LC-MS/MS在2-甲基-3-羟基吡啶合成中的应用

在抗球虫药物常山酮中间体2-甲基-3-羟基吡啶的合成反应中建立了LC-MS测定方法,合成反应液经脱色、过滤后直接测定。色谱条件:色谱柱为ZORBAX Edipse XDB C-18柱(2.1×100mm,3.5 m),流动相为甲醇-醋酸铵(醋酸铵质量分数为0.01%),二者体积比为25∶75,流速为0.2 mL/min,DAD检测器,紫外检测波长为254 nm,进样量为1μL。采用外标峰面积法进行产物定量。方法的线性范围为10~200 mg/L,线性系数r=0.999 02,相对标准偏差为1.3%,回收率在98%以上。在2-甲基-3-羟基吡啶合成反应中利用LC-MS/MS确定了最佳反应条件为反应温度180℃,反应时间16 h。

Application of liquid chromatography tandem mass spectrometry detection in synthesis of 2-methyl-3-hydroxypyridine

A detecting method by liquid chromatography tandem mass spectrometry used in synthesis of 2-methyl-3-hydroxypyridine,the important medium of Halofuginone that has excellent clinical antimalarial and antiparasitic effects on poultry,was established.After decoloring and filtering,the synthetic solution could be detected directly.The conditions of liquid chromatography: ZORBAX Edipse XDB C-18 Column(2.1×100 mm,3.5 m);mobile phase: methol ammonium acetate 0.01%(25∶75,volume ratio);rate: 0.2 mL/min;DAD detector,λUV=254 nm;sample capacity∶1 μL.The content of product was determined by external standard peak area method.The linear range and coefficient are 10～200 mg/L and 0.999 02 respectively.The standard deviation is 1.3% and the standard addition rate of recovery is over 98%.The optimal reacting temperature and time are determined by chromatography tandem mass spectrometry as 180 ℃ and 16 h respectively.