超高效液相色谱-串联质谱法测定新生儿血浆中氟康唑的浓度

Determination of Fluconazole concentration in neonatal plasma by ultra performance liquid chromatography-tandem mass spectrometry

目的建立快速测定新生儿血浆中氟康唑浓度的方法。方法以非那西丁为内标,用乙腈沉淀蛋白处理血浆。色谱柱:Eclipse Plus C18 RRHD(2.1 mm×100 mm,1.8μm);流动相:0.1%甲酸-甲醇梯度洗脱;流速:0.3 ml/min;进样量:1μl。采用电化学喷雾离子源正离子模式电离,多反应监测模式检测,定量分析离子对分别为质核比(m/z)307.1→220.0(氟康唑),m/z 180.1→110.0(非那西丁)。结果该方法氟康唑在0.1001~60.0600μg/ml范围内有良好线性关系,定量下限为0.01μg/ml,准确度为82.5%~101.2%,提取回收率为85.0%~109.0%。结论该方法操作简便、快速、准确、灵敏度高,适用于新生儿血浆中氟康唑浓度的测定。

Objective To establish a method for rapid determination of Fluconazole concentration in neonatal plasma.Methods Plasma was treated with acetonitrile precipitated protein with phenacetin as internal standard.Chromatographic column:Eclipse Plus C18 RRHD(2.1 mm×100 mm,1.8μm);mobile phase:gradient elution of 0.1%formic acid-methanol;flow rate:0.3 ml/min;injection volume:1μl.Electrochemical spray ion source positive ion mode ionization,multi-reaction monitoring mode detection,quantitative analyse the ionization pairs as mass-to-charge ratio(m/z)307.1→220.0(Fluconazole)and m/z 180.1→110.0(phenacetin).Results The method had a good linearity in the range of 0.1001-60.0600μg/ml,the lower limit of quantification was 0.01μg/ml,the accuracy were 82.5%-101.2%,and the extraction recoveries were 85.0%-109.0%.Conclusion The method is simple,rapid,accurate,and high sensitive,suitable for determination of Fluconazole concentration in neonatal plasma.