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目的:建立UPLC-MS/MS法测定血浆中卡泊芬净的浓度。方法:采用AQ C_(18)色谱柱(100mm×2.1 mm,3μm),柱温40℃,流动相为甲醇和0.2%甲酸5 mmol/L乙酸铵水溶液梯度洗脱,流速0.4 mL/min,电喷雾离子化,正离子扫描模式下,卡泊芬净m/z 547.5→538.5,罗红霉素m/z838.6→157.9(内标),分析时长6.5 min。结果:卡泊芬净在0.1~25μg/mL中呈良好的线性关系(R~2=0.9995);定量下限为0.1μg/mL;提取回收率为59.08%;日内及日间RSD<15%、准确度、精密度、稳定性等均符合生物样品测定要求。低、中、高和定量下线浓度点的卡泊芬净提取回收率相一致。结论:本方法操作简单、快捷、准确、灵敏度高且重现性良好,适用于临床上对卡泊芬净血药浓度的快速监测。
Objective: To establish a UPLC-MS / MS method for the determination of plasma concentration of caspofungin. Methods: AQ C 18 column (100 mm × 2.1 mm, 3 μm) was used. The column temperature was 40 ℃. The mobile phase consisted of a gradient of methanol and 0.2% formic acid in 5 mmol / L ammonium acetate. The flow rate was 0.4 mL / Spray ionization, positive ion scan mode, caspofungin m / z 547.5 → 538.5, roxithromycin m / z838.6 → 157.9 (internal standard), analysis time 6.5 min. RESULTS: Caspofungin showed a good linearity (R ~ 2 = 0.9995) in the range of 0.1-25 μg / mL. The lower limit of quantitation was 0.1 μg / mL. The recovery rate was 59.08%. The intra- and inter-day RSD was less than 15% Accuracy, precision, stability, etc. are in line with the requirements of biological samples. Low, medium, high and quantitative off-line concentrations of caspofungin net recovery consistent. Conclusion: The method is simple, rapid, accurate, sensitive and reproducible. It is suitable for the rapid monitoring of plasma concentration of caspofungin in clinic.