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采用间接紫外检测的毛细管区带电泳快速分析烷基膦酸酯类药物。

Rapid analysis of alkylphosphonate drugs by capillary zone electrophoresis using indirect ultraviolet detection.

机构信息

Department of Pharmaceutical Chemistry, Faculty of Pharmacy, Mahidol University, Bangkok, Thailand.

出版信息

J Sep Sci. 2010 Feb;33(2):228-34. doi: 10.1002/jssc.200900518.

DOI:10.1002/jssc.200900518
PMID:20087866
Abstract

A rapid capillary electrophoretic method for the analysis of three alkylphosphonate drugs (i.e. fosfomycin disodium (FOS), clodronate disodium (CLO) and alendronate sodium (ALN)) was developed by using multiple probe BGE and indirect UV detection. BGE containing 30 mM benzoic acid, 5 mM salicylic acid and 0.5 mM CTAB (pH 3.8), temperature of 30 degrees C, applied voltage of -30 kV and detection at 220 nm provided baseline separation of all analytes (resolution (R)>2.2) in 3.2 min. EOF reversal by addition of CTAB and negative voltage polarity leading to the co-EOF flow and short analysis time. Two probe BGE greatly improved peak symmetry. The method showed good linearity (r(2)>0.999 in ranges of 20-1000 microg/mL for FOS, 100-1000 microg/mL for CLO and 100-750 microg/mL for ALN) repeatablitiy (RSD<2.15%), recovery (99.3-101.1%) and sensitivity (LOD<50 microg/mL). Freshly prepared BGE and sample solutions are essential for the method precision and accuracy. This new method can be utilized for routine analysis of FOS, CLO and ALN in dosage forms because of its efficiency, reliability, speed and simplicity.

摘要

建立了一种采用多检测池背景电解质(BGE)和间接紫外检测快速毛细管电泳法同时分析三种有机膦酸盐药物(即磷霉素二钠(FOS)、氯膦酸二钠(CLO)和阿仑膦酸钠(ALN))的方法。BGE 含有 30mM 苯甲酸、5mM 水杨酸和 0.5mM CTAB(pH3.8),在 30℃下,施加-30kV 的电压,于 220nm 检测波长,在 3.2min 内实现了所有分析物的基线分离(分辨率(R)>2.2)。CTAB 的加入和外加负电压实现电渗流反转,导致共电渗流,从而缩短了分析时间。双检测池 BGE 极大地改善了峰形对称性。该方法在 20-1000μg/mL 范围内对 FOS、100-1000μg/mL 范围内对 CLO 和 100-750μg/mL 范围内对 ALN 均显示出良好的线性(r²>0.999)。方法重复性好(RSD<2.15%),回收率高(99.3-101.1%),灵敏度高(LOD<50μg/mL)。新鲜制备的 BGE 和样品溶液对方法的精密度和准确性至关重要。由于该方法效率高、可靠性强、速度快且简单,因此可用于制剂中 FOS、CLO 和 ALN 的常规分析。

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