目的:建立梯度洗脱反相高效液相色谱法测定溴甲纳曲酮中的有关物质.方法:采用高效液相色谱法,色谱柱为Shim-pack CLC-ODS(4.6 mm×150mm,5μm),以甲醇-水-三氟乙酸(5:95:0.1)为流动相A,以甲醇-水-三氟乙酸(65:35:0.1)为流动相B,以1.0mL·min的流速进行梯度洗脱,进样量20μL,检测波长230 nm.电喷雾电离源(ESI),电离源电压4.0 kV,喷雾气氮气的流速为9.0L·min,干燥气温度为325℃,柱后分流;质谱扫描质量范围m/z 100～1000.结果:各有关物质与主成分均达到基线分离,分析了溴甲纳曲酮粗品中的杂质可能结构.结论:本法灵敏、专属,能有效分离降解产物及有关物质,可用于有关物质及降解产物检查.%Objective: To establish an HPLC method to analyze the related substance of methylnaltrexone bromide.Methods: The HPLC on Shim-pack CLC-ODS column (150 mm × 4.6 mm, 5 μm) was adopted;The mobile phase consisted of a mixture of methanol-water-TFA (5∶95∶0.1) as mobile phase A and a mixture of methanol-water-TFA (65∶35∶0.1) as mobile phase B.Gradient elution was used.The flow rate was 1.0 mL·min-1, the wavelength was set at 230 nm.Eletrospray ionization mass spectrum was applied, the spray capillary voltage was 4.0 kV, flow rate of dry gas N2 was 9.0 L·min-1, the dry gas temperature was set at 325 ℃, and the scan range was m/z 100～1000.Results: The structures of impurities appeared in rough product (methylnahrexone bromide) were analyzed.Conclusion: The method was proved to be sensitive and selective for the separation of methylnaltrexone bromide, impurities and degradation products.
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