| 朱靖,赵振霞,苏建,刘永利.三七伤药片中6种乌头类生物碱含量测定及化学计量学分析[J].中国药事,2023,(10):1149-1159 |
| 三七伤药片中6种乌头类生物碱含量测定及化学计量学分析 |
| Determination and Chemometric Analysis of Six Aconitum Alkaloids in Sanqi Shangyao Tablets |
| 投稿时间：2023-05-10 |
| DOI：10.16153/j.1002-7777.2023.10.007 |
| 中文关键词: 高效液相色谱 三七伤药片 乌头碱 次乌头碱 新乌头碱 苯甲酰乌头原碱 苯甲酰次乌头原碱 苯甲酰新乌头原碱 化学计量学 主成分分析 |
| 英文关键词: HPLC Sanqi Shangyao Tablet aconitine hypaconitine mesaconitine benzoylaconine benzoylhypaconine benzoylmesaconine chemometrics principal component analysis |
| 基金项目:国家药典委员会2018年度药品标准提高工作（中药）（编号 2018Z019）；河北省“三三三人才工程”人才培养资助项目（编号A202005016） |
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| 中文摘要: |
| 目的：采用高效液相色谱法，建立三七伤药片中乌头碱、次乌头碱、新乌头碱与苯甲酰乌头原碱、苯甲酰次乌头原碱、苯甲酰新乌头原碱6种生物碱类成分的含量测定方法，并根据测定结果进行化学计量学分析。方法：采用混合型阳离子交换反相吸附树脂（MCX）固相萃取小柱对供试品进行纯化， 高效液相色谱法测定，使用COSMOSIL C18色谱柱（4.6 mm×250 mm，5 μm），以甲醇-乙腈-0.1% 磷酸为流动相，梯度洗脱，流速为1.0 mL·min-1，柱温为25 ℃，检测波长为232 nm。采用SIMCA软件对结果进行处理，运用主成分分析法分析影响产品差异的关键因素。结果：乌头碱、次乌头碱、新乌头碱与苯甲酰乌头原碱、苯甲酰次乌头原碱、苯甲酰新乌头原碱分别在各自范围内线性关系良好 （r=0.9999），平均加样回收率（RSD）分别为101.8%（1.6%）、100.6%（1.4%）、97.8%（1.1%）、 100.8%（1.5%）、101.0%（1.6%）、100.7%（0.8%）。17批次样品测定结果显示不同批次之间6种生物碱含量存在较大差异；单酯型生物碱的含量是影响产品之间差异的关键因素。结论：所建立的方法准确可靠、灵敏度高，可用于三七伤药片中生物碱类成分的含量测定，为三七伤药片质量控制方法的建立提供依据。 |
| 英文摘要: |
| Objective: To establish a HPLC method for the determination of six alkaloids including aconitine, hypaconitine, mesaconitine and benzoylaconine, benzoylhypaconine, benzoylmesaconine in Sanqi Shangyao Tablets, and carry out chemometric analysis according to the research results. Methods: The sample was purifi ed by solid-phase extraction using a mixed cationic exchange adsorption resin(MCX) column and determined by HPLC. The analysis was performed on COSMOSIL C18 column (4.6 mm×250 mm, 5 μm), with methanolacetonitrile-0.1% phosphoric acid solution as the mobile phase with gradient elution and the fl ow rate was 1.0 mL·min-1. The column temperature was 25 ℃ and the detection wavelength was 232 nm. SIMCA software was used to process the results, and principal component analysis (PCA) was used to study the key factors aff ecting product difference. Results: Aconitine, hypaconitine, mesaconitine and benzoylaconine, benzoylhypaconine, benzoylmesaconine showed good linear relationships (r=0.9999), with average recoveries (RSD) of 101.8% (1.6%) , 100.6% (1.4%), 97.8% (1.1%), 100.8% (1.5%), 101.0% (1.6%), 100.7% (0.8%), respectively. The determination results of 17 batches of samples showed significant differences in the content of six alkaloids among different batches. The content of monoester alkaloids is the key factor affecting product difference. Conclusion: The established method is accurate and reliable with a high sensitivity, which can be used for content determination of alkaloid constituents in Sanqi Shangyao Tablets and can provide a basis for the establishment of quality control method for Sanqi Shangyao Tablets. |
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