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

Determination of the sodium dodecyl sulfate in the febuxostat tablets by liquid chromatography-mass spectrometry

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,3.5μm)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0.1007～1.007μg.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.