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dansylation
Canadian Journal of Chemistry · 2024 ·Vol. 102 ·期 9 · IF 1.1

Profiling organic pollutants in environmental water by dansylation-based non-targeted liquid chromatography-high resolution mass spectrometry analysis

Bin Chen,Lirong An,Feng Li,Yanan Tang

Monitoring organic pollutants in rainwater is important to understand relations between air pollutants and water safety. Non-targeted liquid chromatography–mass spectrometry (LC–MS) is a powerful tool but because of big differences of pollutants in polarity, ionization efficiency, and low concentrations, it is challenging to detect all pollutants in a single analysis. Chemical derivatization is a widely adapted strategy to fractionate complex samples with enhanced sensitivity and selectivity. Herein, we propose the usage of dansylation as a chemical derivatization method to improve both LC retention and MS ionization of organic pollutants containing amine, hydroxyl, and carboxyl for non-targeted LC–MS analysis. We first evaluated the labeling coverage of dansylation to organic pollutants in water matrix. Using dansyl chloride (DnsCl) and dansyl hydrazine (DnsHz) to label 100 amine- and hydroxyl-containing compounds and 100 carboxyl compounds, respectively, we found DnsCl and DnsHz had over 60% labeling coverage for 8 categories of compounds. Then dansylation was applied to label the rainwater, source water, disinfected rainwater, and drinking water samples. To facilitate the annotation of dansylated compounds, we also established a web-based tool termed DansylFinder. Using DansylFinder, 3889, 5813, 6077, and 4050 tentative annotations were found in rainwater, source water, disinfected rainwater, and drinking water samples by dansylation-based non-targeted LC-HRMS analysis. Four hundred fifty four were persistently detected in all water samples, suggesting significant organic overlaps of the four water samples. In addition, two degradation pathways reported in drinking water disinfection process were also detected in disinfected rainwater, suggesting rainwater is a potential path for air pollutants to infiltrate drinking water system.

研究领域: 环境科学 · 分析化学
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ANALYTICAL LETTERS · 2014 · IF 1.019

Determination of Biogenic Amines in Digesta by High Performance Liquid Chromatography with Precolumn Dansylation

Yu-Xiang Yang,Chun-Long Mu,Jing-Fei Zhang,Wei-Yun Zhu

A rapid high-performance liquid chromatographic method for the determination of nine biogenic amines in digesta sample from pig cecum and colon was developed using a simple direct derivatization with dansyl chloride. After precipitation with trichloroacetic acid and extraction by n-hexane, the amines were separated on a C18 column using a water–acetonitrile gradient elution program. The calibration curve for each amine was linear over the range of 50 to 250 µmol/L, and the relative standard deviation for intra-assay precision was below 0.5%. The recovery ranged from 86.79% to 117.62% while the limit of detection was 0.1 µmol/L for the amines except for spermine with a value of 0.03 µmol/L. This procedure was successfully applied to identify and quantify biogenic amines in the hindgut digesta of the pig.

研究领域: 分析化学 · 动物营养学
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TALANTA · 2020 · IF 5.339

Determination of estrogens by solid-phase quadruplex stable isotope dansylation coupled with liquid chromatography-high resolution mass spectrometry in environmental samples

Minghuo Wu,Enming Miao,Wenxue Xu,Weiping Xu,Yufeng Hu,Jingjing Zhan,Hao Zhou

Estrogens distribute widely in the environment as endocrine-disrupting chemicals (EDCs), which have to be monitored to evaluate their environmental impact. Aim to improve the analytical throughput of liquid chromatography-high resolution mass spectrometry (LC-HRMS), a quadruplex stable isotope dansylation method was developed, with which three real samples could be quantitatively analyzed in one injection. As the estrogens were at trace level in complex matrices, magnetic solid-phase extraction (MSPE) was applied to enrich these analytes and remove the interfaces. By integrating MSPE and quadruplex stable isotope dansylation, a solid-phase quadruplex labeling method was developed for the LC-HRMS analysis of estrogen analogues . For the tested seven estrogens, the developed method showed low detection limits (0.1–0.5 ng/L for pond water and 0.01–0.05 μg/kg for poultry manure), good precision (RSD < 5.5%) and accuracy (96.8–108.3%). The method was applied in the determination of estrogens in environmental samples, and the results revealed that all the tested estrogens were present in the estuary water (unquantifiable to 71.2 ng/L) and chicken manure (undetectable to 25.43 μg/kg).

