Analytical Chemistry Division, Department of Chemistry, Sri Venkateswara University, Tirupati-517502, India.
Acta Pharm. 2010 Jun;60(2):177-84. doi: 10.2478/v10007-010-0012-0.
A high-performance liquid chromatography-tandem mass spectrometric method was developed and validated for the determination of metoprolol in human plasma. The analyte and internal standard, nevirapine, were extracted from plasma matrix by liquid-liquid extraction with ethyl acetate. Chromatographic separation was achieved on a C-18 analytical column with an isocratic mobile phase of 15:85 (V/V) 10 mmol L-1 ammonium acetate (pH 5.0)/acetonitrile. The atmospheric pressure chemical ionization technique was used for sample ionization in positive ion mode and enhanced selectivity was achieved by tandem mass spectrometric analysis via two multiple reaction monitoring (MRM) transitions, 268.2 → 116.2 for metoprolol and 267.1 → 226.2 for nevirapine, respectively. The assay was validated for human plasma over a concentration range of 1-200 ng mL-1 with the precision and accuracy ranging from 0.9 to 8.8% and 89.9 to 105.8%, respectively.
建立并验证了一种高效液相色谱-串联质谱法，用于测定人血浆中的美托洛尔。采用乙酸乙酯进行液-液萃取，从血浆基质中提取分析物和内标奈韦拉平。采用 C-18 分析柱，以 15:85（V/V）10mmol/L 乙酸铵（pH5.0）/乙腈为等度流动相进行色谱分离。采用大气压化学电离技术在正离子模式下进行样品离子化，通过两条多重反应监测（MRM）跃迁（美托洛尔为 268.2→116.2，奈韦拉平为 267.1→226.2）进行串联质谱分析，从而提高了选择性。该测定方法在 1-200ng/mL 的浓度范围内对人血浆进行了验证，其精密度和准确度的范围分别为 0.9%-8.8%和 89.9%-105.8%。
