HPLC法测定人尿液中奥拉西坦的浓度

Determination of Oxiracetam in Human Urine by HPLC

目的:建立测定人尿液中奥拉西坦浓度的方法,为奥拉西坦代谢途径的研究提供参考。方法:尿液以甲醇沉淀蛋白后,以高效液相色谱法进样测定,其中色谱柱为Symmetry shiedTM RP18柱,流动相为乙腈-水(5∶95),流速为0.5ml/min,检测波长为210nm,柱温为40℃,进样量为20μl,内标为阿昔洛韦。结果:奥拉西坦尿药浓度在20～2400mg/L范围内线性关系良好;低、中、高3种浓度尿液样品的绝对回收率分别为(90.38±4.93)%、(93.71±3.54)%、(95.04±2.31)%,方法回收率分别为(98.32±1.96)%、(104.99±1.74)%、(103.4±2.43)%;日内RSD分别为3.40%、4.76%、1.04%,日间RSD分别为2.82%、3.64%、1.90%;试验数据显示人口服奥拉西坦胶囊(1600mg)24h内尿液中排出原型药32.89%。结论:本方法简便、准确、灵敏度高,可用于人尿液中奥拉西坦药动学的研究。

To establish the method for the determination of oxiracetam in human urine, and to provide reference for the study of metabolic pathways of oxiracetam. METHODS： After precipitated with methanol, HPLC method was adopted for the content determination. With acyclovir as an internal standard, a Symmetry shiedTM RP18 column was used with mobile phase consisted of acetonitrile-water （5：95） at the flow rate of 0.5 ml/min. The column temperature was 40 ℃ and the detection wave- length was set at 210 nm. The injection volume was 20 μl. RESULTS： The linear ranges of oxiracetam were 20-2 400 mg/L. Absolute recoveries of urine at low, middle and high concentrations were （90.38 ± 4.93）%, （93.71 ± 3.54）% and （95.04 ± 2.31）%, and the method recoveries were （98.32 ± 1.96） %, （104.99 ± 1.74） % and （103.4 ± 2.43） %. The intra-day RSDs of urine at three concentrations were 3.40%, 4.76% and 1.04%, and inter-day RSDs were 2.82%, 3.64% and 1.90%, respectively. Trial data showed that 32.89% original drug discharged in 24 h after oral administration of Oxiracetam capsules （1600 mg）. CONCLUSION： The method is simple, accurate, sensitive, and can be used for the pharmacokinetic study of oxiracetam in urine.