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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 NameAffiliationE-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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