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建立了LC-MS/MS法测定人血浆中的氟康唑(1)。采用C_(18)色谱柱,以甲磺酸酚妥拉明(2)为内标,2 mmol/L乙酸铵溶液(含0.05%甲酸)-甲醇(40∶60)为流动相,电喷雾离子化源,选择性正离子多反应监测,检测离子分别为m/z 307.2→238.2(1)和m/z 282.2→212.2(2)。1在0.03～10μg/ml浓度范围内线性关系良好,方法回收率大于94%,提取回收率大于90%,日内和日间RSD均小于5.4%。20名男性健康志愿者单剂量口服1片150 mg,主要药动学参数为c_(max)(3.26±0.54)μg/ml,t_(max)(1.42±0.65)h,t_(1/2)(29.75±4.89)h,AUC_(-120h)(131.4±23.4)μg·ml~1·h和AUC_(0→∞)(140.5±26.3)μg·ml~1·h。
A LC-MS / MS method was developed for the determination of fluconazole in human plasma (1). The mobile phase consisted of 2 mmol / L ammonium acetate solution (containing 0.05% formic acid) and methanol (40:60) with the mobile phase of C 18 column and phentolamine (2) mesylate as the internal standard. The source and selective positive ion multi-reaction monitoring, detection of ions were m / z 307.2 → 238.2 (1) and m / z 282.2 → 212.2 (2). 1 had a good linearity in the concentration range of 0.03 ~ 10μg / ml. The recovery rate was more than 94% and the recovery rate was more than 90%. The RSDs were less than 5.4% in both day and day. Twenty (20) male healthy volunteers took a single oral dose of 150 mg and the main pharmacokinetic parameters were c max (3.26 ± 0.54) μg / ml and t max (1.42 ± 0.65) h, t 1/2 (29.75 ± 4.89) h, AUC_ (-120h) (131.4 ± 23.4) μg · ml ~ 1 · h and AUC_ (0 → ∞) (140.5 ± 26.3) μg · ml ~ 1 · h, respectively.