LC-MS法分析研究依达拉奉中有关物质  

Analysis of Related Substances in Edaravone by LC-MS

作　　者：姚枝玉[1,2] 杭太俊[1] 王玉[2] 蔡美明[2] 黄朝瑜[2] 

机构地区：[1]中国药科大学分析化学教研室,江苏南京210009 [2]江苏省食品药品检验所,江苏南京210008

出　　处：《药学进展》2010年第9期418-422,共5页Progress in Pharmaceutical Sciences

摘　　要：目的:建立LC-MS法,分析研究依达拉奉中有关物质。方法:色谱条件:采用Kromasil100-5C18柱(4.6mm×250mm,5μm),流动相A为10mmol.L-1醋酸铵(用冰醋酸调节pH至4.0),流动相B为甲醇,梯度洗脱,流速为1.0mL·min-1,柱温为40℃,检测波长为254nm。质谱条件:电喷雾电离与大气压化学电离复合离子化源,正负离子扫描,氮气流速为8.0L·min-1,雾化器压力为60psi(1psi=6.895kPa),毛细管电压为2000V,极化电压为2000V。结果:初步鉴定了依达拉奉中3个主要有关物质,并推测了其结构及形成机制。结论:本法可用于依达拉奉中有关物质分析,并为其药品质量控制提供了有效手段。Objective： To establish a LC-MS method for the analysis of related substances in edaravone. Methods： A Kromasil 100-5 C18 column （4.6 mm×250 ram, 5μm）, 10 mmol.L-1 ammonium acetate as mobile phase A and methyl alcohol as mobile phase B were used with a column temperature of 40℃ and a detection wavelength of 254 nm at a flow rate of 1.0 mL.min-1 by gradient elution for LC. A mixed mode of ESI and APCI and full scaning in the positive and negative ion mode were used with a nitrogen flow rate of 8.0 L.min -1, a nebulizer pressure of 60 psi （ 1 psi =6. 896 kPa）, a capillary voltage of 2 000 V and a polarization voltage of 2 000 V for MS. Results： 3 main related substances in edaravone were preliminarily identified and their possible structures and formation mechanisms were speculated on. Conclusion： The method is suitabIe for the analysis of related substances in edaravone and for the quality control of the drug.

关 键 词：依达拉奉 有关物质 LC-MS法 分离 鉴定 

分 类 号：R927.2[医药卫生—药学]