马来酸咪达唑仑片有关物质的液相色谱-电喷雾离子化-质谱分析  

Analysis of the Related Substances in Midazolam Malerte Tablets by LC-ESI-MS

作　　者：黄朝瑜[1] 李忠红[1] 姚枝玉[1] 蔡美明[1] 王玉[1] 

机构地区：[1]江苏省食品药品检验所,南京210008

出　　处：《中国药品标准》2011年第6期454-457,共4页Drug Standards of China

基　　金："十一五"国家科技支撑计划重点项目课题"常用麻醉药;放射药品安全控制检验技术研究"(2008BA155B00-001)

摘　　要：目的:对马来酸咪达唑仑片的有关物质进行分析。方法:采用高效液相色谱-电喷雾离子化-质谱联用法。PhenomenexGemini C18色谱柱(4.6 mm×100 mm,3μm);乙腈-10 mmol.L-1乙酸铵(乙酸调节pH值为4.5)(50∶50)为流动相;流速1.0mL.min-1,柱后分流;进样量10μL;DAD检测器,检测波长254 nm。质谱离子源为ESI,雾化气压力30 Pa,干燥气流量8 L.min-1,干燥温度350℃,质谱扫描质量范围50～1 200。采用全扫描一级质谱(full scan)和选择离子全扫描二级质谱(fullscan MS/MS)两种方式同时测定。结果:确证了马来酸咪达唑仑片中的两个主要杂质的结构。结论:两个主要杂质的结构的鉴定有助于马来酸咪达唑仑及马来酸咪达唑仑片的质量提高。To analyze the related substances of midazolam malerte tablets. Methods ： Detections were performed by an Ag- ilent 1100 ion trap mass spectrometer. Chromatographic separation was carried out at 25°C using a Phenomenex Gemini Cls column （4. 6 mm×100 ram, 3 μm）. The mobile phase consisted of pH 4. 5 ammonium acetate solution and acetonitrile. The flow rate was 1 mL . min-1, split after the column, diode-array detector（DAD） wavelength was at 254 nm. The mass spectrometry detector（MSD） was equipped with an ESI source, mass scan range was 50- 1 200 m/z. Samples were analyzed in two modes： MS and MS/MS full scan modes. Results ： Two main related substances of midazolam malerte were characterized. Conclusion： It＇ s essential to character- ize two main related substances in midazolam malerte tablets, and it＇ s helpful on the quality control of midazolam malerte and midazo- lam malerte tablets.

关 键 词：马来酸咪达唑仑片 有关物质 高效液相色谱-电喷雾离子化-质谱联用 

分 类 号：R921.2[医药卫生—药学]