罗才琴, 肖素芸, 吕冬, 曲媛, 崔秀明, 段嫏环. 三乌胶丸HPLC指纹图谱及多指标成分定量分析研究[J]. 云南大学学报(自然科学版), 2022, 44(1): 150-159. doi: 10.7540/j.ynu.20210394
引用本文: 罗才琴, 肖素芸, 吕冬, 曲媛, 崔秀明, 段嫏环. 三乌胶丸HPLC指纹图谱及多指标成分定量分析研究[J]. 云南大学学报(自然科学版), 2022, 44(1): 150-159. doi: 10.7540/j.ynu.20210394
LUO Cai-qin, XIAO Su-yun, LYU Dong, QU Yuan, CUI Xiu-ming, DUAN Lang-huan. Study on HPLC fingerprint and multi-indicator quantitative analysis of Sanwujiaowan[J]. Journal of Yunnan University: Natural Sciences Edition, 2022, 44(1): 150-159. DOI: 10.7540/j.ynu.20210394
Citation: LUO Cai-qin, XIAO Su-yun, LYU Dong, QU Yuan, CUI Xiu-ming, DUAN Lang-huan. Study on HPLC fingerprint and multi-indicator quantitative analysis of Sanwujiaowan[J]. Journal of Yunnan University: Natural Sciences Edition, 2022, 44(1): 150-159. DOI: 10.7540/j.ynu.20210394

三乌胶丸HPLC指纹图谱及多指标成分定量分析研究

Study on HPLC fingerprint and multi-indicator quantitative analysis of Sanwujiaowan

  • 摘要: 建立三乌胶丸的HPLC指纹图谱及定量研究多种指标性成分的方法,为三乌胶丸的质量评价提供实验根据. 色谱分析柱型号为Agilent ZORBAX Eclipse Plus C18,进行梯度洗脱,柱温为30 ℃,流速为1.0 mL/min,测定波长245 nm,流动相为0.2%二乙胺(磷酸调节其pH为4.0)水溶液(A)−乙腈(B). 结果表明,建立的15批次三乌胶丸的HPLC指纹图谱一共确定了18个共有峰,辨别了指纹图谱中的6个成分,15批三乌胶丸指纹图谱的相似度均大于0.9. 8−去乙酰滇乌碱、苯甲酰新乌头原碱、苯甲酰次乌头原碱、苯甲酰乌头原碱、大黄素、草乌甲素6个成分的质量分数依次为87.291~1182.018、144.150~2193.629、30.307~2229.562、100.810~646.250、4.474~114.140、4.255~13.591 μg/g. 通过CA、PCA、PLS-DA等分析,15个批三乌胶丸按照生产年限被分成2类. 所建立的三乌胶丸HPLC 指纹图谱及6种成分定量分析的方法易操作,重复性好,可为三乌胶丸的质量研究提供参考.

     

    Abstract: A HPLC fingerprint of Sanwujiaowan and a method for the determination of six components in Sanwujiaowan were built, so as to provide experiment basis for its quality evaluation. The chromatographic conditions were that using Agilent ZORBAX Eclipse Plus C18 (ϕ4.6 mm × 250 mm, 5 μ m) liquid chromatographic column, using gradient elution, the temperature of the liquid-analysis column was at 30 ℃ and the wavelength of the detection were set at 245 nm, the flow velocity was set at 1.0 mL/min, the mobile phase is 0.2% diethylamine (phosphoric acid adjusted its pH to 4.0) aqueous solution (A)-acetonitrile (B). The fingerprints of 15 batches of Sanwujiaowan were established, 18 common peaks and 6 components were identified, and their similarity was more than 0.9. The contents of benzoylmesaconine, benzoylaconitine, benzoylhypacoitine, 8-deacetylyunaconitine, emodin and crassicauline A were 144.150~2193.629, 30.307~2229.562, 100.810~646.250, 87.291~1182.018, 4.474~114.140 , 4.255~13.591 μg/g respectively. Through the analysis of CA, PCA and PLS-DA, 15 batches of Sanwujiaowan were divided into 2 types. The HPLC fingerprint and six components quantitative analysis methods established in this paper are easy to operate and reproducible, which can offer reference for the quality research of Sanwujiaowan.

     

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