

关 键 词：近红外 复方丹参片 二氢丹参酮 隐丹参酮 丹参酮Ⅰ 丹参酮ⅡA 相关性模型 

分 类 号：R284.2[医药卫生—中药学]