Giebułtowicz Joanna, Kojro Grzegorz, Piotrowski Roman, Kułakowski Piotr, Wroczyński Piotr
Department of Bioanalysis and Drugs Analysis, Faculty of Pharmacy, Medical University of Warsaw, 1 Banacha Street, 02-097 Warsaw, Poland.
Department of Bioanalysis and Drugs Analysis, Faculty of Pharmacy, Medical University of Warsaw, 1 Banacha Street, 02-097 Warsaw, Poland; Valeant sp. z o.o. sp. j., 15 Przemysłowa 2 Street, 35-959 Rzeszow, Poland.
J Pharm Biomed Anal. 2016 Sep 5;128:294-301. doi: 10.1016/j.jpba.2016.05.042. Epub 2016 May 24.
Cloud-point extraction (CPE) is attracting increasing interest in a number of analytical fields, including bioanalysis, as it provides a simple, safe and environmentally-friendly sample preparation technique. However, there are only few reports on the application of this extraction technique in liquid chromatography-electrospray ionization-tandem mass spectrometry (LC-ESI-MS/MS) analysis. In this study, CPE was used for the isolation of antazoline from human plasma. To date, only one method of antazoline isolation from plasma exists-liquid-liquid extraction (LLE). The aim of this study was to prove the compatibility of CPE and LC-ESI-MS/MS and the applicability of CPE to the determination of antazoline in spiked human plasma and clinical samples. Antazoline was isolated from human plasma using Triton X-114 as a surfactant. Xylometazoline was used as an internal standard. NaOH concentration, temperature and Triton X-114 concentration were optimized. The absolute matrix effect was carefully investigated. All validation experiments met international acceptance criteria and no significant relative matrix effect was observed. The compatibility of CPE and LC-ESI-MS/MS was confirmed using clinical plasma samples. The determination of antazoline concentration in human plasma in the range 10-2500ngmL(-1) by the CPE method led to results which are equivalent to those obtained by the widely used liquid-liquid extraction method.
浊点萃取（CPE）在包括生物分析在内的许多分析领域正吸引着越来越多的关注，因为它提供了一种简单、安全且环保的样品前处理技术。然而，关于这种萃取技术在液相色谱 - 电喷雾电离 - 串联质谱（LC - ESI - MS/MS）分析中的应用报道却很少。在本研究中，CPE被用于从人血浆中分离安他唑啉。迄今为止，从血浆中分离安他唑啉只有一种方法——液液萃取（LLE）。本研究的目的是证明CPE与LC - ESI - MS/MS的兼容性以及CPE在加标人血浆和临床样品中测定安他唑啉的适用性。使用Triton X - 114作为表面活性剂从人血浆中分离安他唑啉。赛洛唑啉用作内标。对氢氧化钠浓度、温度和Triton X - 114浓度进行了优化。仔细研究了绝对基质效应。所有验证实验均符合国际认可标准，未观察到明显的相对基质效应。使用临床血浆样品证实了CPE与LC - ESI - MS/MS的兼容性。采用CPE法测定人血浆中安他唑啉浓度在10 - 2500ng/mL范围内，其结果与广泛使用的液液萃取法所得结果相当。
