摘要
目的 建立一快速、简便的血清伊曲康唑 (ITZ)药物浓度的反相高效液相色谱测定方法。方法 2 0 0 μl血清 ,用叔丁基甲醚一步提取后氮气吹干 ,复溶后直接进样分析。流动相为甲醇 0 .5 %醋酸铵 乙醚 (36 5∶110∶2 5 ) ;流速 0 .8ml·min-1;检测波长2 6 1nm ;SupelcosilLC18色谱柱 ,柱温 40℃ ;室温操作。结果 ITZ与内标在血清中分离良好 ,tR 分别为 8.3和 10min ;10～ 5 0 0ng·ml-1浓度范围线性良好 (r=0 .9997,n =5 ) ,富集进样方法可检出浓度达 2ng·ml-1;样品操作 2 0min内可完成。结论 本方法取样量小 ,操作快速简便 ,灵敏度高 ;适用于治疗药物监测和临床药物动力学和药效学研究。
OBJECTIVE A RP HPLC assay was developed for the determination of itraconazole (ITZ) in human seurm.METHODS Suitable single step extraction proceduers by using 1.0 ml tert Butyl methyl ether were described with only 200 μl of seurm.The mobile phase was consisted of methyl alcohol 0.5% ammonium acetate ether (365∶110∶25) with the detection wavelength at 261 nm.The column Supelcolsil LC 18 (25 cm×4.6 mm,5 μm) was selected.RESULTS The assay allowed excellent linearity ( r =0.9997) over the range of 10 to 500 ng·ml -1 ,and the limit of sensitivity was 2 ng·ml -1 (50 μl inj.).The coefficients of variation for 25,150 and 400 ng·ml -1 check asmples were 1.69% to 2.91% for inter run ( n =6),and 1.78% to 3.09% for intra run ( n =10),respectively.The average recovery for them were 95% to 104% ( n =16).CONCLUSION The assay was successfully applied to the analysis of serum samples after oral administration of 200 mg ITZ in a PK/PD study.
出处
《中国药学杂志》
CAS
CSCD
北大核心
2000年第12期838-840,共3页
Chinese Pharmaceutical Journal
