Selective Solid Phase Extraction Using a Mixed-Mode Cation Exchange Cartridge Facilitates the Mass Spectrometry Analysis on Dissolved Organic Nitrogen

IF 1.8 3区化学 Q4 BIOCHEMICAL RESEARCH METHODS

Rapid Communications in Mass Spectrometry Pub Date : 2025-04-09 DOI:10.1002/rcm.10037

Yuanyuan Dong, Wenrui Yao, Yulin Qi, Yufu Han, Chao Ma, Dietrich A. Volmer

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引用次数: 0

Abstract

Rationale

Dissolved organic nitrogen (DON) is a crucial component in environment, which acts as the largest reservoir of nitrogen and plays a significant role in the nitrogen cycling, pollutant transport, and substrate utilization among various environmental systems. DON exhibits a relatively low concentration in environment, which presents a great challenge for DON detection, and an efficient separation and enrichment lab protocol is required to fully understand its structural and compositional characteristics. However, there is no standard method to extract DON from complex environmental samples efficiently.

Methods

The DON was extracted utilizing solid-phase extraction (SPE), with a one-step elution by the Bond Elut PPL cartridge and the Waters HLB cartridge, and a three-step elution by the Waters MCX cartridge. UV-Vis, fluorescence, mass spectrometry (MS), and gas chromatography-nitrogen chemiluminescence detector (GC-NCD) techniques were utilized to investigate and compare the characteristics of DON from the three different SPE strategies.

Results

Combined the fluorescence and MS results, it is found that the stepwise extraction using the MCX cartridge exhibits the best recovery of DON for both standard and environmental samples, and its performance is less affected by the chemical interferences such as surfactants during MS analysis. Furthermore, the MCX fraction exhibits the highest number of DON molecular formulas with a low O/C ratio and a high H/C ratio in environmental samples, and such a fraction also shows an enrichment of nitrosamine-type substances.

Conclusions

This work establishes an efficient MCX-SPE protocol to extract and analyze DON, which can be applied to environmental samples straightforward. The presented work provides a theoretical support for the analysis of DON, which facilitates a comprehensive understanding of the chemical composition and environmental effect of nitrogen-containing substances.

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选择性固相萃取使用混合模式阳离子交换筒有利于溶解有机氮的质谱分析

溶解有机氮（DON）是环境中的重要组成部分，是最大的氮库，在各种环境系统的氮循环、污染物运输和底物利用中起着重要作用。环境中DON的浓度相对较低，这给DON的检测带来了很大的挑战，需要一个高效的分离富集实验室方案来充分了解其结构和组成特征。然而，目前还没有标准的方法可以有效地从复杂的环境样品中提取DON。方法采用固相萃取法（SPE）提取DON， Bond Elut PPL和Waters HLB分别洗脱一步，Waters MCX洗脱三步。利用UV-Vis、荧光、质谱（MS）、气相色谱-氮化学发光检测器（GC-NCD）等技术对三种不同SPE策略下DON的特性进行了研究和比较。结果结合荧光和质谱分析结果，发现MCX分步萃取法对标准样品和环境样品的DON回收率最高，且在质谱分析过程中受表面活性剂等化学干扰的影响较小。此外，MCX馏分在环境样品中表现出最多的低O/C比和高H/C比的DON分子式，并且该馏分还表现出亚硝胺类物质的富集。结论建立了一种高效的MCX-SPE分离分析DON的方法，可直接应用于环境样品中。本研究为DON的分析提供了理论支持，有助于全面了解含氮物质的化学组成和环境效应。

本文章由计算机程序翻译，如有差异，请以英文原文为准。

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来源期刊

Rapid Communications in Mass Spectrometry 化学-分析化学

CiteScore

4.10

自引率

5.00%

发文量

219

审稿时长

2.6 months

期刊介绍： Rapid Communications in Mass Spectrometry is a journal whose aim is the rapid publication of original research results and ideas on all aspects of the science of gas-phase ions; it covers all the associated scientific disciplines. There is no formal limit on paper length ("rapid" is not synonymous with "brief"), but papers should be of a length that is commensurate with the importance and complexity of the results being reported. Contributions may be theoretical or practical in nature; they may deal with methods, techniques and applications, or with the interpretation of results; they may cover any area in science that depends directly on measurements made upon gaseous ions or that is associated with such measurements.