Structural elucidation of 3-nitrophenylhydrazine derivatives of tricarboxylic acid cycle acids and optimization of their fragmentation to boost sensitivity in liquid chromatography-mass spectrometry

Hodek, Ondřej; Henderson, John M.; Argemi-Muntadas, Lidia; Khan, Anzar; Moritz, Thomas

doi:10.1016/j.jchromb.2023.123719

Cited by 10 publications

(3 citation statements)

References 34 publications

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“…As already investigated by Hodek and co-workers [ 20 ], dicarboxylic acids were mainly derivatized on both carboxylic acid groups. The most intense precursor ion in MS/MS analysis was the doubly derivatized and singly charged ion.…”

Section: Resultsmentioning

confidence: 99%

“…Especially high signals in blanks originated from lactic acid. Hodek and co-workers [ 20 ] also detected lactic acid in 3-NPH-derivatized blanks and assumed that it was present already in laboratory equipment or in solvents or reagents used for derivatization. After derivatization with aniline, also medium- and long-chain fatty acids showed carryover with signal intensity tending to increase with increasing chain length.…”

Section: Resultsmentioning

confidence: 99%

“…In contrast, derivatization with 3-NPH passed all validation experiments and quantification results matched those obtained by AIC-HR-MS. In addition, 3-NHP has been successfully used for derivatization of CAs in other studies [ 17 , 20 ]. Consequently, of the two approaches tested, derivatization with 3-NPH is preferable for metabolome profiling.…”

Section: Resultsmentioning

confidence: 99%

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Comparison of LC-MS-based methods for the determination of carboxylic acids in animal matrices

Schwartz-Zimmermann,

Hündler,

Reiterer

et al. 2024

Anal Bioanal Chem

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Carboxylic acids (CAs) are key players in human and animal metabolism. As they are hardly retained under reversed-phase liquid chromatography (RP-LC) conditions in their native form, derivatization is an option to make them accessible to RP-LC and simultaneously increase their response for mass spectrometric detection. In this work, two RP-LC tandem mass spectrometry-based methods using aniline or 3-nitrophenylhydrazine (3-NPH) as derivatization agents were compared with respect to several factors including completeness of derivatization, apparent recoveries (RAs) in both cow feces and ruminal fluid, and concentrations obtained in feces and ruminal fluid of cows. Anion exchange chromatography coupled to high-resolution mass spectrometry (AIC-HR-MS) served as reference method. Derivatization efficiencies were close to 100% for 3-NPH derivatization but variable (20–100%) and different in solvent solutions and matrix extracts for aniline derivatization. Likewise, average RAs of 13C-labeled short-chain fatty acids as internal standards were around 100% for 3-NPH derivatization but only 45% for aniline derivatization. Quantification of CAs in feces and ruminal fluid of cows initially fed a forage-only diet and then transitioned to a 65% high-grain diet which yielded similar concentrations for 3-NPH derivatization and AIC-HR-MS, but concentrations determined by aniline derivatization were on average five times lower. For these reasons, derivatization with aniline is not recommended for the quantitative analysis of CAs in animal samples. Graphical abstract

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Section: Resultsmentioning

confidence: 99%

Section: Resultsmentioning

confidence: 99%

Section: Resultsmentioning

confidence: 99%

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Comparison of LC-MS-based methods for the determination of carboxylic acids in animal matrices

Schwartz-Zimmermann,

Hündler,

Reiterer

et al. 2024

Anal Bioanal Chem

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Sensing of Liver‐Derived Nicotinamide by Intestinal Group 2 Innate Lymphoid Cells Links Liver Cirrhosis and Ulcerative Colitis Susceptibility

Shen,

Li,

Liu

et al. 2024

Advanced Science

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The correlation between liver disease and the progression of ulcerative colitis (UC) has remained elusive. In this study, it demonstrates that liver injury is intricately linked to the heightened severity of UC in patients, and causes more profound intestinal damage during DSS‐induced colitis in mice. Metabolomics analysis of plasma from liver cirrhosis patients shows liver injury compromising nicotinamide supply for NAD+ biosynthesis in the intestine. Subsequent investigation identifies intestinal group 2 innate lymphoid cells (ILC2s) are responsible for liver injury‐exacerbated colitis. Reconstitution of ILC2s or the restoration of NAD+ metabolism proves effective in relieving liver injury‐aggravated experimental colitis. Mechanistically, the NAD+ salvage pathway regulates gut ILC2s in a cell‐intrinsic manner by supporting the generation of succinate, which fuels the electron transport chain to sustaining ILC2s function. This research deepens the understanding of cellular and molecular mechanisms in liver disease‐UC interplay, identifying a metabolic target for innovative treatments in liver injury‐complicated colitis.

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Determination of trace chelating carboxylic acids in rice by green extraction combined with liquid chromatography–mass spectrometry analysis and its application in the evaluation of old and new rice

Kang,

Wang,

Feng

et al. 2024

Rapid Comm Mass Spectrometry

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RationaleAccurate identification of old rice samples from new ones benefits their market circulation and consumers. However, the current detection methods are still not satisfactory because of their insufficient accuracy or (and) time‐consuming process.MethodsChelating carboxylic acids (CCAs) were selectively extracted from rice, by stirring with chelating resin and a dilute Na2CO3 solution. The green analytical chemistry guidelines for sample preparation were investigated by using the green chemistry calculator AGREE prep. The extractant was determined by liquid chromatography–mass spectrometry (LC/MS), and statistical analysis of the analytical data was carried out to evaluate the significance of the difference by ChiPlot.ResultsThe limit of quantitation for the CCAs is in the range of 1 to 50 ng/mL, with a reasonable reproducibility. The CCAs in 23 rice samples were determined within a wide concentration range from 0.03 to 1174 μg/g. Intriguingly, the content of citric acid, malonic acid, α‐ketoglutaric acid and cis‐aconite acid in new rice was each found to be distinctively higher than that in old rice by several times. Even mixtures of old and new rice were found to show much difference in the concentration of citric acid and malic acid.ConclusionA green analytical method has been developed for the simultaneous determination of CCAs by LC/MS analysis, and the identification of old rice samples from new ones was easily carried out according to their CCA content for the first time. The results indicated that the described method has powerful potential for the accurate identification of old rice samples from new ones.

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Structural elucidation of 3-nitrophenylhydrazine derivatives of tricarboxylic acid cycle acids and optimization of their fragmentation to boost sensitivity in liquid chromatography-mass spectrometry

Cited by 10 publications

References 34 publications

Comparison of LC-MS-based methods for the determination of carboxylic acids in animal matrices

Comparison of LC-MS-based methods for the determination of carboxylic acids in animal matrices

Sensing of Liver‐Derived Nicotinamide by Intestinal Group 2 Innate Lymphoid Cells Links Liver Cirrhosis and Ulcerative Colitis Susceptibility

Determination of trace chelating carboxylic acids in rice by green extraction combined with liquid chromatography–mass spectrometry analysis and its application in the evaluation of old and new rice

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