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混合模式阳离子交换柱和气相色谱-质谱联用技术用于人血浆中丙泊酚的选择性精准测定方法

Selective and Accurate Determination Method of Propofol in Human Plasma by Mixed-Mode Cation Exchange Cartridge and GC-MS.

作者信息

Pyo Jae Sung

机构信息

College of Pharmacy, Kyungsung University, Busan 48434, Republic of Korea.

出版信息

J Anal Methods Chem. 2016;2016:9531769. doi: 10.1155/2016/9531769. Epub 2016 Aug 11.

Abstract

A gas chromatography-mass spectrometry (GC-MS) method for the determination of propofol in human plasma has been developed and validated. Propofol was extracted from human plasma by using mixed-mode cation exchange/reversed-phase (MCX) cartridges. As propofol easily volatilizes during concentration, 100% methanol was injected directly into GC-MS to elute propofol. Despite avoiding concentration process of the eluted solution, lower limit of quantization (LLOQ) of propofol was 25 ng/mL. The validated method exhibited good linearity (R (2) = 0.9989) with accuracy and precision -5.8%11.7% and 3.7%11.6%, respectively. The other validation parameters, recovery and matrix effect, ranged from 96.6% to 99.4% and 95.3% to 101.4%, respectively. Propofol standard was quantified to evaluate possible loss due to the concentration processes, nitrogen gas and centrifugal vacuum. These two concentration processes resulted in notable decrease in the quantity of propofol, signifying avoiding any concentration processes during propofol quantification. Also, to confirm suitability of the developed method, authentic human plasma samples were analyzed. The selective assay method using MCX cartridge and GC-MS facilitated quantification of propofol in plasma sample accurately by preventing any losses due to the concentration processes.

摘要

已开发并验证了一种用于测定人血浆中丙泊酚的气相色谱 - 质谱(GC-MS)方法。使用混合模式阳离子交换/反相(MCX)柱从人血浆中提取丙泊酚。由于丙泊酚在浓缩过程中容易挥发,将100%甲醇直接注入GC-MS以洗脱丙泊酚。尽管避免了洗脱液的浓缩过程,但丙泊酚的定量下限(LLOQ)为25 ng/mL。验证后的方法具有良好的线性(R (2) = 0.9989),准确度和精密度分别为-5.8%11.7%和3.7%11.6%。其他验证参数,回收率和基质效应,分别为96.6%至99.4%和95.3%至101.4%。对丙泊酚标准品进行定量以评估浓缩过程、氮气和离心真空可能导致的损失。这两个浓缩过程导致丙泊酚量显著减少,这意味着在丙泊酚定量过程中应避免任何浓缩过程。此外,为了确认所开发方法的适用性,对真实的人血浆样本进行了分析。使用MCX柱和GC-MS的选择性测定方法通过防止浓缩过程导致的任何损失,促进了血浆样本中丙泊酚的准确定量。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/fc17/4997078/10d41927fc73/JAMC2016-9531769.001.jpg

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