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Headspace Solid-Phase Microextraction Coupled with Gas Chromatography–Mass Spectrometry for the Determination of Volatile Organic Compounds in Urine
Journal of Analytical Chemistry ( IF 1.0 ) Pub Date : 2020-06-30 , DOI: 10.1134/s1061934820060088
Natalia Drabińska , Małgorzata Starowicz , Urszula Krupa-Kozak

Abstract

Determination of volatile organic compounds (VOCs), the metabolites produced in human body, contributes to better understanding of the mechanisms responsible for the progression of diseases and facilitates monitoring of the responses to treatment. Urine samples are a rich source of VOCs and they constitute a non-invasive tool for diagnosis of various metabolic and pathological states. The aim of this study was to optimize the headspace solid-phase microextraction coupled with gas chromatography−mass spectrometry (HS-SPME−GC/MS) method for analysis of urine samples on the example of urine collected from children with celiac disease. Pooled urine samples from three children with celiac disease were used to select the optimal fibers, time and temperature of extraction, salt dose, and pH to achieve the highest SPME efficiency. Analysis performed with the use of divinylbenzene/carboxen/polydimethylsiloxane fiber in acidic pH with the addition of 1.5 g of sodium chloride supported the extraction of the highest number of VOCs with the largest total peak area. The extraction conducted at 60°C for 45 min led to an optimal improvement in efficiency with a reduced number of siloxane derivatives, indicative of degradation of septa, fiber, and/or GC column stationary phase. The optimized HS-SPME−GC/MS method can be successfully applied to the determination of VOCs in urine samples.


中文翻译:

顶空固相微萃取-气相色谱-质谱法测定尿液中的挥发性有机物

摘要

挥发性有机化合物(VOCs)的测定,是人体产生的代谢产物,有助于更好地理解导致疾病进展的机制,并有助于监测对治疗的反应。尿液样本是挥发性有机化合物的丰富来源,它们构成了诊断各种代谢和病理状态的非侵入性工具。这项研究的目的是优化顶空固相微萃取结合气相色谱-质谱法(HS-SPME-GC / MS)以从腹腔疾病患儿收集的尿液为例分析尿液样本的方法。使用来自三个乳糜泻患儿的合并尿液样本来选择最佳纤维,提取时间和温度,盐剂量和pH值,以实现最高的SPME效率。在酸性pH下使用二乙烯基苯/羧甲基/聚二甲基硅氧烷纤维进行的分析以及加入1.5 g氯化钠的过程中,提取的VOC数量最多,总峰面积最大。在60°C下进行45分钟的萃取可导致效率得到最佳的提高,同时减少了硅氧烷衍生物的数量,表明隔垫,纤维和/或GC色谱柱固定相的降解。优化的HS-SPME-GC / MS方法可以成功地用于尿样中VOC的测定。
更新日期:2020-06-30
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