柱前衍生HPLC法测定阿仑膦酸钠骨化三醇片中阿仑膦酸钠的含量

目的建立阿仑膦酸钠骨化三醇片中阿仑膦酸钠的含量测定方法。方法用0.1%FMOC的乙腈溶液进行柱前衍生,色谱柱填料为苯乙烯-二乙烯苯共聚物（Hamilton PRP-1柱适用）;流动相为乙腈-甲醇-0.05mol/L磷酸氢二钠和0.05mol/L枸橼酸钠混合液（用磷酸调pH8.0）（20∶5∶75）;检测波长266nm。结果阿仑膦酸钠（以阿仑膦酸计）在5～15μg/ml的浓度范围内有良好的线性关系（r=0.99998,n=5）;平均回收率为100.8%,RSD=1.1%（n=9）。结论该方法稳定,准确度、精密度高,重复性好,可用于阿仑膦酸钠骨化三醇片中阿仑膦酸钠的含量测定。

Determination of the content of Sodium alendronate in Sodium alendronate and calcitriol tablets by HPLC with precolumn derivatization

Objective To establish a method for the content determination of Sodium Alendronate in Sodium Alendronate and Caleitriol Tablets. Methods Preeolumn derivatization was carried out with O. 1% FMOC solution in acetonitrile. The packing material of the column was styrene-divinylbenzene copolymer, and the mobile phase consisted of acetonitrile-methanolmixed solution containing 0.05mol/L disodium hydrogen phosphate and 0.05 mol/L sodium citrate （ pH value was adjusted to 8.0 with phosphoric acid） （20： 5：75 ）. The detective wavelength was 266 nm. Results The calibration carve of sodium alendronate （ calculated by alendronic acid） showed good linearity over the range of 5 - 15μg/ml （ r = 0. 99998 ,n = 5 ）. The average recovery was 100. 8% with RSD of 1.1% （n = 9）. Conclusion This method is stable, accurate,precise and with good repeatability,it can be used for the content determination of Sodium Alendronate in Sodium Alendronate and Calcitriol Tablets.