摘要
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×150 mm,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1.0 mL.min-1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9.0 L.min-1,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 methylnahrexone bromide. Methods： The HPLC on Shim-pack The mobile phase consisted of a mixture of CLC-ODS column （4.6mm×150mm,5μm） was adopted; 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 （methylnaltrexone bromide） were analyzed. Conclusion： The method was proved to be sensitive and selective for the separation of methylnaltrexone bromide, impurities and degradation products.
出处
《药学与临床研究》
2011年第4期374-376,共3页
Pharmaceutical and Clinical Research
