高效毛细管电泳法分析D-苯丙氨酸与D-N-乙酰苯丙氨酸的对映体杂质含量  

Analysis of optical impurity of D-phenylalanine and D-N-acetylphenylalanine enantiomers by high performance capillary electrophoresis

作　　者：赵燕[1] 黄海涛[2] 郭艳艳[2] 马千里[2] 姜茹[1] 

机构地区：[1]第四军医大学药学系化学教研室,陕西西安710033 [2]第四军医大学学员旅,陕西西安710033

出　　处：《第四军医大学学报》2007年第13期1218-1220,共3页Journal of the Fourth Military Medical University

基　　金：第四军医大学优秀博士资助课题(2004003);第四军医大学学员课外课题(2005)

摘　　要：目的:建立高效毛细管电泳法(HPCE)测定不对称合成D-苯丙氨酸和D-N-乙酰苯丙氨酸对映体杂质含量的新方法.方法:采用HPCE法对苯丙氨酸和N-乙酰苯丙氨酸对映体的分离条件进行优化,并将该HPCE方法用于样品测定.结果:在40mmol/LTris-H3PO4(pH=2.5),60g/LS-β-CD,-15kV分离电压,20℃柱温的优化条件下,苯丙氨酸和N-乙酰苯丙氨酸对映体得到基线分离.在药物浓度为0.01～0.20g/L的考察范围内,浓度和峰面积呈良好线性,L-苯丙氨酸和L-N-乙酰苯丙氨酸的回归方程分别为:Y=1065.42X+31.02(R2=0.9989)和Y=996.02X+34.44(R2=0.9984),其中,Y为校正峰面积A/t,X为浓度(g/L).结论:该HPCE方法简单、准确,可用于苯丙氨酸和N-乙酰苯丙氨酸对映体的手性拆分和对映体杂质含量的测定.AIM： To develop a new method for determining optical impurity of D-phenylalanine and D-N-acetylphenylalanine in asymmetricly synthetic samples by high performance capillary electrophoresis （HPCE）. METHODS ： The enantioseparation of phenylalanine and N-acetylphenylalanine were investigated by HPCE to give the optimized separation condition. Furthermore, the developed method was applied for the determination of a set of samples. RESULTS： Under the optimized condition of 40 mmol/ L Tris-H3PO4 buffer of pH 2.5 containing 60 g/L S-β-CD at capillary temperature 20℃ and separation voltage - 15 kV, respectively phenylalanine and N-acetylphenylalanine enantiomers were baseline separated. Regression equations of L-phenylalanine and L-N-acetylphenylalanine were Y = 1065. 42X ＋ 31. 02 （ R^2 = 0.9989） and Y = 996.02X ＋ 54.44 （ R^2 = 0. 9984）, where Y was corrected peak area （A/t） and X was concentration （g/L）. CONCLUSION： This method is simple, precise and can be applied to the chiral separation of phenylalanine and N-acetylphenylalanine enantiomers and determination of the optical impurity.

关 键 词：高效毛细管电泳 苯丙氨酸 N-乙酰苯丙氨酸 手性分离 对映体杂质 

分 类 号：R927.2[医药卫生—药学]