首页|女贞子-墨旱莲药对提取物的指纹图谱和化学成分鉴定研究

女贞子-墨旱莲药对提取物的指纹图谱和化学成分鉴定研究

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目的 建立女贞子-墨旱莲药对提取物的HPLC指纹图谱以控制其质量,并对提取物中所含有的化学成分进行结构鉴定.方法 采用HPLC法,固定相为 ZORBAX Extend C18色谱柱(4.6 mm×250 mm,5 μm),流动相为乙腈-体积分数为0.1%甲酸溶液梯度洗脱,流速为 1.0 mL·min-1,检测波长为265 nm,柱温为35℃,进样量为10 μL;建立 15 批不同产地女贞子-墨旱莲药对提取物的 HPLC 指纹图谱,对其进行相似度评价、聚类分析和正交偏最小二乘方判别分析;采用超高效液相色谱-静电场轨道阱高分辨质谱(UPLC-Q-Exactive Orbitrap MS)联用技术,分别在正、负离子扫描模式下对提取中的化学成分进行检测,基于高分辨质谱一级和二级数据进行结构鉴定.结果 由不同产地药材随机组合的 15 批女贞子-墨旱莲药对提取物的相似度介于 0.865~0.992 之间,药对指纹图谱中共确定了 16 个共有峰,指认了其中 7 个色谱峰;液质联用共检测到 55 个化合物,采用对照品准确鉴定了 7 个成分的化学结构,并推测了其它 48 个化合物的可能化学结构.结论 建立的指纹图谱方法简便可靠,重复性好,可用于女贞子-墨旱莲药对提取物的质量控制研究;UPLC-Q-Exactive Orbitrap MS联用技术可实现对女贞子-墨旱莲药对提取物中化合物的结构鉴定,为其后续研究奠定了基础.
Fingerprint and Identification of Chemical Constituents of the Extract of Fructus Ligustri Lucidi-Ecliptae Herba
OBJECTIVE To establish high performance liquid chromatography(HPLC)fingerprints of the extract of Fructus Li-gustri Lucidi-Ecliptae Herba and to identify the structure of its chemical constituents.METHODS The chromatographic separation was performed on ZORBAX Extend C18(250 mm×4.6 mm,5 μm)column with the mobile phase consisting of acetonitrile and 0.1%formic acid solution in gradient elution mode at a flow rate of 1.0 mL·min-1.The optimum column temperature was set at 35℃,the detection wavelength was 265 nm,and the injection volume was 10 μL.The HPLC fingerprints of 15 batches of herb pair from different origins were established.Then,similarity evaluation,cluster analysis,and orthogonal partial least squares discriminant analysis were carried out.The chemical structures of the constituents of the herb pair were identified based on the high-resolution mass spectrometry utilizing the UPLC-Q-Exactive Orbitrap MS in positive and negative-ion modes.RESULTS As a result,the similarity of the 15 bat-ches of samples varied from 0.865 to 0.992.A total of 16 common peaks were identified in the fingerprints,and 7 of them were identi-fied by comparision with the reference substances.Furthermore,55 chemical compounds were detected,and 7 of them were accurately identified based on the reference substances,and the chemical structures of the rest 48 components were temporarily speculated.CON-CLUSION The fingerprint method established in this study is simple,reliable,and reproducible,and can be further used for the quality control of Fructus Ligustri Lucidi-Ecliptae Herba herb pair.The developed UPLC-Q-Exactive Orbitrap MS method can be applied to identify the structures of chemical constituents in this herb pair and lay a foundation for further research.

Fructus Ligustri LucidiEcliptae HerbafingerprintUPLCQ-Exactive Orbitrap MSchemical constituents

高雨桐、宋秀苹、李楠、尚涌琳、韩飞

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沈阳药科大学药学院,辽宁 沈阳 110016

墨旱莲 女贞子 指纹图谱 超高效液相 静电场轨道阱高分辨质谱 化学成分

辽宁省科技厅面上项目辽宁省教育厅项目

2021-MS-220JYTMS20231378

2024

南京中医药大学学报
南京中医药大学

南京中医药大学学报

CSTPCD北大核心
影响因子:1.658
ISSN:1672-0482
年,卷(期):2024.40(4)
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