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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 :本方法可用于盐酸反式曲马朵口服制剂中盐酸顺式曲马朵对映体的限量检查和盐酸反式曲马朵对映体的含量测定
Objective: To establish a method for the separation and determination of four stereoisomers of Tramadol Hydrochloride in oral preparations of trans tramadol hydrochloride. Methods: High-performance capillary electrophoresis (CE) with uncoated capillary 75 μm × 37 cm (effective length 30 cm) was used. The separation medium consisted of 40 mmol·L-1 Tris buffer (pH 25) containing 0 8 mmol·L -1 sulfobutyl- β-cyclodextrin; separation voltage 15kV, column temperature 25 ℃, detection wavelength 2 14nm; injection voltage 10kV, 20s, the entrance for the anode. Results: The enantiomers of trans - tramadol and cis - tramadol were baseline separated with (-) - deoxynemethyltramadol as the internal standard. The translocation of (+) - trans tramadol, ) - trans tramadol was 0.55-1.5 μg · mL-1. The average recoveries of (+) - tramadol hydrochloride and (-) - tramadol hydrochloride were 87% -102 4%, 96 2 8% -101 3%, RSD <5%, n = 5; The lowest detection concentration of 4 stereoisomers of tramadol hydrochloride was 5 ng · mL- The enantiomers of cis-tramadol hydrochloride in the oral formulation of trans-tramadol hydrochloride do not exceed 0 12%, and the enantiomers of the trans-tramadol hydrochloride in the labeled amount of 45 5 8% to 5 0 93 %. CONCLUSION: This method can be used to determine the enantiomers of cis-tramadol hydrochloride and the enantiomers of trans-tramadol hydrochloride in oral trans Tramadol hydrochloride preparations