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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 Δ

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閤雪晴 ，黄建猷 2， 3 # ，黄周锋 ，高美美 ，黄宏妙 ，陆国寿（1.广西中医药大学药学院，南宁 530200；2.广西壮
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1＊
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族自治区中医药研究院，南宁 530022；3.广西中药质量标准研究重点实验室，南宁 530022）
中图分类号 R917；R284.1 文献标志码 A 文章编号 1001-0408（2024）05-0560-06
DOI 10.6039/j.issn.1001-0408.2024.05.09

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
TM
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Echway Gowon C18
（250 mm×4.6 mm，5 μm）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269 nm，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、pleuropyrone A、大黄
素-8-O-β-D-葡萄糖苷。HPLC-QAMS法结果表明，pleuropyrone A、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
1.147 2、0.874 7、0.644 4。上述4种成分在各自检测范围内线性关系良好（r≥0.999 6），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、pleuropyrone A、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。
关键词 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

Extraction， isolation， identification and content determination of four chemical components in Yao
medicine Ventilago leiocarpa
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2， 3
XIA Xueqing ，HUANG Jianyou ，HUANG Zhoufeng ，GAO Meimei ，HUANG Hongmiao ，LU Guoshou 2
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（1. College of Pharmacy， Guangxi University of Chinese Medicine， Nanning 530200， China；2. Guangxi
Zhuang Autonomous Region Institute of Traditional Medical and Pharmaceutical Sciences， Nanning 530022，
China；3. Guangxi Key Laboratory of Traditional Chinese Medicine Quality Standards， Nanning 530022， China）
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 Gowon C18 （250 mm×
TM
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，
Δ 基金项目 广西自然科学基金面上项目（No.2020GXNSFAA259- respectively. The content of these four components was
076）；广西研究生联合培养基地资助项目（No.桂学位〔2021〕6号） measured as a good linearity （r≥0.999 6）； relative standard
＊第一作者 硕士研究生。研究方向：中药化学成分的研究与应
deviation （RSD） of precision， stability and reproducibility
用。E-mail：2991005743@qq.com
# 通信作者 副主任药师。研究方向：中药药效物质基础。 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

· 560 · China Pharmacy 2024 Vol. 35 No. 5 中国药房 2024年第35卷第5期