Division of Clinical and Translational Research, Department of Anesthesiology, Washington University in St. Louis, St. Louis, MO 63110, United States.
J Pharm Biomed Anal. 2011 Jun 1;55(3):487-93. doi: 10.1016/j.jpba.2011.01.040. Epub 2011 Mar 5.
A fast, sensitive and selective liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for the determination of alfentanil and midazolam in human plasma has been developed and validated. Alfentanil and midazolam were extracted from plasma using a mixed-mode cation exchange solid phase extraction method, with recoveries of both compounds greater than 80% at 3 different concentrations (1, 10 and 100ng/ml). Compounds were analyzed on a C(18) column with a water and methanol mobile phase gradient with acetic acid as an additive, at a flow rate of 0.3ml/min. The working assay range was linear from 0.25 to 100ng/ml for each compound. The signal to noise ratio was 80 and 40 for alfentanil and midazolam, respectively, at the lowest concentration calibration standard, with less than 10% matrix suppression by human plasma at this concentration. Alfentanil and midazolam were stable in human plasma during storage at -80°C, processing, and analysis. The procedure was validated and applied to the analysis of plasma samples from healthy human subjects administered oral and intravenous alfentanil and midazolam.
建立并验证了一种快速、灵敏和选择性的液相色谱-串联质谱（LC-MS/MS）法，用于测定人血浆中的阿芬太尼和咪达唑仑。阿芬太尼和咪达唑仑采用混合模式阳离子交换固相萃取法从血浆中提取，在 3 种不同浓度（1、10 和 100ng/ml）下，两种化合物的回收率均大于 80%。化合物在 C（18）柱上用含有乙酸的水和甲醇流动相梯度进行分析，流速为 0.3ml/min。工作检测范围对每个化合物均为 0.25-100ng/ml 呈线性。在最低浓度校准标准下，阿芬太尼和咪达唑仑的信噪比分别为 80 和 40，在该浓度下，人血浆的基质抑制小于 10%。阿芬太尼和咪达唑仑在-80°C 下储存、处理和分析过程中在人血浆中稳定。该方法经过验证后，应用于口服和静脉给予阿芬太尼和咪达唑仑的健康人体血浆样品的分析。
