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].现代生物医学进展英文版,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 |
Received:August 28, 2018 Revised:September 24, 2018 |
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) |
Author Name | Affiliation | E-mail | YUAN Liang | School of Pharmacy Shanghai Jiao Tong University, Shanghai, 200240, China | yuanliang0105@163.com | GAO Qing-sha | School of Pharmacy Shanghai Jiao Tong University, Shanghai, 200240, China | | WANG Yan | School of Pharmacy Shanghai Jiao Tong University, Shanghai, 200240, China | | YAN Chao | School of Pharmacy Shanghai Jiao Tong University, Shanghai, 200240, China | |
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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. |
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