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当归补血丸指纹图谱及3种指标成分含量测定方法的建立
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| 篇名： | 当归补血丸指纹图谱及3种指标成分含量测定方法的建立 |
| TITLE： | Establishment of the fingerprints for Danggui buxue pills and the method for the content determination of three indicative constituents |
| 摘要： | 目的 建立当归补血丸的指纹图谱以及3种指标性成分（阿魏酸、毛蕊异黄酮葡萄糖苷、黄芪甲苷）的含量测定方法。方法以来自2个厂家的15批当归补血丸为样品，采用高效液相色谱（HPLC）法进行分析。色谱柱为HypersilODS2C18；柱温为25℃；流动相为乙腈-0.2％甲酸溶液（梯度洗脱）；流速为1.0mL/min；进样量为20μL；检测器为紫外检测器[检测波长分别为250nm（毛蕊异黄酮葡萄糖苷）、323nm（阿魏酸）]和蒸发光散射检测器（黄芪甲苷）。通过《中药色谱指纹图谱相似度评价系统（2012版）》建立15批当归补血丸的HPLC指纹图谱并进行相似度评价，通过与对照品图谱及对照药材图谱比对进行色谱峰的指认和归属，并测定其中阿魏酸、毛蕊异黄酮葡萄糖苷、黄芪甲苷的含量。结果15批样品指纹图谱中有33个共有峰，相似度均不低于0.893，并指认出13号峰为阿魏酸、15号峰为毛蕊异黄酮葡萄糖苷；通过与对照药材色谱图进行比对，发现1～3、7、8、10、12、13（阿魏酸）、17～19、27～29、32、33号峰归属于当归，14、15（毛蕊异黄酮葡萄糖苷）、20～23、25号峰归属于黄芪。含量测定方法学考察结果均符合相关要求，15批样品中阿魏酸、毛蕊异黄酮葡萄糖苷、黄芪甲苷的平均含量分别为0.0501、0.4026、0.9134mg/g。结论本研究建立了当归补血丸的HPLC指纹图谱及3种指标成分的HPLC定量分析方法，所建方法准确可靠、重复性好。 |
| ABSTRACT： | OBJECTIVE To establish the fingerprints of Danggui buxue pills a nd the method for the content determination of three indicative constituents （ferulic acid ，calycosin 7-O-β-D-glucoside and astragaloside Ⅳ）. METHODS Fifteen batches of Danggui buxue pills from two manufacturers were analyzed by high performance liquid chromatography （HPLC）. The determination was performed on a Hypersil ODS 2 C18 column with mobile phase consisted of acetonitrile- 0.2％ formic acid （gradient elution ）at the flow rate of 1.0 mL/min. The column temperature was set at 25 ℃，and the sample size was 20 μL. UV detector [detection wavelengths were 250 nm （calycosin 7-O-β-D-glucoside），323 nm （ferulic acid ）] and evaporative light scattering detector （astragaloside Ⅳ）were selected as detectors. HPLC fingerprints of 15 batches of Danggui buxue pills were established with Similarity Evaluation System of TCM Chromatographic Fingerprint （2012 edition）. The chromatographic peaks were identified and assigned by comparing with the chromatogram of the reference substance and reference medicinal material ；the contents of ferulic acid ，calycosin 7-O-β-D-glucoside and astragaloside Ⅳ were also determined. RESULTS There were 33 common peaks in the fingerprints of 15 batches of samples with the similarities not lower than 0.893. Ferulic acid and calycosin 7-O-β-D-glucoside were identified as peak 13 and 15，respectively. Compared with the chromatogram of reference medicinal material，it could be found that peaks 1-3，7，8，10，12，13（ferulic acid ），17-19，27-29，32 and 33 belonged to Angelica sinensis，and peak 14，15（calycosin 7-O-β-D-glucoside），20-23，25 belonged to Astragalus membranaceus . The methodology of content determination met the requirements. The mean contents of ferulic acid ，calycosin 7-O-β-D-glucoside and astragaloside Ⅳ in 15 batches of samples were 0.050 1，0.402 6，0.913 4 mg/g. CONCLUSIONS In this study ，HPLC fingerprints of Danggui buxue pills and the method of HPLC quantitative analysis for three indicative constituents are established. Established methods are accurate，reliable and repeatable. |
| 期刊： | 2022年第33卷第11期 |
| 作者： | 范佳儿，刘银榕，晁志，田恩伟 |
| AUTHORS： | FAN Jia ’er，LIU Yinrong ，CHAO Zhi，TIAN Enwei |
| 关键字： | 当归补血丸；指纹图谱；阿魏酸；毛蕊异黄酮葡萄糖苷；黄芪甲苷；含量测定；质量控制 |
| KEYWORDS： | Danggui buxue pills ； fingerprints； ferulic |
| 阅读数： | 214 次 |
| 本月下载数： | 6 次 |
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