研究领域: 环境科学 · 分析化学 · 环境监测
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Analytical Methods · 2021 ·Vol. 13 ·期 11 ·1404-1411 · IF 2.896

Determination of phenolic compounds in estuary water and sediment by solid-phase isotope dansylation coupled with liquid chromatography-high resolution mass spectrometry

Wenxue Xu,Yufeng Hu,Minghuo Wu,Enming Miao,Hao Zhou,Xuwang Zhang,Jingjing Zhan

A method consisting of solid-phase isotope dansylation (derivatization with dansyl chloride) and liquid chromatography-high resolution mass spectrometry (LC-HRMS) was developed for the quantitative analysis of phenolic compounds (phenols) in environmental samples. A magnetic-HLB (hydrophilic lipophilic balanced) material was synthesized and applied as an adsorbent in magnetic solid-phase extraction (MSPE) for the enrichment of the analytical targets. Furthermore, with the solid-phase isotope labeling, the desalting and removal of labeling residuals could be simplified over conventional in-solution labeling. In addition to overcoming the matrix effect by isotope dansylation, the sensitivity for the analysis of phenols by LC-HRMS was remarkably improved by over 100-fold. The method was systematically verified, and good accuracy (86.5–104.9%) and precision (<8.6% and <11.4% for intra- and inter-day, respectively) were achieved for the tested 15 phenols. The limits of detection (LODs) of this method were estimated to be 0.2–5 ng L−1 and 5–100 ng kg−1 in estuary water and sediment samples, respectively. With this method, samples collected from the Daliao River estuary (Panjin, China) were analyzed. It was found that all of the targeted phenols were detected at concentrations ranging from unquantifiable to 485 ng L−1 (the total concentration of analytes found in each sample were in the range 822–957 ng L−1) and unquantifiable to 1368 ng kg−1 (the total concentration of analytes found in each sample were in the range 2251–2992 ng kg−1) in water and sediment, respectively.

研究领域: 环境科学 · 分析化学 · 水质 · 环境监测
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FOOD CONTROL · 2022 · IF 6.652

Analytical method for histamine, urocanic acid isomers, and their precursor histidine in fish sauce based on precolumn dansylation and high-performance liquid chromatography

Jian-Jun Zhong,Liping Xia,Liuru Xue,Boyu Liu,Lingling Zhao,Hua Ye,Zhanming Li

Histamine food poisoning (HFP) or scombrotoxic fish poisoning is a major public health concern associated with seafood and seafood products containing copious amounts of free histidine , which may be decarboxylated into scombrotoxic histamine, the main culprit of HFP. Moreover, the deamination product of the histidine, trans -urocanic acid, is assumed to be scombrotoxic by degranulating mast cells to release endogenous histamine after isomerizing to the cis -form, as well as known to have immunosuppressive effects. In recognition of the potential health risks associated with the histidine degradatives, this work aimed to provide a method for the simultaneous determination of histidine, histamine, and urocanic acid isomers in food, based on precolumn dansylation and subsequent reversed-phase HPLC analysis. The dansylation conditions were optimized for yield with the design of experiments approach consisted of a center point-enhanced 2 4 factorial design followed by sequential steepest ascent searches. Satisfactory chromatographic separation of fish sauce was achieved within 9 min by retention modeling of both the analytes and potentially interfering peaks. The method was fully validated with limits of detection between 0.004 and 0.017 mg 100 g −1 fish sauce, and successfully applied to several fish sauce samples, in which the histamine and urocanic acid levels were found low and unlikely of concern, with correspondingly low levels of the precursor histidine.

研究领域: 食品科学 · 分析化学 · 公共卫生
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