离子对RP-HPLC法测定利塞膦酸钠原料药及其制剂的含量

Content Determination of Risedronate Sodium Raw Material and Its Preparations by Ion-pair RP-HPLC

目的：建立利塞膦酸钠原料药及其制剂的分析方法。方法：采用离子对反相高效液相色谱法。色谱柱为Hypersil C8，流动相为甲醇．5mmol／L磷酸二氢钠缓冲液（含6mmol／L离子对试剂四丁基溴化铵溶液，pH调至7．0）（20：80），流速为1．0ml／min，紫外检测波长为240nm，柱温为30℃。结果：利塞膦酸钠与其杂质2．（3．吡啶）乙酸及其他氧化分解产物分离良好，各峰间分离度大于2．5；利塞膦酸钠检测质量浓度线性范围为79．96-799．6Ixg／ml（r=0．9998），平均回收率为100．6％，RSD为0．5％（n=3）。结论：建立的方法简单、可靠，适用于利塞膦酸钠原料药及其制剂的常规检验。

OBJECTIVE： To establish the method for the analysis of risedronate sodium （RS） raw material and its preparations. METHODS： Ion-pair RP-HPLC method was adopted. The determination was performed on Hypersil C8 column with mobile phase consisted of methanol-5 mmol/L sodium dihydrogen phosphate buffer （containing 6 mmol/L ion-pair reagent tetrabutylammonium bromide, pH adjusted to 7.0, 20：80） at the flow rate of 1,0 ml/min. The detection wavelength was set at 240 nm and column tem- perature was 30 ~C. RESULTS： RS was well-separated from impurities as 2-（3-pyridine） acetic acid and other products of oxida- tion and decomposition with separating degree more than 2.5. The linear range of RS were 79.96-799.6μg/ml （r=0.999 8） with av- erage recovery of 100.6% （RSD=0.5%, n=3）. CONCLUSIONS： The method is simple and reliable, and it is suitable for the routine determination of RS raw material and its preparations.