液相色谱-串联质谱法测定血浆中甲氧基肾上腺素和甲氧基去甲肾上腺素

Determination of Metanephrine and Nometanephrine in Plasma by Liquid Chromatography-Tandem Mass Spectrometry

建立了血浆中甲氧基肾上腺素和甲氧基去甲肾上腺素的液相色谱-串联质谱定量测定方法。生物样本经过固相萃取方式进行前处理,采用Venusil XBP Silica色谱柱(100 mm×2.1 mm,3μm)分离,流动相为甲酸-甲酸铵水溶液(A相)和甲酸-水-甲酸铵乙腈溶液(B相),梯度洗脱。在电喷雾正离子模式下,以多反应监测模式检测待测组分。在最优条件下,分析物在相应的浓度范围内相关系数均大于0.999,加标回收率为85%~109%。

A method for determining metanephrine and nometanephrine in plasma by liquid chromatography-tandem mass spectrometry was developed.The biological sample was pretreated by solid phase extraction,then the separation was performed using a Venusil XBP Silica column.Electrospray ionization mass spectrometry was operated in the positive monitoring mode for the analytes.The mobile phases of formic acid-ammonium formate in deionized water(mobile phase A)and formic acid-water-ammonium formate in acetonitrile(mobile phase B)were used at a flow rate of 0.6 mL/min.Under the optimized conditions,the correlation coefficients of linear calibration curves were over 0.999 in the corresponding concentration ranges.The overall recoveries varied from 85%to 109%.