目的:建立利福昔明及其制剂杂质谱分析的超临界流体色谱法(SFC法)。方法:采用Torus DIOL(100 mm×3.0 mm,1.7 μm)色谱柱,以二氧化碳-乙醇和异丙醇的混合溶液(90∶10)为流动相,梯度洗脱,流速1.2 mL·min-1,柱温35 ℃,背压13.8 MPa;检测波长240 nm。结果:该方法可实现利福昔明杂质A、利福昔明Y+羟基利福昔明之间、工艺副产物和降解杂质之间及利福昔明和其相邻杂质之间的良好分离,分析速度快,该方法减小了有机试剂如甲醇和乙腈的消耗量,更为绿色环保;且可以与质谱仪直接串联,利于未知杂质的结构推测。结论:本方法可同时测定利福昔明及其制剂中的有关物质,可以区分不同工艺来源的利福昔明原料,为制剂原料供应商的筛选和制剂工艺的监控提供技术保障。
Objective: To develop a supercritical fluid chromatography (SFC) method to determine the related substances in rifaximin and its preparations. Methods: A Torus DIOL column (100 mm×3.0 mm,1.7 μm) was used. The mobile phase was CO2-the mixture of alcohol and isopropanol (90∶10) at a flow rate of 1.2 mL·min-1 with gradient mode, the column temperature was 35 ℃, the detection wavelength was 240 nm and the back pressure was 13.8 MPa. Results: Satisfied resolutions were obtained between rifaximin related process impurities, degraded impurities, rifaximin impurity A and impurity Y & hydroxy rifaximin, rifaximin and adjacent impurities. And the method was proved rapid, green, and was convenient to identify unknown impurities directly by be connected to mass detector. Conclusion: The method can be used to determine the related substances in rifaximin and its preparations, and it will play a unique and important role in fast quality evaluation of rifaximin and its preparations by distinguishing the quality of substances from different manufactures.
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