引用本文: | 其其格,包晓玲,李淑艳,乌日吉木斯,韩阿斯如,吴东兴.基于UPLC-Q/TOF-MS技术的蒙药黑云香成分分析及HPLC含量测定研究[J].中国现代应用药学,2025,42(6):95-101. |
| QI Qige,BAO Xiaoling,LI Shuyan,WU Rijimusi,HAN Asiru,WU Dongxing.Study on composition analysis and HPLC content determination of Mongolian medicine Commiphora mukul(Hook. ex Stocks)Engl based on UPLC-Q/TOF-MS technique[J].Chin J Mod Appl Pharm(中国现代应用药学),2025,42(6):95-101. |
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摘要: |
目的 基于UPLC-Q/TOF-MS技术分析蒙药黑云香成分,并基于HPLC技术建立同时测定黑云香中2种成分含量的方法。方法 UPLC-Q/TOF-MS法采用Waters acquity UPLC BEH C18色谱柱(2.1x100mm,1.7μm),柱温35℃,流动相为甲醇(A)-0.1%甲酸水(B),梯度洗脱;体积流量0.3ml/min;电喷雾离子源,正离子模式下采集质谱数据,质量扫描范围m/z100~1000。使用UNIFI Portal 软件进行成分分析。HPLC使用Waters SymmetryR C18色谱柱(4.6×250㎜,5μm);流动相为甲醇(A)-0.1%磷酸水(B),梯度洗脱;体积流量1.0ml/min;检测波长252nm。柱温25℃,同时测定黑云香中2-甲氧基-5-乙酰基-呋喃吉玛(10)-烯-6-酮(FSA)和脱氢松香酸2种成分的含量。结果 基于UPLC-Q/TOF-MS技术在正离子模式下检测出42个化合物;通过化合物的保留时间、母离子、碎片离子等相关信息,并查阅没药属药材的分离等相关文献,初步推测出化合物名称。采用HPLC进行2种成分的含量测定,分别在0.124~0.744、0.04~0.24μg范围内线性关系良好(r >0.9991),平均加样回收率分别为99.01%、99.46%,RSD分别为0.62%、0.66%。结论 基于UPLC-Q/TOF-MS技术可以快速、准确分析黑云香化学成分;建立的HPLC测定黑云香中2种成分的含量方法简便可靠,重复性好,可为黑云香质量控制提供参考。 |
关键词: 黑云香 UPLC-Q/TOF-MS HPLC 成分分析 含量测定 |
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基金项目:内蒙古自治区科技计划项目(2021GG0428);内蒙古自治区高等学校“青年科技英才支持计划”项目(NJYT22049);蒙医药研发工程教育部重点实验室开放课题项目(MDK2023065);内蒙古民族大学中药学(蒙药学)重点学科建设项目(ZYX010) |
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Study on composition analysis and HPLC content determination of Mongolian medicine Commiphora mukul(Hook. ex Stocks)Engl based on UPLC-Q/TOF-MS technique |
QI Qige, BAO Xiaoling, LI Shuyan, WU Rijimusi, HAN Asiru, WU Dongxing
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College of Mongolian Medicine and Pharmacy,Inner Mongolia University for Nationalities
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Abstract: |
AIM Based on the UPLC-Q/TOF-MS technique, the components of Commiphora mukul(Hook. ex Stocks)Engl were analyzed, a method for the simultaneous determination of the two components were established based on HPLC technology. METHODS The UPLC-Q/TOF-MS method was performed on Waters acquity UPLC BEH C18 column (2.1x100mm, 1.7μm),column temperature was 35℃, the mobile phase was methanol (A) -0.1% formic acid water (B). Volume flow rate was 0.3ml/min. mass scanning range m/z100~1000.The UNIFI Portal software was used for component analysis. Waters SymmetryR C18 column (4.6×250㎜,5μm) was used for HPLC. The mobile phase was methanol (A) -0.1% phosphoric acid water (B). Volume flow rate was 1.0ml/min. The detection wavelength was 252nm. Column temperature was 25℃, at the same time, the contents of 2- methoxy- 5 - acetoxy - furanogermacr- 1(10) -en -6 -one and dehydroabietic acid were determined. RESULTS Based on the UPLC-Q/TOF-MS technique, 42 compounds were detected in positive ion modes. The name of the compound was preliminarily inferred by the retention time, parent ion, fragment ion and other relevant information of the compound, as well as the separation of myrrh and other related literature. HPLC was used to determine the contents of the two components, and the linear relationships were good (r >0.9991) in the range of 0.124-0.744 and 0.04-0.24μg, respectively. The average recoveries were 99.01% and 99.46%, and RSD were 0.62% and 0.66%, respectively. CONCLUSION Based on the UPLC-Q/TOF-MS technique , the chemical components of the Commiphora mukul(Hook. ex Stocks)Engl can be analyzed quickly and accurately. The established HPLC method for the determination of the two components in Commiphora mukul(Hook. ex Stocks)Engl was simple, reliable and reproducible, which can provide reference for the quality control of Commiphora mukul(Hook. ex Stocks)Engl. |
Key words: Commiphora mukul(Hook. ex Stocks)Engl UPLC-Q/TOF-MS HPLC Component analysis Content determination |