新型在线柱萃取高效液相色谱法测定异烟肼的血药浓度

目的建立新型在线柱萃取HPLC法测定人血浆中异烟肼血药浓度,用于异烟肼的日常治疗药物监测。方法新型在线柱萃取HPLC由萃取系统和分析系统两部分构成。萃取柱为Aston RG SCX（20 mm×4.6 mm,5μm,ANAX）,分析柱为Aston RG C18（250 mm×4.6 mm,5μm）;两系统通过六通阀连接,采用＂中心切割＂模式及陷阱柱转移目标物;检测波长为340 nm,样品经蛋白沉淀、衍生,进样量为50μL,采用外标法计算结果。结果异烟肼在0.18～35.84μg.mL^-1与峰面积呈良好线性关系,相关系数为0.999 8,最低检测限为0.02μg.mL^-1,低（0.18μg.mL^-1）、中（2.24μg.mL^-1）、高（35.84μg.mL^-1）浓度的绝对回收率为91.6%～95.9%,日内和日间RSD均〈5.0%,准确度为98.7%～101.5%。结论本方法具有抗干扰能力强、自动化程度高、准确度和精密度好等优点,完全适合异烟肼的日常治疗药物监测。

Determination of isoniazid in human plasma by new online column extraction HPLC

Objective To establish a method to determine isoniazid in human plasma by the new online column extraction HPLC to monitor isoniazid in human plasma.Methods New column extraction HPLC consisted of extraction system and analysis system.The extraction column was Aston RG SCX（20 mm×4.6 mm,5 μm,ANAX）,and the analytical column was Aston RG C 18（250 mm×4.6 mm,5 μm）.Two systems were connected through the 6-way valve,and the ＂central cutting＂ mode to transfer targets to trap column was used.The detection wavelength was 340 nm.Samples were pretreated by derivatization and protein precipitation.Injection volume was 50 μL.Results were calculated by the external standard method.Results Isoniazid had good linearity at 0.18-35.84 μg.mL-1（r = 0.999 8）.LOD was 0.02 μg.mL-1.Absolute recoveries of all concentrations were between 91.6% and 95.9%.RSD of intra-day and inter-day precisions were less than 5%.Accuracy ranged from 98.7% to 101.5%.Conclusion This method has strong anti-interference capability,a high degree of automation,high accuracy and high sensitivity and perfectly suitable for routine isoniazid therapeutic drug monitoring.