UHPLC-MS/MS测定人血浆中美托洛尔的含量

Determination of Metopolol in Human Plasma Using UHPLC Coupled to Mass Spectrometry

目的建立测定人血浆中美托洛尔含量的UHPLC-MS/MS分析方法。方法采用Agilent RRHD PLUS C18色谱柱(2.1 mm×50 mm,1.8μm),0.2%甲酸水溶液-乙腈(68∶32)为流动相。质谱采用电喷雾离子源(ESI),多反应监测(MRM),检测离子为正离子,分别选择m/z 268/116、237/194作为美托洛尔和内标(卡马西平)的检测离子对。结果血浆中美托洛尔在1.012~759.0 ng·mL^(-1)内线性关系良好(r=0.999 2)。高、中、低浓度美托洛尔的基质效应分别为105.9%,106.1%,106.9%;平均回收率分别为83.0%,99.3%,95.2%。批内精密度RSD≤3.22%,批间精密度RSD≤4.14%。结论该方法简便、灵敏、快速、准确,适用于血浆中美托洛尔的含量测定。

OBJECTIVE To establish a method for determine metopolol in human plasma using UHPLC coupled to mass spectrometry. METHODS The chromatographic separation was achieved on Agilent RRHD PLUS C_（18） column（2.1 mm× 50 mm, 1.8 μm）, using mobile phase as a mixture of water（0.2% formicacid）-acetonitrile（68∶32）. The multiple reaction monitoring mode of the positive ion was adopted during MS detection（electrospray ion source）, and precursors to the product ion transitions of m/z 268/116, 237/194 were used to measure metoprolol and the internal standard（carbamazepine）. RESULTS The calibration curve was linear in the range of 1.012-759.0 ng·mL^-1 for metopolol in human plasma（r=0.999 2） with matrix effect of 105.9%, 106.1%, 106.9% and extraction recovery experiments of metoprolol of 83.0%, 99.3%, 95.2%, respectively. The within-run accuracy RSD was ≤3.22%, and between-run accuracy RSD was ≤4.14%. CONCLUSION The method is simple, accurate, quick and sensitive for determination of metopolol in human plasma.