Gubbins P O, Gurley B J, Bowman J
Department of Pharmacy Practice, University of Arkansas for Medical Sciences, Little Rock 72205, USA.
J Pharm Biomed Anal. 1998 Feb;16(6):1005-12. doi: 10.1016/s0731-7085(97)00062-9.
Published high performance liquid chromatographic (HPLC) methods for the determination of itraconazole (ITZ) in biological matrices are labor intensive, extraction-based procedures which operate at a pH approaching the limit of column tolerance, and unless modified, cannot measure its hydroxy-metabolite (OH-ITZ). A protein precipitation-based method requiring no solvent extraction and utilizing a base-deactivated C18 analytical column to minimize peak tailing is described herein. Calibration curves for OH-ITZ and ITZ were linear from 25-1500 ng ml-1 (r2 > or = 0.999). Intra-assay relative standard deviations (R.S.D.) were below 12%. Inter-assay R.S.D. were below 14%. This method provides a rapid means for the accurate and precise determination of both OH-ITZ and ITZ concentrations in human serum.
已发表的用于测定生物基质中伊曲康唑（ITZ）的高效液相色谱（HPLC）方法是劳动密集型的、基于萃取的程序，其在接近色谱柱耐受极限的pH值下运行，并且除非进行改进，否则无法测量其羟基代谢物（OH-ITZ）。本文描述了一种基于蛋白质沉淀的方法，该方法无需溶剂萃取，并使用碱钝化的C18分析柱来最小化峰拖尾。OH-ITZ和ITZ的校准曲线在25-1500 ng ml-1范围内呈线性（r2≥0.999）。批内相对标准偏差（R.S.D.）低于12%。批间R.S.D.低于14%。该方法为准确、精确地测定人血清中OH-ITZ和ITZ的浓度提供了一种快速手段。
