FMOC柱前衍生化HPLC法测定阿仑膦酸钠片含量及有关物质4-氨基丁酸

目的建立9-氯甲酸芴甲酯（FMOC）柱前衍生化高效液相色谱法测定阿仑膦酸钠片的含量及其有关物质4-氨基丁酸。方法碱性条件下供试品与FMOC衍生化反应,采用ODS-2HYPERSILC18色谱柱,乙腈-0.4%EDTA（pH=7.2）（35∶65）为流动相,测定阿仑膦酸钠的衍生化产物;以乙腈-0.4%EDTA（pH=7.2）（40∶60）为流动相,测定4-氨基丁酸衍生化产物,紫外检测器（λ=265nm）,荧光检测器（λex=260nm,λem=310nm）。结果阿仑膦酸钠浓度在10～60μg·mL-1范围内（UV265nm）线性关系良好（r=0.9996）;平均回收率100.3%（n=9）。有关物质4-氨基丁酸浓度在1～5μg·mL-1范围内（UV265nm）线性关系良好（r=0.9998）。结论本方法简单、准确、灵敏。

Determination of Alendronate Sodium Tablets and Its Related Substances 4-Aminobutyric by HPLC Pre-column Derivatization with FMOC

Objective A HPLC method with pre-column derivatization has been developed for test of related substances 4-aminobutyric and determination of Alendronate Sodium Tablets.Methods Alendronate sodium was derivatized with 9-fluorenylmethyl chloroformate（FMOC）in 0.05mol Na2CO3 solution,the analytical column was ODS-2 HYPERSIL C18,acetonitrile-0.4%EDTA（pH7.2）（35∶65）as mobile phase for alendronate sodium and acetonitrile-0.4%EDTA（pH7.2）（35∶65）as mobile phase for 4-aminobutyric acid,UV detection at 265nm;FLD λex=260nm, λem= 310nm. Results Alendronate sodium was linear at the concentration range of 10～60μg·mL^-1 （UV265nm; r= 0. 9996） and 4-aminobutyric acid was linear at the concentration range of 1μg·mL^-1 （UV265nm;r=0. 9998）. The average recovery rate of alendronate sodium was 100. 3%（n=9）. Conclusions The method is sample, accurate and sensitive.