高效液相色谱-质谱联用测定非布司他片剂中十二烷基硫酸钠含量

目的:建立了高效液相色谱-质谱联用技术测定非布司他片剂中十二烷基硫酸钠(SDS)含量的方法。方法: 采用Eclipse plus C₁₈(100 mm×4.6 mm,3.5 μm)色谱柱,以乙腈-0.1 mol·L^-1乙酸胺(50:50)为流动相,采用电喷雾电离(ESI^-)、单一离子(SIM)检测模式。结果: 在优化的条件下,SDS的保留时间为8.5 min,浓度在0.1007~1.007 μg·mL^-1范围内线性关系良好(r=0.9999),回收率在98%~102%之间(RSD=1.1%)。结论: 本方法操作简便、快捷、准确,重复性好,适用于片剂中十二烷基硫酸钠的含量测定。

Objective: To develop a high performance liquid chromatography-mass spectrometry (HPLC-MS) method for determination of the sodium dodecyl sulfate (SDS) in febuxostat tablets. Methods: An Eclipse plus C18 column (100 mm×4.6 mm,3.5 μm) was adopted,and the analysis was performed with a mobile phase of acetonitrile-0.1 mol·L^-1 ethyl amide(50:50) and electrospray ionization tandem mass spectrometry in negative ionization mode (ESI^-) with single ion monitor(SIM). Results: The retention time of SDS was at 8.5 minutes under optimum conditions.A good linearity was observed in the range of 0.1007~1.007 μg·mL^-1 (r=0.9999).The average recovery was 98%~102% and the relative standard deviation(RSD) were 1.1%. Conclusion: The method is rapid,effective,reproducible,sensitive and easy to handle,which is suitable for the determination of sodium dodecyl sulfate in tablets.