摘要
目的:建立黄连解毒汤的指纹图谱,测定其中8种成分的含量,并进行正交偏最小二乘判别法(OPLS-DA)分析。方法:采用HPLC法,色谱柱为Sepax Bio-C_(18),流动相为甲醇-0.05%磷酸溶液(梯度洗脱),检测波长为238 nm,柱温为35℃,流速为0.6 mL·min^(-1)。采用《中药色谱指纹图谱相似度评价系统》2012年版进行相似度评价,确定共有峰,并测定其中8种成分的含量;采用SIMCA 14.0软件进行OPLS-DA分析,并利用分析变量重要性投影值(VIP)筛选影响其质量的标志物。结果:10批黄连解毒汤共有18个共有峰,与对照指纹图谱的相似度均>0.98;共指认了8个色谱峰并分别测定了含量,各成分在考察的范围内线性良好,r值在0.999 1~0.999 9之间,平均加样回收率为97.89%~100.10%(RSD为1.19%~2.36%,n=6)。OPLS-DA分析结果显示,盐酸小檗碱、栀子苷、黄芩苷是影响黄连解毒汤质量的主要成分物质。结论:结合多元统计分析,建立的指纹图谱和含量测定方法准确、稳定、可行,可用于黄连解毒汤的质量控制。
Objective: The fingerprint of Huanglian Jiedu Decoction was established, the contents of 8 components were determined, and the orthogonal least squares criterion(OPLS-DA) was analyzed. Methods: The contents of 8 components were determined by HPLC with a Sepax Bio-C_(18) column applying the mobile phase of methanol-0.05% phosphate solution in a gradient elution. The flow rate was 0.6 mL·min^(-1), the detection wavelength was set at 238 nm, and the column temperature was 35 ℃. The similarity was evaluated with “TCM Chromatographic Fingerprint Similarity Evaluation System”(2012 Edition) by determining common peaks and the contents of 8 components. Finally, OPLS-DA analysis with SIMCA 14.0 software and the analytical variable importance projection(VIP) values was used to screen the markers. Results: There were 18 peaks in 10 batches of Huanglian Jiedu Decoction with the similarity above 0.98. A total of 8 chromatographic peaks were identified and determined. Each component was linearly in the range with r value of 0.999 1~0.999 9 and average sample recovery of 97.89%~100.10%(RSD 1.19%~2.36%, n=6). The OPLS-DA analysis results showed that berberine hydrochloride, gardeniside and baicalin are the main components evaluating the quality of Huanglian Jiedu Decoction. Conclusion: Combined with the multivariate statistical analysis, the established fingerprint map and content determination method are accurate, stable and feasible, which can be used for quality control of Huanglian Jiedu Decoction.
作者
李军鸽
邱智东
赵莹
王永春
孟珈同
唐秋竹
LI Jun-ge;QIU Zhi-dong;ZHAO Ying;WANG Yong-chun;MENG Jia-tong;TANG Qiu-zhu(Innovation Practice Center,Changchun University of Chinese Medicine,Changchun 130117,China;College of Pharmacy,Changchun University of Chinese Medicine,Changchun 130117,China)
出处
《中国新药杂志》
CAS
CSCD
北大核心
2022年第15期1524-1530,共7页
Chinese Journal of New Drugs
基金
吉林省中医药事业传承发展资金支持项目《重大疫情防治中药方剂储库备建设项目》(吉中医药发[2021]11号)。
关键词
黄连解毒汤
指纹图谱
含量测定
聚类分析
Huanglian Jiedu Decoction
fingerprint
content determination
cluster analysis