利塞膦酸钠片有关物质的方法学研究

Determination method of related substances in risedronate sodium tablets

目的建立测定利塞膦酸钠片有关物质的高效液相色谱法。方法采用ODS C18色谱柱(5μm,150 mm×4.6mm),以缓冲液(取四丁基溴化铵3.22g加入1 000ml 0.05mol/L氯化铵缓冲液中,用氨水调pH至7.8±0.05)-甲醇-乙腈(2505025)为流动相;柱温:室温;流速:1.0ml/min;检测波长:254nm。结果在高温、酸、碱、氧化、强光降解下用HPLC测定,各杂质峰和主峰均有较好的分离效果,线性关系为Y=1.28×107 X-1.62×105(r=0.999 9),线性良好,稳定性良好。结论该方法测定快速、简单、准确,灵敏度高,适用于利塞膦酸钠片有关物质的测定。

Objective To establish a HPLC method for determination of related substances of risedronate sodium tablets .Methods The C18 column ,5 μm ,150 mm × 4 .6 mm ,the buffer solution （3 .22 g tetrabutyl ammonium bromide was added to a buffer solution of 1 000 ml 0 .05 mol/L ammonium chloride ,then adjusted pH to 7 .8 ±0 .05 by ammonia）methanolacetonitrile =250：50：25 as mobile phase ,column temperature：room temperature ,flow rate：1 .0 ml/min ,detection length：254 nm . Results Determined by HPLC at high temperature ,acid ,alkali degradation ,the main peak and the impurity peaks were separated well ,and the peaks had a linear relationship ,Y=1 .28 × 10^7 X-1 .62 × 10^5 （r=0 .999 9） .Conclusion The method was rapid ,simple ,accurate and sensitive ,and suitable for determination of risedronate sodium tablets related substances .