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

关键词:  超高效液相色谱-质谱  美托洛尔  血浆

Key words:  UHPLC-MS/MS  metopolol  human plasma

摘要:

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，1.8 μm），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。

Abstract:

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 C₁₈column (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^-1for 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.