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瑶药紫九牛中4种化学成分的提取分离、鉴定及含量测定
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| 篇名： | 瑶药紫九牛中4种化学成分的提取分离、鉴定及含量测定 |
| TITLE： | Extraction，isolation，identification and content determination of four chemical components in Yao medicine Ventilago leiocarpa |
| 摘要： | 目的 提取分离瑶药紫九牛中的4种化学成分并对其进行鉴定和含量测定。方法采用溶剂提取、萃取和硅胶柱色谱分离法、制备液相色谱技术对紫九牛中的化学成分进行分离、纯化，根据化合物的波谱数据对分离得到的4种化学成分进行结构鉴定。采用高效液相色谱（HPLC）-一测多评（QAMS）法同时测定紫九牛中4种化学成分的含量，色谱条件为：以EchwayGowonTMC18（250mm×4.6mm，5μm）为色谱柱，以乙腈-0.1%磷酸溶液为流动相进行梯度洗脱，检测波长为269nm，柱温为25℃；以大黄素为内参物，建立该成分与其他3种成分的相对校正因子，利用相对校正因子计算含量；同时采用外标法计算各成分的含量，并比较2种方法所得结果的差异。结果从紫九牛中分离得到的4种化学成分经鉴定分别为大黄素、欧鼠李苷A、pleuropyroneA、大黄素-8-O-β-D-葡萄糖苷。HPLC-QAMS法结果表明，pleuropyroneA、大黄素-8-O-β-D-葡萄糖苷、欧鼠李苷A的相对校正因子分别为1.1472、0.8747、0.6444。上述4种成分在各自检测范围内线性关系良好（r≥0.9996），精密度、稳定性、重复性试验的RSD均小于2.00%，平均加样回收率为99.41%～100.46%（RSD≤2.05%）。QAMS法与外标法得到的10批紫九牛样品含量测定结果无明显差异（RSD＜3.00%）。结论从紫九牛中分离得到了大黄素、欧鼠李苷A、pleuropyroneA、大黄素-8-O-β-D-葡萄糖苷，其中后3种成分均为首次从该药材中分离得到。所建立的同时测定紫九牛中4种化学成分的HPLC-QAMS法准确、可靠，可用于该药材的质量控制。 |
| ABSTRACT： | OBJECTIVE To extract and isolate the four chemical components of Yao medicine Ventilago leiocarpa， and to conduct identification and content determination for them. METHODS The chemical components of V. leiocarpa were separated and purified by solvent extraction， extraction， silica gel column chromatography and preparative liquid chromatography； then the chemical structures of four isolated compounds were identified based on their spectral data. The contents of four components were determined by high performance liquid chromatography（HPLC）-quantitative analysis of multi-components by single-marker （QAMS） method， with the following chromatographic conditions： chromatographic column was Echway GowonTM C18 （250 mm× 4.6 mm， 5 μm）. The mobile phase was acetonitrile-0.1% phosphoric acid for gradient elution； the detection wavelength was 269 nm， and the column temperature was 25 ℃ . Using emodin as internal reference， the relative correction factors （fi/s） between emodin and the other 3 components were established and used to calculate the content. At the same time， the content of each component was calculated with the external standard method （ESM）， and the differences between these two methods were compared. RESULTS Four compounds were isolated from V. leiocarpa， and they were identified as emodin， frangulin A， pleuropyrone A， emodin-8-O-β-D-glucoside. The result of HPLC-QAMS showed that the fi/s of pleuropyrone A， emodin-8-O-β-D- glucoside and frangulin A were 1.147 2， 0.874 7 and 0.644 4， respectively. The content of these four components was measured as a good linearity （r≥0.999 6）； relative standard deviation （RSD） of precision， stability and reproducibility tests were all lower than 2.00%， and average recoveries were E-mail：dearhuangjianyou@126.com 99.41%-100.46%（RSD≤2.05%）. There was no significant difference between QAMS method and ESM （RSD＜3.00%）. CONCLUSIONS Emodin， frangulin A， pleuropyrone A and emodin- 8-O-β-D-glucoside are isolated from V. leiocarpa； among them， the last three components are all isolated from for the first time. The established HPLC-QAMS method is accurate and reliable for the determination of 4 components in V. leiocarpa， and can used for quality control of V. leiocarpa. |
| 期刊： | 2024年第35卷第05期 |
| 作者： | 閤雪晴；黄建猷；黄周锋；高美美；黄宏妙；陆国寿 |
| AUTHORS： | XIA Xueqing，HUANG Jianyou，HUANG Zhoufeng，GAO Meimei，HUANG Hongmiao，LU Guoshou |
| 关键字： | 紫九牛；化学成分；一测多评法；大黄素-8-O-β-D-葡萄糖苷；欧鼠李苷A；pleuropyrone A；大黄素；质量控制 |
| KEYWORDS： | Ventilago leiocarpa； chemical component； quantitative analysis of multi-components by single-marker； emodin-8- |
| 阅读数： | 71 次 |
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