摘要
目的:建立消栓肠溶胶囊HPLC指纹图谱并测定苦杏仁苷、芍药苷、阿魏酸、毛蕊异黄酮苷和藁本内酯的含量,为消栓肠溶胶囊的质量控制提供参考。方法:采用Diamonsil C_(18)(2)色谱柱(4.6 mm×250 mm,5μm),以乙腈(A)-0.1%磷酸水溶液(B)为流动相,梯度洗脱(0～5 min,8%A;5～12 min,8%A→15%A;12～20 min,15%A→37%A;20～28 min,37%A;20～45 min,37%A→50%A;45～65 min,50%A→65%A),流速1.0 mL·min^(-1),检测波长220 nm(0～30 min)和310 nm(30～65 min),柱温35℃。结果:在特征图谱研究中,共确定消栓肠溶胶囊HPLC指纹图谱21个共有峰,通过与混合对照品比较,指认其中5个指标成分:苦杏仁苷(2号峰)、芍药苷(10号峰)、阿魏酸(14号峰)、毛蕊异黄酮苷(17号峰)和藁本内酯(20号峰),利用相似度软件对12批样品指纹图谱进行分析,各批样品相似度均在0.99以上。在建立的色谱条件下,5个成分分离度良好,方法精密度和重复性RSD均<2.0%,供试品溶液在24 h内稳定,各成分具有良好的线性关系和较宽线性范围;12批消栓肠溶胶囊中苦杏仁苷、芍药苷、阿魏酸、毛蕊异黄酮苷和藁本内酯质量分数分别为0.27～0.39、2.54～2.66、2.71～2.79、0.44～0.56和1.47～1.59 mg·g^(-1)。结论:所建立的消栓肠溶胶囊HPLC指纹图谱和定量测定分析方法快速、准确,灵敏度高,专属性强,可以有效地评价该制剂的质量。
Objective:To establish the HPLC fingerprint and determine the contents of amygdalin,paeoniflorin,ferulic acid,calycosin and ligustilide in Xiaoshuan enteric-coated caplsules,so as to provide the reference for quality control of Xiaoshuan enteric-coated capsules.Methods:The analysis was carried out on an analytical Diamonsil C18(2) column(4.6 mm×250 mm,5 μm)with gradient elution of acetonitrile(A)-0.1% phosphoric acid solution(B)(0-5 min,8%A;5-12 min,8%A → 15%A;12-20 min,15%A → 37%A;20-28 min,37%A;20-45 min,37%A → 50%A;45-65 min,50%A → 65%A).The detection wavelengths were 220 nm(0-30 min)and 310 nm(30-65 min)and the flow rate was 1.0 mL·min^-1.The column temperature was 35 ℃.Results:The common mode of the fingerprint was set up with 21 common peaks,and 5 of them were identified by comparison with the reference.They were amygdalin(peak 2),paeoniflorin(peak 10),ferulic acid(peak 14),calycosin(peak17) and ligustilide(peak 20).The similar degrees of 12 batches of samples were over 0.99.The 5 compounds were well separated under the determined chromatographic conditions.The RSDs of precision and repeatability experiments were all less than 2.0%.And the sample solution was stable during 24 h.All the compounds had good linearity and wide linear range.The content of amygdalin,paeoniflorin,ferulic acid,calycosin and ligustilide in 12 batches of Xiaoshuan enteric-coated caplsules were 0.27-0.39 mg·g^-1,2.54-2.66 mg·g^-1,2.71-2.79 mg·g^-1,0.44-0.56 mg·g^-1 and 1.47-1.59 mg·g^-1,respectively.Conclusion:The established method is fast,accurate,sensitive and specific,and can be used for the quality control of Xiaoshuan enteric-coated caplsules.
作者
阚艳红
KAN Yan-hong(The Pharmacology Department of Tangshan Gongren Hospital,Tangshan 063000,China)
出处
《药物分析杂志》
CAS
CSCD
北大核心
2019年第5期937-944,共8页
Chinese Journal of Pharmaceutical Analysis
