摘要
目的 :建立柱前手性衍生化反相高效液相色谱法分离酮洛芬对映体的方法。方法 :分别以二氯亚砜和 1 ,1′ 羰基二咪唑为酰化剂 ,R (+) α 甲基苄胺作为柱前手性衍生化试剂 ,甲醇 0 .0 2 5mol·L-1磷酸二氢钾溶液 (70∶30 )作流动相 ,在Shim PackCLC ODS柱上反相色谱分离酮洛芬对映体衍生物 ,柱温 ,室温。结果 :在选定的条件下 ,酮洛芬的对映体衍生物得到分离 ,并确认了R (- ) 和S (+) 两个衍生物的色谱峰。结论 :通过酰化 ,再以R (+) α 甲基苄胺为柱前手性衍生化试剂 ,用反相色谱法 ,实现了对酮洛芬对映体的分离。
OBJECTIVE:To establish a pre column chiral derivatization reversed phase high performance liquid chromatographic method for the separation of ketoprofen enantiomers.METHODS:Thionyl chloride and 1,1′ carbonyldiimidazole were chosen as the reagents for acylation,respectively. R (+) α methylbenzylamine as the reagent for pre column chiral derivation to give two diastereomeric acylamide derivatives.These derivatives were separated on a Shim Pack CLC ODS column using MeOH 0.025 mol·L -1 KH 2PO 4(70∶30) as the mobile phase and detected by UV detector at a wavelength of 254 nm.RESULTS:Two diastereomeric acylamide derivatives were effectively separated under the chosen conditions,and two peaks were determined.CONCLUSION:A simple highly sensitive method for the separation of ketoprofen was established.It may be a suitable analysis method for ketoprofen enantiomers pharmacology studies.It may also be a purity detective method for ketoprofen eanantiomers.
出处
《中国药学杂志》
EI
CAS
CSCD
北大核心
2000年第3期194-196,共3页
Chinese Pharmaceutical Journal
