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目的 :建立测定人血清中盐酸反式曲马多对映体的高效毛细管电泳方法。方法 :血清中盐酸曲马多以乙酸乙酯提取、浓缩。含 0 8mmol·L-1磺丁基 - β -环糊精的 40mmol·L-1Tris缓冲液 (磷酸调pH至 2 5 )为分离介质 ;进样电压 10kV ,2 0s,入口为阳极 ;分离电压 15kV ,柱温 2 5℃ ,检测波长 2 14nm。结果 :盐酸曲马多的 4种立体异构体达到基线分离 ,且血清组分无干扰峰 ;以盐酸顺式曲马多的一对映体为内标 ,(+) -盐酸反式曲马多、 (- ) -盐酸反式曲马多的血清浓度在 2 5～ 32 0ng·mL-1范围内 ,峰面积与内标峰面积的比值和浓度呈良好的线性关系 ;回收率在 90 %和 10 8%之间 ;日内、日间RSD分别小于 18%和 2 1% ;最低检测浓度为1 2 5ng·mL-1。结论 :本方法适用于临床药代动力学研究。
Objective: To establish a high performance capillary electrophoresis method for the determination of trans tramadol hydrochloride enantiomers in human serum. Methods: Tramadol hydrochloride was extracted with ethyl acetate and concentrated. 40 mmol·L-1 Tris buffer (adjusted to pH 2.5 with phosphoric acid) containing 0 8 mmol·L -1 sulfobutyl-β-cyclodextrin was used as the separation medium. The injection voltage was 10 kV for 20 seconds and the inlet was anodic. The separation voltage 15kV, column temperature 25 ℃, detection wavelength 2 14nm. Results: The four stereoisomers of tramadol hydrochloride reached baseline separation with no interference of serum components. One enantiomer of cis-tramadol hydrochloride was used as an internal standard, and the trans-(+) - trans tramadol (-) - trans tramadol hydrochloride in the range of 25 ~ 32 0 ng · mL-1, the peak area and internal standard peak area ratio and concentration showed a good linear relationship; recovery of 90% And 10 8% respectively. The intra-day and inter-day RSD were less than 18% and 21% respectively. The lowest detection concentration was 125 ng · mL-1. Conclusion: This method is suitable for clinical pharmacokinetic studies.