基于全方特征图谱质量表征的芩连制剂质量评价研究  

Quality evaluation of Qinlian preparations based on quality characterization of whole prescription characteristic spectrum

作　　者：彭平 熊少哲 张蓓 易剑平 杜菁 杨璇 范国强 顾海鸥 王志斌 PENG Ping;XIONG Shao-zhe;ZHANG Bei;YI Jian-ping;DU Jing;YANG Xuan;FAN Guo-qiang;GU Hai-ou;WANG Zhi-bin(Pharmaceutical Factory of Beijing Tongrentang Technology Development Co.,Ltd.,Beijing 100079,China;Beijing Tongrentang Group Co.,Ltd.,Beijing 100079,China)

机构地区：[1]北京同仁堂科技发展股份有限公司制药厂,北京100079 [2]中国北京同仁堂(集团)有限责任公司,北京100079

出　　处：《中草药》2021年第5期1312-1322,共11页Chinese Traditional and Herbal Drugs

基　　金：国家重点研发计划资助项目(2017YFC1702604)。

摘　　要：目的建立芩连制剂特征图谱质量表征方法,以全面表征芩连制剂质量,并应用于芩连制剂的质量评价。方法采用UHPLC-DAD多波长分析方法,Waters Cortecs T3(100 mm×2.1 mm,1.6μm)色谱柱,以乙腈(含0.02%甲酸)-(10 mol/L乙酸铵-0.09%甲酸缓冲液)为流动相,梯度洗脱,体积流量0.3 mL/min,柱温30℃,检测波长230、330 nm。结果建立了芩连制剂特征图谱质量表征方法,指认了38个特征峰,且检测了12个指标性成分的含量,平均加样回收率为83.58%~106.76%;测得11批芩连制剂中12个指标性成分质量分数分别为连翘酯苷A 0.21~9.08 mg/g、盐酸黄柏碱0.39~1.91 mg/g、芍药内酯苷0.13~9.28 mg/g、芍药苷3.02~20.24 mg/g、甘草苷0.19~0.51 mg/g、黄芩苷12.36~27.64 mg/g、1,2,3,4,6-五-O-倍酰-D-葡萄糖(PGG)0.22~3.63 mg/g、汉黄芩苷1.92~6.12 mg/g、连翘苷0.22~4.10 mg/g、盐酸小檗碱5.37~16.85 mg/g、盐酸巴马汀0.53~2.26mg/g、甘草酸0.45~2.06mg/g。不同厂家及其不同批次芩连制剂中成药的质量表征差异主要来源于黄芩(峰22、38、27)、赤芍[峰2、21(PGG)、7(芍药内酯苷)]、连翘[峰36(连翘酯素)、30]、黄连(峰24)、黄连-川黄柏(峰8、4)、连翘-赤芍(峰3)。结论建立的特征图谱质量表征方法可全面地表征与评价芩连制剂中成药,为该类品种的质量控制提供了科学依据,亦为中成药的质量控制提供方法学借鉴。Objective To establish the characteristic spectrum analysis method of Qinlian preparations,and comprehensively characterize the quality,so as to apply the established method to the quality evaluation of Qinlian preparation of Chinese patent medicine.Methods The UHPLC-PDA multi-wavelength was used in the method,and a Waters Cortecs T3 column(100 mm×2.1μm,1.6μm)was used,the mobile phase was acetionitrile with 0.02%formic acid and 10 mol/L ammonium acetate-0.09%formic acid buffer for gradient elution,and the flow rate was 0.3 m L/min,the column temperature was kept at 30℃,the detection wavelength was set at 230 nm and 330 nm.Results The characteristic spectrum of Qinlian preparations was established,38 characteristic peaks were marked,and 12 index components were determined.The recovery range for the content determination was 83.58%—106.76%,and the content range of 12 index components in 11 batches of Qinlian preparations was as follows:forsythoside A 0.21—9.08 mg/g;phellodendrine chloride 0.39—1.91 mg/g;albiflorin 0.13—9.28 mg/g;paeoniflorin 3.02—20.24 mg/g;liquiritin 0.19—0.51 mg/g;baicalin 12.36—27.64 mg/g;1,2,3,4,6-penta-O-galloyl-D-glucose(PGG)0.22—3.63 mg/g;oroxindin 1.92—6.12 mg/g;phillyrin 0.22—4.10 mg/g;berberine 5.37—16.85 mg/g;palmatine chloride 0.53—2.26 mg/g;glycyrrhizic acid 0.45—2.06 mg/g.Through analysis,the difference in quality characterization of Qinlian preparations was derived from Huangqin(Scutellariae Radix,peak 22,38,27),Chishao(Paeoniae Radix Rubra)[peak 2,21(PGG),7(albiflorin)],Lianqiao(Forsythiae Fructus)[peak 36(forsythingenin),30],Huanglian(Coptidis Rhizoma,peak 24),Coptidis Rhizoma-Chuanghuangbai(Phellodendri Chinensis Cortex)(peak 8,4),Forsythiae Fructus-Paeoniae Radix Rubra(peak 3).Conclusion In conclusion,the quality characterization method established in this study can comprehensively characterize and evaluate Qinlian preparations,thus providing scientific basis and methodological reference for the quality control of this kind of Chinese traditional pa

关 键 词：特征图谱质量表征 芩连制剂 质量评价 UHPLC-DAD 多波长分析法 连翘酯苷A 盐酸黄柏碱 芍药内酯苷 芍药苷 甘草苷 黄芩苷 1 2 3 4 6-五-O-倍酰-D-葡萄糖 汉黄芩苷 连翘苷 盐酸小檗碱 盐酸巴马汀 甘草酸 黄芩 赤芍 连翘 黄连 川黄柏 

分 类 号：R286.02[医药卫生—中药学]