HPLC法同时测定洛索洛芬钠片中的5个已知杂质

Simultaneous determination of five known impurities in loxofen sodium tablets by HPLC

目的:对洛索洛芬钠片的有关物质检测方法进行优化,提高杂质分离度和检出率。方法:采用Intersil ODS-3(4.6 mm×250 mm, 5μm);流动相为0.01 mol·L^(-1)的磷酸二氢钾溶液(pH 4.5)-乙腈(85∶15)(A)和0.01 mol·L^(-1)的磷酸二氢钾溶液(pH 4.5)-乙腈(15∶85)(B),梯度洗脱,流速1.0 mL·min^(-1);检测波长220 nm;柱温40℃;进样体积20μL。结果:洛索洛芬钠与相邻杂质以及5个已知杂质之间均达到的分离、洛索洛芬钠和5个已知杂质的浓度与峰面积之间线性关系(r>0.999 9)、精密度、准确度和耐用性均良好;洛索洛芬钠片3批自制制剂与3批参比制剂的杂质谱基本一致,各批样品均符合制订质量标准的规定。结论:本法可用于洛索洛芬钠片有关物质的质量控制。

Objective:To improve the separation and detection rate of impurities by optimizing the detection method of related substances in loxofen sodium tablets.Methods:Intersil ODS-3(4.6 mm×250 mm,5μm)was adopted with 0.01 mol·L^(-1) potassium dihydrogen phosphate solution(pH 4.5)-acetonitrile(85∶15)(A)and 0.01 mol·L^(-1) potassium dihydrogen phosphate solution(pH 4.5)-acetonitrile(15∶85)(B)as mobile phase bygradient elution at a flow rate of 1.0 mL·min^(-1).Detection wavelength was set at 220 nm.Column temperature was 40℃.Injection volume was 20μL.Results:Loxofen sodium and adjacent impurities and five known impurities were separated and the linear relationship between the concentration and peak area(r>0.9999),the precision,accuracy and durability were met requirements.The impurity spectra of three batches of loxofen sodium tablets from self-made were basically the same as those of three batches of reference preparations.All batches of samples were in accordance with the provisions of quality standards.Conclusion:The method can be used for the quality control of related substances in loxoprofen sodium tablets.