UPLC法测定人血浆中卡马西平的游离浓度

UPLC method for the analysis of free concentrations of carbamazepine in human plasma

目的建立一种测定人血浆中卡马西平游离浓度的中空纤维离心超滤(HFCF-UF)-超高效液相色谱(UPLC)法。方法血浆样本经中空纤维离心超滤技术预处理。色谱柱:Waters UPLC BEH C_(18)柱(50.0 mm×2.1 mm,1.7μm),流动相:乙腈-水=35∶65,流速:0.2 mL·min^(-1),柱温:30℃,进样量:2μL。考察该方法的专属性、标准曲线与定量下限、精密度与回收率、稳定性。结果血浆中游离卡马西平在0.2~50.0μg·mL^(-1)内,线性关系良好,标准曲线为y=2.04×10^(4) x-4.61×10^(2)(r=0.9989)。游离浓度分析方法的回收率为96.86%~104.89%,绝对回收率达到98.40%~102.40%,批内、批间RSD均小于3.00%。结论本方法简便、准确,适用于血浆中卡马西平游离浓度的分析。

Objective To establish a hollow fiber centrifugal ultrafiltration(HFCF-UF)coupled ultra-high performance liquid chromatography(UPLC)method for the analysis of free carbamazepine concentration in human plasma.Methods The plasma samples were prepared by hollow fiber centrifugal ultrafiltration.Waters UPLC BEH C_(18) column(50.0 mm×2.1 mm,1.7μm)was used.The mobile phase consisted of acetonitrile and water(35∶65)at the flow rate of 0.2 mL·min^(-1).The column temperature was maintained at 30℃.The injection volume was 2μL.The linearity,precision,accuracy and stability of the method were investigated.Results The good linear relationship of free carbamazepine were obtained in the the concentration range of 0.2-50.0μg·mL^(-1),and the standard curve was y=2.04×10^(4)x-4.61×10^(2)(r=0.9989).The method recovery rates were 96.86%-104.89%.The absolute recovery rates were 98.40%-102.40%.The intra-day and inter-day precisions(RSD)were all less than 3.00%.Conclusion The present method is simple and accurate,suitable for the analysis of free carbamazepine concentration in human plasma.