盐酸反式曲马朵口服制剂中盐酸曲马朵立体异构体的分离与测定  

Separation and Determination of the Isomers of Tramadol Hydrochloride in the Oral Preparations of trans- Tramadol Hydrochloride

作　　者：刘会臣[1] 杨燕燕[1] 胡玉钦[1] 侯艳宁[1] 

机构地区：[1]白求恩国际和平医院临床药理室,石家庄050082

出　　处：《药物分析杂志》2001年第5期344-346,共3页Chinese Journal of Pharmaceutical Analysis

摘　　要：目的 :建立盐酸反式曲马朵口服制剂中盐酸曲马朵 4种立体异构体的分离测定方法。方法 :采用高效毛细管电泳法 ,未涂层毛细管 75 μm× 37cm (有效长度 30cm) ;分离介质为 40mmol·L-1Tris缓冲液 (pH 2 5 ) ,内含 0 8mmol·L-1磺丁基 - β-环糊精 ;分离电压 15kV ,柱温 2 5℃ ,检测波长 2 14nm ;进样电压 10kV ,2 0s ,入口为阳极。 结果 :以 (- ) -氧去甲基曲马朵为内标 ,反式曲马朵、顺式曲马朵的对映体达到基线分离 ,(+) -盐酸反式曲马朵、 (- ) -反式曲马朵的线性浓度范围为 0 5～ 1 5 μg·mL-1;4种制剂中 (+) -盐酸反式曲马朵和 (- ) -盐酸曲马朵平均回收率 96 87%～10 2 4%和 96 2 8%～ 10 1 3 % ,RSD <5 % ,n =5 ;盐酸曲马朵 4种立体异构体的最低检测浓度为 5ng·mL-1;4种盐酸反式曲马朵口服制剂中盐酸顺式曲马朵各对映体含量不超过 0 12 % ,盐酸反式曲马朵各对映体的含量为标示量的 45 5 8%～5 0 93 %。结论Objective:To establish a method to separate and determine the four isomers of tramadol hydrochloride in the oral preparations of trans -tramadol hydrochloride.Methods:A high performance capillary electrophoresis method was used.The electrophoretic medium was 40 mmol·L -1 Tris buffer(pH adjusted to 2 5 by H\-3PO\-4)containing sulfobutylether-β-cyclodextrin.An uncoated capillary used was 75 μm×37 cm(30 cm to the detector).Detection was carried out with an UV detector at 214 nm.The separations were performed at 25 ℃ with a positive voltage of 15 kV.Samples were injected into the capillary by voltage (10 kV) for 20 s.Results:With(-)- O -demethyltramadol as the internal standard,the four isomers of tramadol hydrochloride were well separated.Within the concentration range of 0 5～1 5 μg·mL -1 ,the peak-area ratios of the enantiomers of trans -tramadol hydrochloride were linearly related to their concentrations.For(+)and (-)- trans -tramadol hydrochloride,the relative recoveries were 96\^87%～102\^4% and 96\^28%～101\^3%;RSD was less than 5%,respectively.The lowest detection concentration was 5 ng·mL -1 for each isomer of tramadol hydrochloride.In the four tested oral preparations of trans -tramadol hydrochloride,each enantiomer of cis -tramadol hydrochloride was less than 0 12%,and each enantiomers of trans -tramadol hydrochloride was equivalant to 45 58%～50 93% of its labelled amount.Conclusion:This method could be used to analyze quantitatively the isomers of tramadol hydrochloride in its oral preparations.

关 键 词：曲马朵 立体异构体 高效毛细管电泳 手性拆分 分离 测定 镇痛药 

分 类 号：R971.1[医药卫生—药品] R927.2[医药卫生—药学]