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| UHPLC-MS/MS法同时测定补骨脂药材中17种成分的含量 |
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夏宁1, 张孝莹1, 成丽媛2, 张玥1,2,3, 周昆1,2,3
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1.天津中医药大学药物安全评价中心, 天津 301617;2.天津中医药大学中医药研究院, 天津 301617;3.省部共建组分中药国家重点实验室, 天津 301617
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| 摘要: |
| [目的] 建立UHPLC-MS/MS法同时测定25批补骨脂中17种成分的含量。[方法] 采用超高效液相色谱-三重四级杆串联质谱技术检测，色谱柱为Thermofisher Scientific Hypersil GOLD（100 mm×2.1 mm 1.9 μm），流动相为水（A）-乙腈（B），梯度洗脱，进样量为3 μL，流速为0.2 mL/min，柱温40 ℃；离子源为电喷雾离子源（ESI）；在多反应检测（MRM）模式下正、负离子同时测定。[结果] 补骨脂素、异补骨脂素、补骨脂酚、4，5-去氢异补骨脂定、补骨脂查尔酮、异补骨脂色烯查尔酮、补骨脂二氢黄酮甲醚、补骨脂宁、补骨脂定、补骨脂甲素、补骨脂乙素、8-甲氧基补骨脂素、异补骨脂二氢黄酮、新补骨脂异黄酮、5-甲氧基补骨脂素、巴库查尔酮、Corylifol A 17 种成分线性关系良好（r>0.99），平均加样回收率（n=6）为95.66%~101.38%，RSD为0.77%~3.04%；精密度、重复性，稳定性试验的RSD均小于2.57%，符合分析要求。含量测定显示，不同批次补骨脂中各成分含量差别较大。[结论] 本实验建立的检测方法快速、准确、重复性好，可适用于补骨脂的质量控制研究。 |
| 关键词: 补骨脂 UHPLC-MS/MS 含量测定 |
| DOI：10.11656/j.issn.1673-9043.2024.11.03 |
| 分类号:R284.2 |
| 基金项目:国家自然科学基金项目(81673826);组分中药国家重点实验室资助课题项目(CBCM2023203)。 |
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| Simultaneous quantification of 17 components in psoraleae fructus by UHPLC-MS/MS method |
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XIA Ning1, ZHANG Xiaoying1, CHENG Liyuan2, ZHANG Yue1,2,3, ZHOU Kun1,2,3
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1.Center of Drug Safety Evaluation, Tianjin University of Traditional Chinese Medicine, Tianjin 301617, China;2.Institute of Traditional Chinese Medicine, Tianjin University of Traditional Chinese Medicine, Tianjin 301617, China;3.State Key Laboratory of Component-based Chinese Medicine, Tianjin 301617, China
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| Abstract: |
| [Objective] To establish a UHPLC-MS/MS method for the simultaneous determination of 17 components in 25 batches of psoraleae fructus. [Methods] The UHPLC-MS/MS method was performed on Thermofisher Scientific Hypersil GOLD（100×2.1mm 1.9μm）. The mobile phase was water（A）-acetonitrile（B）；Gradient elution；The injection volume was 3 μL. The flow rate was 0.2 mL/min and column temperature were 40 ℃. The ion source was ESI, the ion source temperature was 500 ℃. The positive and negative ions were measured simultaneously in multiple reaction detection（MRM） mode. [Results] psoralen, isopsoralen, bakuchiol, 4, 5-dehydroisopsoralidin, bavachalcone, isobavachromene, bavachinin, corylin, psoralidin, bavachin, isobavachalcone, 8-methoxypsoralen, isobavachin, neobavaisoflavone, 5-methoxypsoralen, bakuchalone, corylifol a 17 components with good linear relationship（r>0.99）, the average recoveries（n=6） were 95.66%~101.38%, RSD was 0.77%~3.04%. RSDS of precision, repeatability and stability tests were all less than 2.57%, which met the requirements of analysis. The content determination showed that the content of each component in different batches of psoralen was different. [Conclusion] The method established in this experiment is rapid, accurate and reproducible, and can be applied to the quality control of psoraleae fructus. |
| Key words: psoraleae fructus UHPLC-MS/MS content determination |
