UPLC-MS/MS法测定卡泊芬净血浆浓度

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 C₁₈色谱柱(100 mm×2.1 mm, 3 μm)，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/z 838.6→157.9（内标），分析时长6.5 min。结果: 卡泊芬净在0.1~25 μg/mL中呈良好的线性关系（R²=0.999 5）；定量下限为0.1 μg/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。

Determination of caspofungin in human plasma by UPLC-MS/MS

AIM: To establish a method to determine the concentration of caspofungin in human plasma by UPLC-MS/MS. METHODS: Plasma samples were spiked with roxioxithromycin as the internal standard and precipitated by methanol. The column was Ultimate AQ C₁₈ (100 mm×2.1 mm,3 μm) with the column temperature of 40 ℃. The mobile phase was acetonitrile and aqueous solution (5 mmol/L ammonium acetate, 0.2% formic acid), and the pump flow rate was 0.4 mL/min. The ion transitions were performed under ESI positive MRM model at m/z 547.5→538.2 for caspofungin and m/z 838.6→157.9 for internal standard. The analysis time was 6.5 min. RESULTS: Calibration curves of caspofungin showed good linear regression in the range of 0.1-25 μg/mL (R ²=0.999 5). The lowest quantification limit of caspofungin was 0.1 μg/mL. The extraction recovery was about 59.08%. The intra-day and inter-day relative standard deviation (RSD) were less than 15%. CONCLUSION: The established method is simple, accurate, sensitive and had good reproducibility, which can be used for the blood concentration determination of caspofungin.