柱前衍生化HPLC法测定注射用帕米膦酸二钠含量  

The Content Determination of Pamidronate Disodium Injection by Pre-column Derivatization HPLC

作　　者：张燕[1,2] 戴河双 胡培[2] 李开金[2] 李洁[2] 罗帅[2] 陈琴华[1,2] 

机构地区：[1]湖北医药学院附属东风医院实验中心,湖北十堰442008 [2]湖北医药学院药学院,湖北十堰442000 [3]重庆医科大学药学院,重庆400016

出　　处：《湖北医药学院学报》2014年第6期585-587,591,共4页Journal of Hubei University of Medicine

基　　金：湖北省2011协同创新中心基金项目(编号:4);湖北医药学院2013年校级大学生创新创业训练项目(2013XS04)

摘　　要：目的：建立9-氯甲酸芴甲酯（9-fluorenyl methyl chloroformate,FMOC-Cl）柱前衍生化高效液相色谱法（HPLC）测定注射用帕米膦酸二钠含量的方法。方法：碱性条件下供试品与FMOC衍生化反应,采用Linksil HPLC ODS C18色谱柱（4.6 mm×250 mm,5μm）,乙腈-0.4%EDTA（p H=7.2）（25∶75）为流动相,流速1 m L·min-1,检测波长为264 nm。结果：帕米膦酸二钠浓度在2-35μg·m L-1范围内与峰面积呈良好线性关系（r=0.9995）,检测限为0.5μg·m L-1,平均回收率101.2%（n=9）。结论：本法简单、准确、灵敏,适用于注射用帕米膦酸二钠的含量测定。Objective To develop a HPLC method with pre-eolumn derivatization for the determination of disodium pamidronate during its injection. Methods Disodium pamidronate was derivatized with 9-fluorenyl methyl chloroformate. The HPLC column was Hypersil ODS C18 column （4.6 mm × 250 mm, 5 μm）. The mobile phase consisted of acetonitrile and 0.4% EDTA with pH 7.2 （25： 75） at the flow rate of 1 mL · min^-1 ,and the detective wavelength was 265 nm. Results The linear range was from 2 to 35 μg · mL ^- 1 with good eood cient values （ r = 0. 9995 ）, detective limitation was 0.5 μg · mL ^- 1 and the average recovery was 101.2% （n = 9 ）. Conclusion The method is simple, accurate, specific and can be used for determination of disedium pamidronate during its injection.

关 键 词：帕米膦酸二钠 9-氯甲酸芴甲酯 柱前衍生化 高效液相色谱法 

分 类 号：R965[医药卫生—药理学] O657.72[医药卫生—药学]