双苯氟嗪中杂质的结构分析  

Structure analysis on impurities in dipfluzine

作　　者：陈汝红[1] 王熳[1] 刘松雁 边铭 赵曦[3] 王永利[4] 

机构地区：[1]河北省药品检验所,河北石家庄050011 [2]石家庄市兽产品质量监测中心,河北石家庄050041 [3]石药集团中奇制药技术有限公司,河北石家庄050051 [4]河北医科大学药学院,河北石家庄050017

出　　处：《中国医院药学杂志》2011年第15期1241-1244,共4页Chinese Journal of Hospital Pharmacy

基　　金：国家一类新药-双苯氟嗪的开发;国家高科技研究发展计划(863计划)资助项目(编号:2002AA2Z3132)

摘　　要：目的:采用高效液相色谱-串联质谱(HPLC-MS/MS)和高效液相色谱-二极管阵列检测(HPLC-PDA)法对双苯氟嗪中的杂质进行结构分析。方法:采用C18柱,甲酸铵溶液(用甲酸调节pH至3.2)-甲醇为流动相,线性梯度洗脱,流速0.5 mL.min-1,柱温45℃,MS/MS和PDA分别检测。结果:双苯氟嗪中的主要杂质有效分离,通过解析获取的质谱和紫外信息,结合原料合成工艺,对其中3个未知杂质的结构进行了推断。结论:本实验分离鉴别了双苯氟嗪中的主要杂质,为双苯氟嗪的质量控制和工艺优化提供了参考。OBJECTIVE To analyze structures of impurities in dipfluzine by means of HPLC-MS/MS and HPLC-PDA. METHODS The HPLC separation was carried on an ODS column by linear gradient elution with a mixture solution of ammonium formate solution （adjust pH to 3. 2 with formic acid） and methanol. The flow rate was 0. 5 mL·min^-1 and the column temperature was 45℃. Sample was detected by MS/MS and PDA respectively. RESULTS Major impurities in dipfluzine could be effectively separated. Through analysing informations of MS and UV acquired and combining synthetic process of raw material,deduced structures of three unknown impurities in dipfluzine. CONCLUSION The test separated and identified major impurities in dipfluzine sample and was useful for its quality control and process optimization.

关 键 词：双苯氟嗪 杂质 结构分析 高效液相色谱-串联质谱 高效液相色谱-二极管阵列检测 

分 类 号：R917[医药卫生—药物分析学]