| 袁 亮,高青山,王 彦,阎 超.利用超高效液相色谱和离子色谱法测定注射用磷酸川芎嗪的含量[J].,2019,19(8):1410-1415 |
| 利用超高效液相色谱和离子色谱法测定注射用磷酸川芎嗪的含量 |
| Determination of Ligustrazine Phosphate for Injection by Ultra Performance Liquid Chromatography and Ion Chromatography |
| 投稿时间：2018-08-28 修订日期：2018-09-24 |
| DOI：10.13241/j.cnki.pmb.2019.08.003 |
| 中文关键词: 超高效液相色谱 离子色谱 磷酸川芎嗪 川芎嗪 磷酸 含量测定 |
| 英文关键词: Ultra high performance liquid chromatography (UPLC) Ion chromatography (IC) Ligustrazine phosphate Ligustrazine Phosphoric acid Content determination |
| 基金项目:上海市科委科研计划项目(16142200300) |
|
| 摘要点击次数: 701 |
| 全文下载次数: 701 |
| 中文摘要: |
| 摘要 目的：建立超高效液相色谱法（UPLC）和离子色谱法（IC）测定磷酸川芎嗪中川芎嗪和磷酸的含量，为质量评价提供依据。方法：UPLC测定川芎嗪的色谱柱为Waters Acquity BEH C18 (2.1 mm × 50 mm，1.7 μm)；检测波长：300 nm检测川芎嗪，274 nm检测有关物质邻苯二甲酸二甲酯；流动相为0.1%甲酸水溶液（A）-0.1%甲酸乙腈( B )，梯度洗脱（0.0~0.8 min，10% B→90% B；0.8~0.81 min，90% B→10% B；0.81~1.00 min，10% B），流速：0.7 mL/min。IC测定磷酸的离子交换色谱柱为Dionex IonPac AS11-HC-4 ?滋m (4 × 250 mm)，流动相为30 mmol/L KOH溶液等度洗脱15 min，流速1.0 mL/min，柱温35℃；电导检测器；抑制器电流为50 mA。结果：川芎嗪和磷酸在10~100 g/mL内具有良好的线性关系，相关系数均为1.0，UPLC法测定川芎嗪的回收率为102.0 %。IC测定磷酸的回收率为99.8%。7个公司生产的注射剂中川芎嗪的含量均在药典规定的范围90%~110%内。但是其中3个公司生产的注射剂磷酸超出药典规定范围90%~110%。结论：与常规HPLC/UPLC测定磷酸川芎嗪含量方法比较，本文所用方法测定结果更加准确、全面、且重复性好，能够真实反应注射用磷酸川芎嗪的实际含量，对于注射用磷酸川芎嗪的安全性和有效性评估提供了一定的依据。 |
| 英文摘要: |
| ABSTRACT Objective: To establish a method based on ultra-high performance liquid chromatography (UPLC) and an ion chromatography (IC) for analysis of ligustrazine and phosphoric acid, providing the basis for their qualitative evaluation. Methods: Ligustrazine was separated on Waters Acquity BEH C18 (2.1 mm × 50 mm, 1.7 μm). The detection wavelengths were 300 nm for ligustrazine and 274 nm for dimethyl phthalate. Mobile phase A was 0.1% formic acid in water and B was 0.1% formic acid in acetonitrile with gradient elution（0.0~0.8 min，10% B→90% B; 0.8~0.81 min, 90% B→10% B; 0.81~1.0 min, 10% B). The flow rate was 0.7 mL/min. Phosphate anion was separated on Dionex IonPac AS11-HC-4 μm column (4 mm × 250 mm). Equivalent diluted with 30 mmol/L KOH for 15 minutes. The flow was 1.0 mL/min. Column temperature was 35 ℃. The conductivity detector suppressor current was 50 mA. Results: Ligustrazine and phosphoric acid had good linearity in the range of 10~100 g/mL and both of the correlation coefficients were 1.0. The recoveries of UPLC method for ligustrazine was 102.0%．The recoveries of IC method for phosphoric acid was 99.8%．The obtained results of the 7 companies' injections of ligustrazine phosphate are all in pharmacopeia range of 90%~110%. But the phosphoric acid contents in 3 companies are out of the range. Conclusion: Compared with the commonly used content of ligustrazine phosphate by HPLC/UPLC, the results of this method are more accurate, comprehensive and reproducible, which can truly reflect the actual content of ligustrazine phosphate in the injection. It provides a better basis for the safety and effectiveness of ligustrazine phosphate for Injection. |
|
查看全文
查看/发表评论 下载PDF阅读器 |
| 关闭 |
