摘要
目的建立超高效液相色谱法测定人血清中卡马西平（CBZ）、苯妥英钠（PHT）、苯巴比妥（PB）、奥卡西平（OXC）活性代谢产物利卡西平（MHD）的浓度。方法于2014年1月～2015年6月收集血清样品经甲醇沉淀蛋白后直接进样测定,采用Shim-pack XR-ODSⅢ柱（1.6μm,75 L×2.0）。流动相为甲醇-水,采用梯度洗脱程序;扫描波长200～360 nm,检测波长为210 nm,流速：0.4 m L/min,柱温：35℃,进样体积：10μL。结果 CBZ、PHT、PB、MHD均能达到良好分离,与相邻峰的分离度（R）均〉1.5;线性范围分别为（1.00～32.00）μg/m L（r=0.9997）、（2.55～81.60）μg/m L（r=0.9997）、（2.35～75.20）μg/m L（r=0.9999）、（2.50～80.00）μg/m L（r=0.9998）;方法回收率〉97%;日内和日间精密度的相对标准偏差（RSD）均〈1.6%。结论超高效液相色谱法（UPLC）快速、简便、准确,适用于临床治疗药物监测。
Objective To establish a simple UPLC method for the simultaneous determination of carbamazepine（CBZ）,phenytoin sodium（PHT）,phenobarbital（PB）,active metabolite of oxcarbazpine（OXC）-licarbazepine（MHD） in human serum.Methods The analytes were extracted by methanol protein precipitation in our hospital from January 2014 to June 2015.The extracts were injected onto an Shim-pack XR-ODS Ⅲ column.The mobile phase was methanol-water by gradient elution.The wavelength for scanning ranged from 200-360 nm,and the detective wavelength was 210 nm.The flow rate was 0.4 m L/min,and the column temperature was set at 35°C.The volume of loading sample was 10 μL.Results Carbamazepine,phenytoin sodium,phenobarbital and licarbazepine were separated well under the chromatographic condition,with the degree of separation（R） of adjacent peaks were greater than 1.5.The method was found to be linear over the concentration ranges investigated,1.00-32.00 μg/m L（r=0.9997） for CBZ,2.55-81.60 μg/m L（r=0.9997）for PHT,2.35-75.20 μg/m L（r=0.9999） for PB,2.50-80.00 μg/m L（r=0.9998） for MHD.The recoveries of CBZ,PHT,PB,OXC were more than 97%,and the intra-and inter-day validation were adequate with the RSDs of 1.6% or below.Conclusion UPLC is proved to be convenient,accurate and suitable to measure concentrations of the four analytes in clinical samples.
出处
《中国现代医生》
2016年第12期105-107,111,共4页
China Modern Doctor
基金
福建省科技厅社会发展引导性项目(2015Y0055)
福建省卫计委青年科研课题(2015-1-60)
