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一种混合深共晶溶剂的空气辅助液-液微萃取方法,用于在 HPLC-MS/MS 分析前从呼出冷凝物样品中提取表面活性剂。

A mixed deep eutectic solvents-based air-assisted liquid-liquid microextraction of surfactants from exhaled breath condensate samples prior to HPLC-MS/MS analysis.

机构信息

Tuberculosis and Lung Diseases Research Center, Tabriz University of Medical Sciences, Tabriz, Iran; Department of Anesthesiology and Intensive Care, Faculty of Medicine, Tabriz University of Medical Sciences, Tabriz, Iran.

Pharmaceutical Analysis Research Center and Faculty of Pharmacy, Tabriz University of Medical Sciences, Tabriz, Iran; Faculty of Pharmacy, Near East University, PO BOX: 99138, Nicosia, North Cyprus, Mersin 10, Turkey.

出版信息

J Chromatogr B Analyt Technol Biomed Life Sci. 2022 Jul 15;1204:123289. doi: 10.1016/j.jchromb.2022.123289. Epub 2022 May 12.

Abstract

A ternary solvent system-based air-assisted liquid-liquid microextraction procedure was developed for the extraction of three surfactants from exhaled breath condensate samples prior to their determination by high performance liquid chromatography-tandem mass spectrometry. In this approach, different deep eutectic solvents were synthesized based on phosphocholine chloride and fatty acids and their mixtures were used as the extraction solvents to effective extraction of the analytes. To obtain the optimum composition of the extraction solvents, a simplex centroid design approach was used. Then the effective parameters were studied by response surface methodology using central composite design. The obtained data after optimization showed that 6 times was the best extraction time for the developed procedure. When the sample solution pH was adjusted at 3.7, the method reached to higher extraction efficiency which can be related to the fact that the analytes were in the protonated forms. Increasing the sample solution temperature up to 50 °C enhanced the migration rate of the analytes into the extraction solvent and the method efficacy was increased. Also addition of sodium chloride at 2.8% (w/v) had a positive effect on the method efficiency which can be related to decreasing the analytes solubility in the sample solution. Under optimal conditions, the method showed satisfactory coefficient of determination (≥0.9979), low limit of detection (0.12-0.23 ng mL) and quantification (0.39-0.76 ng mL), acceptable repeatability in deionized water (relative standard deviation ≤ 8.2%) and in exhaled breath condensate (relative standard deviation ≤ 7.2%), and acceptable extraction recovery (75-86%) and enrichment factor (71-86). Considering these results, the developed method provided a quick and efficient way to determine surfactants in the exhaled breath condensate collected from expiratory circuit of the mechanical ventilator. It can be used in drug monitoring and clinical studies.

摘要

建立了一种基于三元溶剂体系的空气辅助液-液微萃取方法,用于在高效液相色谱-串联质谱法测定呼出冷凝物样品中的三种表面活性剂之前对其进行萃取。在这种方法中,根据磷酰胆碱氯化物和脂肪酸合成了不同的深共晶溶剂,并将其混合物用作萃取溶剂,以有效萃取分析物。为了获得萃取溶剂的最佳组成,使用单纯形质心法设计方法。然后使用中心复合设计的响应面法研究有效参数。优化后获得的数据表明,对于所开发的方法,6 倍是最佳萃取时间。当将样品溶液 pH 值调节至 3.7 时,该方法达到了更高的萃取效率,这可以归因于分析物处于质子化形式。将样品溶液温度升高至 50°C 会增强分析物进入萃取溶剂的迁移率,从而提高方法效率。此外,添加 2.8%(w/v)的氯化钠对方法效率也有积极影响,这可以归因于降低了分析物在样品溶液中的溶解度。在最佳条件下,该方法表现出令人满意的决定系数(≥0.9979)、低检测限(0.12-0.23ngmL)和定量限(0.39-0.76ngmL)、在去离子水(相对标准偏差≤8.2%)和呼出冷凝物(相对标准偏差≤7.2%)中的可接受重复性以及可接受的萃取回收率(75-86%)和富集因子(71-86%)。考虑到这些结果,所开发的方法为从机械通气器的呼气回路中收集的呼出冷凝物中快速有效地测定表面活性剂提供了一种方法。它可用于药物监测和临床研究。

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