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Facile derivatization of ultratrace carboxylic acids in saliva for quantification by HPLC–MS/MS
Analytical and Bioanalytical Chemistry ( IF 3.8 ) Pub Date : 2018-05-11 , DOI: 10.1007/s00216-018-1078-7
Chao Guo , Dongmei Li , Cuimei Liu , Zhenpeng Guo , Yi Chen

It remains an issue to directly quantify trace biologically important carboxyl compounds in body fluids. Herein we propose an innovative method to determine α-lipoic acid, 2-(β-carboxyethyl)-6-hydroxy-2,7,8-trimethylchroman, prostaglandin E2, cholic acid, and chenodeoxycholic acid in saliva. The method consists of two successive steps: fast and direct labeling of the target analytes with N-(3-dimethylaminopropyl)-N′-ethylcarbodiimide followed by ultrahigh-performance liquid chromatography–tandem mass spectrometry analysis. The method exhibited a wide linear range from 2.5 to 2500 pg/mL, with linear coefficients greater than 0.9963 and limits of detection and quantification as low as 0.10 and 0.33 pg/mL, respectively. The method precision was evaluated, with relative standard deviations ranging from 2.12% to 10.63% for intraday assays and from 2.98% to 12.88% for interday assays. The recoveries were measured by our spiking saliva samples with standards at three different levels, and ranged from 72.5% to 98.0%. Real applicability was validated by direct quantification of trace target analytes in human saliva, with simple pretreatment, use of a small sample volume, and a short analysis time.

Open image in new windowGraphical abstract
Graphical abstract

Sequential steps to extract, label, and determine the ultratrace carboxylic acids in saliva. CDCA chenodeoxycholic acid, γ-CEHC 2-(β-carboxyethyl)-6-hydroxy-2,7,8-trimethylchroman, α-LA α-lipoic acid, PGE2 prostaglandin E2, UHPLC-MS/MS ultrahigh-performance liquid chromatography–tandem mass spectrometry



中文翻译:

唾液中超痕量羧酸的便捷衍生化,通过HPLC-MS / MS进行定量

直接定量体液中的痕量生物学上重要的羧基化合物仍然是一个问题。在本文中,我们提出了一种创新的方法来测定唾液中的α-硫辛酸,2-(β-羧乙基)-6-羟基-2,7,8-三甲基苯并二氢吡喃,前列腺素E 2,胆酸和鹅去氧胆酸。该方法包括两个连续步骤:用N-(3-二甲基氨基丙基)-N快速和直接标记目标分析物'-乙基碳二亚胺,然后进行超高效液相色谱-串联质谱分析。该方法的线性范围从2.5到2500 pg / mL,线性系数大于0.9963,检出限和定量限分别低至0.10 pg / mL和0.33 pg / mL。评估了方法的精确度,日内测定的相对标准偏差为2.12%至10.63%,日间测定的相对标准偏差为2.98%至12.88%。回收率是通过将唾液样品加标为三种不同水平的标准来测量的,范围从72.5%到98.0%。通过直接定量人类唾液中的痕量目标分析物,简单的预处理,使用少量的样品以及较短的分析时间,验证了其实际适用性。

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图形概要

提取,标记和确定唾液中超痕量羧酸的顺序步骤。CDCA鹅去氧胆酸,γ-CEHC2-(β-羧乙基)-6-羟基-2,7,8-三甲基苯并二氢吡喃,α-LAα-硫辛酸,PGE 2前列腺素E 2,UHPLC-MS / MS超高性能液体色谱-串联质谱

更新日期:2018-05-11
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