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HPLC指纹图谱结合一测多评法控制马齿苋药材质量
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| 篇名： | HPLC指纹图谱结合一测多评法控制马齿苋药材质量 |
| TITLE： | Quality control of Portulaca oleracea by HPLC fingerprint combined with quantitative analysis of multi-components by single-marker |
| 摘要： | 目的 建立马齿苋药材的高效液相色谱（HPLC）指纹图谱，同时建立一测多评法测定该药材中咖啡酸、阿魏酸、染料木苷、槲皮素的含量，为该药材的质量控制提供参考依据。方法色谱柱为EclipseXDB-C18，流动相为甲醇-0.2%磷酸溶液（梯度洗脱），柱温为25℃，流速为1.0mL/min，检测波长为360nm，进样量为10μL，以上述色谱条件建立马齿苋药材的HPLC指纹图谱；对15批药材样品进行聚类分析和主成分分析；以咖啡酸作为内标物，使用一测多评法计算其他3种成分的相对校正因子，再根据相对校正因子计算成分含量，并与外标法结果进行比较。结果15批马齿苋药材样品的HPLC指纹图谱中有17个共有峰被标定，4种成分（咖啡酸、阿魏酸、染料木苷、槲皮素）被指认；15批样品的相似度均大于0.890。聚类分析结果显示，样品S1～S10聚为一类，S11～S15聚为一类；主成分分析结果显示，前2个主成分的累计贡献率为92.502%，分类结果与聚类分析结果一致。咖啡酸、阿魏酸、染料木苷和槲皮素检测质量浓度的线性范围分别为0.0031～0.1571、0.0036～0.1817、0.0085～0.4256、0.0004～0.0218mg/mL（R2≥0.9997）；精密度、重复性、稳定性（24h）、加样回收率试验结果均符合《中国药典》要求。一测多评法计算得到阿魏酸、染料木苷、槲皮素的平均相对校正因子分别为1.534、5.302、0.174，该方法与外标法所测的成分含量无显著差异。结论所建立的HPLC指纹图谱结合一测多评的方法，可用于马齿苋药材中多指标成分的质量控制。产地对马齿苋药材质量有一定影响，四川所产马齿苋药材质量略优于安徽和河北所产药材。 |
| ABSTRACT： | OBJECTIVE To establish HPLC fingerprint of Portulaca oleracea， establish quantitative analysis of multi- components by single-marker （QAMS） method for the content determination of caffeic acid， ferulic acid， genistin and quercetin， and provide reference for quality control of the medicine. METHODS The determination was performed on Eclipse XDB-C18 column with mobile phase consisted of methanol-0.2% phosphoric acid solution （gradient elution） at the flow rate of 1.0 mL/min. The column temperature was 25 °C， and detection wavelength was set at 360 nm. The sample size was 10 μL. HPLC fingerprint of P. oleracea was established according to the above chromatographic conditions. Cluster analysis （CA） and principal component analysis （PCA） were performed for 15 batches of specimens. Using caffeic acid as internal standard， relative correction factors of other three components were calculated by QAMS， and then the component content was calculated on the basis of relative correction factors， which was compared with the external standard method. RESULTS HPLC fingerprints of 15 batches of P. oleracea were calibrated with a total of 17 common peaks， and 4 components （caffeic acid， ferulic acid， genistin， quercetin） were identified； the similarities of 15 batches of samples were greater than 0.890. The results of CA showed that S1-S10 were clustered into one category， and S11-S15 were clustered into one category. The results of PCA revealed that the accumulative contribution rate of the two main components was 92.502%， and the classification results were basically consistent with CA. The linear range of caffeic acid， ferulic acid， genistin and quercetin were 0.003 1-0.157 1， 0.003 6-0.181 7， 0.008 5-0.425 6，0.000 4-0.021 8 mg/mL （R2≥0.999 7）； the results of precision， repeatability， stability （24 h） and recovery tests all complied with the requirements of Chinese Pharmacopoeia. The relative correction factors of ferulic acid， genistin and quercetin calculated by QAMS were 1.534， 5.302 and 0.174； there was no significant difference in the contents of components measured between this method and the external standard method. CONCLUSIONS The established HPLC fingerprint combined with QAMS can be used for the quality control of multiple index components in P. oleracea. The origin has a certain influence on the quality of P. oleracea， and the quality of P. oleracea produced in Sichuan is better than that produced in Anhui and Hebei. |
| 期刊： | 2023年第34卷第09期 |
| 作者： | 王佳佳；李希；冯建安；楼冠华；陈诗韵；黄嫣；皮雪莲；刘畅；李颖 |
| AUTHORS： | WANG Jiajia，LI Xi，FENG Jian’an，LOU Guanhua，CHEN Shiyun，HUANG Yan，PI Xuelian，LIU Chang，LI Ying |
| 关键字： | 马齿苋；质量控制；高效液相色谱法；指纹图谱；一测多评法；咖啡酸；阿魏酸；染料木苷；槲皮素 |
| KEYWORDS： | Portulaca oleracea； quality control； high-performance liquid chromatography； fingerprint； quantitative analysis of |
| 阅读数： | 191 次 |
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