摘要
目的:建立测定血浆中赖诺普利浓度的方法,为临床血药浓度的测定提供快速、有效的分析手段。方法:高效液相色谱法荧光法,采用HypersilODS柱,流动相为20mmol/LKH2PO4缓冲液(pH=3.0)-甲醇(35∶65,V/V),流速为1.0mL/min;血浆样品经固相萃取后与荧光试剂(荧光胺)发生衍生化反应,进样量为20μL;荧光检测器的激发波长为383nm,发射波长为477nm。结果:赖诺普利浓度在2~200ng/mL范围内线性关系良好(r=0.9978),平均绝对回收率为68.55%(n=15),日内与日间精密度均小于3%,最低检测限为1ng/mL;内源性物质不干扰测定。结论:高效液相色谱荧光法工作曲线稳定,灵敏度高,操作步骤简单,可以用于赖诺普利的药动学和药效学研究及临床血药浓度的监测。
Objective:To develop and validate HPLC-fluorescence method for lisinopr il determination in human plasma.Methods:Hypersil ODS column was applied,and mob ile phase was potassium dihydrogen phosphate solutions (20 mmol/L,pH=3.0)-methan ol (35 ∶65,V/V). The flow rate was 1.0 mL/min.Detection and quantification of l isinopril was by fluorescence (λex=373 nm;λem=477 nm) and the injected volume was 20 μL.Plasma samples were treated using a solid-phase extraction procedure. Results:The calibration curve for lisinopril assay exhibited excellent linear re lationship with a correlation coefficient 0.997 8 in the concentration range of 2~200 ng/mL.The absolute recovery of assay was 68.55%(n=15).The within-day and inter-day precision (RSD) was less than 3%.The detection limit was 1 ng/mL. Conc lusion:The method is simple,accurate and allows to be used as analytical method to analyze samples from clinical studies.
出处
《中国药业》
CAS
2005年第7期72-73,共2页
China Pharmaceuticals