摘要
目的使用电雾式检测器(CAD)建立一种HPLC方法测定人血浆中白消安的浓度。方法取血浆样品,以卡马西平为内标,加入乙酸乙酯进行液液萃取,氮气吹干后用流动相复溶,取上清液进样。使用Hypersil GOLD C18(4.6 mm×250 mm,5μm)色谱柱分离,以甲醇-水为流动相进行梯度洗脱,流速:1.0 mL·min^(-1),柱温:30℃,检测器为电雾式检测器,雾化气体为氮气,蒸发温度:35℃,进样量:20μL。结果在该色谱条件下,待测物及内标可良好分离,其他内源性物质峰均无干扰。白消安在0.1~10μg·mL^(-1)线性关系良好,批内、批间精密度RSD均小于3.0%,提取回收率高于85%。结论本研究所建立的HPLC法操作简洁,选择性强,灵敏度高,结果准确可靠,适用于临床诊疗监测及药效学研究。
Objective To develop a new high performance liquid chromatography(HPLC)method for determination the concentration of Busulfan in human plasma by using charged aerosol detection(CAD).Methods Plasma samples and carbamazepine solution which was used as the internal standard were extracted with ethyl acetate,re-dissolved with the mobile phase after drying with nitrogen and took the supernatant for the determination.Chromatographic separation was performed on a Hypersil GOLD C18 column(4.6 mm×250 mm,5μm)at 30℃using the mobile phase of methanol-water with gradient elution at a flow rate of 1.0 mL·min^(-1).CAD was used as the detector,nitrogen was used as the nebulizer gas and the evaporation temperature was set at 35℃,the injection volume was 20μL.Results Under this chromatographic conditions,the analytes and internal standard were completely separated and other endogenous compounds had no interference.The calibration curve of busulfan was linear over the range of 0.1-10μg·mL^(-1).The precision and accuracy RSDs of intra-day and inter-day were both less than 3.0%.The average extraction recovery was above 85%(n=6).Conclusion The HPLC-CAD method established in this study has the advantages of simple operation,strong selectivity,high sensitivity,accurate and reliable results,which can be applied in pharmacokinetics and pharmacodynamics study and therapeutic drug monitoring.
作者
刘思鲁
胡蕾
刘博宇
陶依然
黄琳
封宇飞
LIU Si-lu;HU Lei;LIU Bo-yu;TAO Yi-ran;HUANG Lin;FENG Yu-fei(Department of Pharmacy,Peking University People’s Hospital,Beijing 100044,China)
出处
《中国临床药理学杂志》
CAS
CSCD
北大核心
2023年第5期738-741,共4页
The Chinese Journal of Clinical Pharmacology
关键词
高效液相色谱法
电雾式检测器
白消安
血浆浓度
high performance liquid chromatography(HPLC)
charged aerosol detection(CAD)
busulfan
plasma drug concentration
