柱前衍生化/毛细管电泳法测定阿伦膦酸钠  

Determination of Alendronate by Capillary Electrophoresis with Pre-column Derivatization

作　　者：周世美[1] 张瑶瑶[2] 温群英[2] 王赪胤[2] 

机构地区：[1]扬州职业大学资源与环境工程学院,江苏扬州225009 [2]扬州大学化学化工学院,江苏扬州225002

出　　处：《分析测试学报》2013年第11期1364-1368,共5页Journal of Instrumental Analysis

基　　金：国家自然科学基金资助项目(20975091;21375116)

摘　　要：建立了一种以对甲氧基苯磺酰氯为紫外衍生试剂柱前衍生，毛细管电泳法测定阿伦膦酸钠的分析方法。阿伦膦酸钠与对甲氧基苯磺酰氯的衍生条件为：在20 mmol/L的硼酸盐缓冲溶液（pH 11.5）中，摩尔比为1∶10的阿伦膦酸钠与对甲氧基苯磺酰氯在50 ℃下反应10 min。将衍生产物在毛细管电泳上进行分离，使用pH 9.3 20 mmol/L的硼酸盐缓冲溶液为分离缓冲体系，柱温25 ℃，分离电压20 kV，在 0.5 psi压力下进样5 s，以二级管阵列（DAD）检测器在233 nm处进行检测。测得阿伦膦酸钠的线性范围为1.0-400 μg/mL，检出限为0.5-1.0 μg/mL。方法用于药物制剂阿伦膦酸钠片和尿液介质中阿伦膦酸钠的测定，结果满意。A capillary electrophoresis（CE） method for the determination of alendronate was developed by using 4-methoxybenzenesulfonyl chlorine（MOBS-Cl） as a pre-column derivatization reagent.The derivative reaction conditions were investigated,and the optimal derivative conditions were as follows：the alendronate reacted with MOBS-Cl in 20 mmol/L borate buffer solution（pH 11.5）,and the molar ratio of alendronate to MOBS-Cl was 1∶10.The temperature for the derivatization reaction was 50 ℃ and the reaction time was 10 min.The separation of the derivatives was achieved on capillary column by using 20 mmol/L borate buffer solution（pH 9.3） at a temperature of 25 ℃ and a separation voltage of 20 kV.The injection was carried out under the pressure of 0.5 psi for 5 s,and the detecting wavelength of diode array（DAD） was 233 nm.The calibration curves were linear in the range of 1.0-400 μg/mL,and the limits of detection were 0.5-1.0 μg/mL.This proposed method was applied in the determination of alendronate in pharmaceutical preparations and urine samples with satisfactory results.

关 键 词：毛细管电泳 对甲氧基苯磺酰氯 阿伦膦酸钠 柱前衍生 

分 类 号：O657.8[理学—分析化学] TQ460.72[理学—化学]