手性动态固定相HPLC法拆分2-甲胺基-2-邻氯苯基环己酮对映体

Resolution of 2-Methylamino-2-o-chlorophenylcyclohexanone Enantiomers by HPLC with Chiral Dynamic State Stationary Phase

在Nova PakPhenyl色谱柱上建立了拆分2 甲胺基 2 邻氯苯基环己酮(氯胺酮)对映体的HPLC方法。以甲醇、c(H3PO4)=0 2mmol/L磷酸水溶液为流动相,V(甲醇)∶V(磷酸)=45∶55,再添加N 苄氧羰基 S 苯基 L 半胱胺酸(BPC)为手性动态固定相试剂,c(BPC)=6 5mmol/L,流动相流速1 0mL/min,检测波长254nm,氯胺酮对映体的分离选择性系数1 08,分离度1 94,质量浓度测定的线性范围0 1～2 0mg/mL,相对标准偏差0 30%～0 68%,最小检测限为0 78μg。

Resolution of enantiomers of 2methylamino2ochlorophenylcyclohexanone(ketamine) was studied by means of HPLC.Methanol and 02 mmol/L aqueous phosphoric acid〔V(methanol)∶V(aqueous phosphoric acid)=45∶55〕 was used as mobile phase,containing NbenzyloxycarbonylSphenylLcysteine (BPC) 〔c(BPC)=65 mmol/L〕as chiral dynamic state stationary phase agent,at flow rate of 10 mL/min in NovaPak Phenyl column with UVdetector of 254 nm.This method gave separation selectivity coefficient of 108,separation degree of 194,linear range of 01-20 mg/mL and relative standard deviation of 030%-068% in determination of concentration.The minimum detection limit was 078 μg.