Department of Molecular Anatomy, Hamamatsu University School of Medicine, 1-20-1 Handayama, Higashi-ku, Hamamatsu, Shizuoka 431-3192, Japan.
J Chromatogr B Analyt Technol Biomed Life Sci. 2011 Jan 1;879(1):35-40. doi: 10.1016/j.jchromb.2010.11.005. Epub 2010 Nov 12.
Matrix-assisted laser desorption/ionization mass spectrometry (MALDI-MS) has been applied for the quantitative determination of β-blocker drugs in one-drop of human serum samples using drop-to-drop solvent microextraction (DDSME) as a preconcentrating probe. The optimum experimental conditions for β-blocker drugs were investigated and 1.8 μL volume of toluene for 10 min extraction time with the 5% addition of NaCl under pH 11.0 was found to be the best conditions for the separation and preconcentration of drugs from 30 μL of serum sample from a patient with high blood pressure. The optimized methodologies for DDSME/MALDI-MS analyses exhibited a good linearity with intra- and inter day precision value of 8.5-10.5% and 9.4-12.6%, respectively. The proposed DDSME/MALDI-MS offers a very simple, rapid and low-cost technique for the determination of β-blocker drugs in one drop of serum sample. The reported method has been successfully applied for the determination of propranolol and nadolol in small volume of serum sample from patient suffering from high blood pressure. In future, this technique could be applied for pharmacokinetic and clinical studies.
基质辅助激光解吸电离质谱(MALDI-MS)已被应用于一滴人血清样品中β受体阻滞剂药物的定量测定,采用液滴-液滴溶剂微萃取(DDSME)作为浓缩探针。对β受体阻滞剂药物的最佳实验条件进行了研究,发现最佳条件为:在 pH 11.0 下,加入 5%的 NaCl,用 1.8 μL 的甲苯萃取 10 min,可从高血压患者的 30 μL 血清样品中分离和浓缩药物。经优化的 DDSME/MALDI-MS 分析方法具有良好的线性关系,日内和日间精密度分别为 8.5-10.5%和 9.4-12.6%。所提出的 DDSME/MALDI-MS 提供了一种非常简单、快速和低成本的技术,可用于在一滴血清样品中测定β受体阻滞剂药物。该方法已成功应用于高血压患者小体积血清样品中普萘洛尔和纳多洛尔的测定。在未来,这项技术可以应用于药代动力学和临床研究。