芩连胶囊HPLC指纹图谱研究及多指标成分定量分析  

Study on HPLC fingerprint and multi-index determination of Qinlian capsules

作　　者：周娟娟 吴嫣艳 冯友龙 田京歌 ZHOU Juan-juan;WU Yan-yan;FENG You-long;TIAN Jing-ge(Jiangsu Institute for Food and Drug Control,Nanjing 210019,China)

机构地区：[1]江苏省食品药品监督检验研究院,南京210019

出　　处：《药物分析杂志》2022年第2期253-262,共10页Chinese Journal of Pharmaceutical Analysis

摘　　要：目的:建立芩连胶囊的HPLC指纹图谱,并同时测定芍药苷、盐酸黄连碱、连翘酯苷A、盐酸小檗碱、盐酸巴马汀、黄芩苷、甘草酸7个指标性成分的含量。方法:采用Agela Durashell RP C_(18)(4.6 mm×250 mm,5μm)色谱柱,以甲醇-0.05 mol·L^(-1)磷酸二氢钾水溶液(含0.05%磷酸)为流动相进行梯度洗脱,流速1.0 mL·min^(-1),柱温35℃,检测波长分别为230 nm(芍药苷、甘草酸)、280 nm(黄芩苷)和346 nm(盐酸黄连碱、连翘酯苷A、盐酸小檗碱、盐酸巴马汀)。结果:建立了芩连胶囊的HPLC指纹图谱,共确定了20个共有峰,利用相似度评价系统对20批样品指纹图谱进行分析,各批样品相似度均在0.97以上。在建立的色谱条件下,定量分析的7个成分分离度良好,方法精密度和重复性的RSD均<2.0%,供试品溶液在48 h内稳定,各成分具有良好的线性关系和较宽的线性范围,加样回收率为96.5%~101.9%,RSD为0.30%~1.9%;20批芩连胶囊中芍药苷、盐酸黄连碱、连翘酯苷A、盐酸小檗碱、盐酸巴马汀、黄芩苷、甘草酸的含量范围分别为6.95~14.37、0.27~2.46、3.47~8.43、9.82~17.80、1.90~3.55、13.12~25.90、1.64~4.40 mg·g^(-1)。结论:所建立的HPLC指纹图谱方法和多指标成分测定方法可有效地评价芩连胶囊的质量。Objective:To establish HPLC fingerprint of Qinlian capsules and simultaneously determine the contents of seven components including paeoniflorin,coptisine hydrochloride,forsythoside A,berberine hydrochloride,palmatine hydrochloride,baicalin and glycyrrhizic acid.Methods:The HPLC analysis was performed on a column of Agela Durashell RP C_(18)(250 mm×4.6 mm,5μm)with gradient elution of methanol-0.05 mol·L^(-1) potassium dihydrogen phosphate aqueous solution containing 0.05%phosphoric acid at a flow rate of 1.0 mL·min^(-1).The detection wavelengths were 230 nm for paeoniflorin and glycyrrhizic acid,280 nm for baicalin,346 nm for coptidine hydrochloride,forsythin A,berberine hydrochloride and palmatine hydrochloride,and the column temperature was 35℃.Results:The HPLC fingerprint of Qinlian capsules was stablished and 20 commonpeaks were found.The similarities of 20 batches of samples were above 0.97.The seven compounds were well separated under the chromatographic conditions.The RSD values for precision and repeatability were all less than 2.0%and the test solution was stable in 48 h.Seven compounds showed good linearities and wide linear ranges,whose recoveries were 96.5%-101.9%with the RSDs of 0.30%-1.9%.The contents of paeoniflorin,coptisine hydrochloride,forsythoside A,berberine hydrochloride,palmatine hydrochloride,baicalin and glycyrrhizic acid in 20 batches of Qinlian capsules were 6.95-14.37,0.27-2.46,3.47-8.43,9.82-17.80,1.90-3.55,13.12-25.90 and 1.64-4.40 mg·g^(-1),respectively.Conclusion:The method of HPLC fingerprint analysis and multi-index components determination is simple and accurate,which can be used for the quality control of Qinlian capsules.

关 键 词：芩连胶囊 多指标成分定量分析 芍药苷 盐酸黄连碱 连翘酯苷A 盐酸小檗碱 盐酸巴马汀 黄芩苷 甘草酸 指纹图谱 质量控制 

分 类 号：R917[医药卫生—药物分析学]