| 高青山,袁 亮,王 彦,阎 超.超高效液相色谱法测定麻黄中l-麻黄碱和d-伪麻黄碱的含量[J].,2020,(5):832-837 |
| 超高效液相色谱法测定麻黄中l-麻黄碱和d-伪麻黄碱的含量 |
| Determination of l-Ephedrine and d-Pseudoephedrine by Ultra Performance Liquid Chromatography |
| 投稿时间：2019-07-28 修订日期：2019-08-23 |
| DOI：10.13241/j.cnki.pmb.2020.05.007 |
| 中文关键词: 超高效液相色谱 l-麻黄碱 d-伪麻黄碱 非对映异构体 含量测定 |
| 英文关键词: Ultra high performance liquid chromatography (UPLC) l-Ephedrine d-Pseudoephedrine Diastereomer Content determination |
| 基金项目:国家自然科学基金项目（21874088） |
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| 中文摘要: |
| 摘要 目的：建立超高效液相色谱法（UPLC）测定麻黄中l-麻黄碱和d-伪麻黄碱含量的方法，为麻黄药材质量评价提供依据。方法：UPLC测定麻黄碱色谱柱为Waters Acquity BEH-C18 (2.1 mm × 50 mm, 1.7 μm)；检测波长：214 nm；流动相为0.15%氨水水溶液（A）和乙腈( B )，梯度洗脱（0.0~4.0 min，5% B→55% B；4.0~ 4.1 min，55% B→95% B；4.1~4.7 min，95% B；4.7~4.8 min，95% B→5% B；4.8~5.0 min，5% B），流速：0.7 mL/min；柱温：25 ℃。结果：l-麻黄碱和d-伪麻黄碱分别在12.50~500.00 μg/mL和10.50~420.00 μg/mL范围内具有良好的线性关系，相关系数均为0.9999，UPLC方法测定l-麻黄碱和d-伪麻黄碱的回收率分别为101.99 %和98.68%。应用UPLC方法测定麻黄药材中的l-麻黄碱和d-伪麻黄碱的含量，麻黄药材两者含量分别为0.80%和0.18 %。结论：与常规HPLC测定l-麻黄碱和d-伪麻黄碱含量方法比较，本文所用方法测定结果更加准确、全面、且重复性好，能够快速测定麻黄药材中的l-麻黄碱和d-伪麻黄碱的实际含量；并且对麻黄碱及相关物质的测定有一定的指导意义。 |
| 英文摘要: |
| ABSTRACT Objective: To establish a method based on ultra-high performance liquid chromatography (UPLC) for analysis of l-Ephedrine and d-Pseudoephedrine, providing the basis for their qualitative evaluation of Ephedra sinica. Methods: l-Ephedrine and d-Pseudoephedrine were separated on Waters Acquity BEH-C18 (2.1 mm × 50 mm, 1.7 μm). The detection wavelength was 214 nm. Mobile phase A was 0.15% ammonium in water and B was acetonitrile with gradient elution（0.0~4.0 min, 5% B→55% B; 4.0~4.1 min, 55% B→95% B; 4.1~4.7 min, 95% B; 4.7~4.8 min, 95% B→5% B; 4.8~5.0 min, 5% B). The flow rate was 0.7 mL/min. Column temperature was 25 ℃. Results: The developed method had good linearity in the range of 12.50~500.00 μg/mL for l-Ephedrine and 10.50~420.00 μg/mL for d-Pseudoephedrine respectively, and both of the correlation coefficients were 0.9999. The recoveries of UPLC method for l-Ephedrine and d-Pseudoephedrine were 101.99% and 98.68%, respectively. The content determination of l-Ephedrine and d-Pseudoephedrine from E. sinica was used by the UPLC method, the obtained results of l-Ephedrine and d-Pseudoephedrine were 0.80% and 0.18%, respectively. Conclusion: Compared with the commonly used content determination of l-Ephedrine and d-Pseudoephedrine by HPLC, the established method has been proven to be accurate, comprehensive and reproducible, and can be applied for rapid determination of l-Ephedrine and d-Pseudoephedrine for E. sinica. Furthermore, it might shed light on the determination of ephedrine and related substance. |
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