Solid-phase extraction with strong anion-exchange columns for selective isolation and concentration of urinary organic acids.

Verhaeghe, B. J.; Lefevere, M.F.; Leenheer, A.P. De

doi:10.1093/clinchem/34.6.1077

Cited by 27 publications

(5 citation statements)

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“…Liquidliquid extraction using ethyl acetate or ethyl acetate-diethyl ether is commonly employed for organic acids in acidified urine. Solid phase extraction (anion exchange) techniques have also been employed (Verhaeghe et al, 1988;Chalmers and Lawson, 1982). A more general profile of urine samples (organic acids, amino acids, sugars) has been carried out by the use of urease followed by trimethylsilylation of the residue after drying (Shoemaker and Elliott, 1991).…”

Section: Sample Extractionmentioning

confidence: 99%

Chemical derivatization and mass spectral libraries in metabolic profiling by GC/MS and LC/MS/MS

Halket¹,

Waterman²,

Przyborowska³

et al. 2004

Journal of Experimental Botany

559

306

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An overview is presented of gas chromatography/mass spectrometry (GC/MS) and liquid chromatography/mass spectrometry (LC/MS), the two major hyphenated techniques employed in metabolic profiling that complement direct 'fingerprinting' methods such as atmospheric pressure ionization (API) quadrupole time-of-flight MS, API Fourier transform MS, and NMR. In GC/MS, the analytes are normally derivatized prior to analysis in order to reduce their polarity and facilitate chromatographic separation. The electron ionization mass spectra obtained are reproducible and suitable for library matching, mass spectral collections being readily available. In LC/MS, derivatization and library matching are at an early stage of development and mini-reviews are provided. Chemical derivatization can dramatically increase the sensitivity and specificity of LC/MS methods for less polar compounds and provides additional structural information. The potential of derivatization for metabolic profiling in LC/MS is demonstrated by the enhanced analysis of plant extracts, including the potential to measure volatile acids such as formic acid, difficult to achieve by GC/MS. The important role of mass spectral library creation and usage in these techniques is discussed and illustrated by examples.

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Section: Sample Extractionmentioning

confidence: 99%

Chemical derivatization and mass spectral libraries in metabolic profiling by GC/MS and LC/MS/MS

Halket¹,

Waterman²,

Przyborowska³

et al. 2004

Journal of Experimental Botany

559

306

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“…Mass spectra were measured in electron impact mode at 70 eV on a JEOL DX 303 instrument with DA 5000 data station coupled with Hewlett-Packard 5890 gas chromatograph. Carboxylic acids were isolated from urine using strong anion exchanger columns by a modified procedure of Verhaege et al (29). In brief, 0.5-mL aliquots of pooled urine were mixed with 0.1 mL of 0.01 M barium hydroxide solution to precipitate sulfates and a part of phosphates.…”

Section: Jv-acetyl-s-[2-(butoxycarbonyl)-2-hydroxyethyl]cysteine (2-bhc)mentioning

confidence: 99%

“…Samples were centrifuged at 200g, 0.2 mL of the supernatant was diluted with 0.4 mL of water, and the pH was adjusted to 7.5-8. The resulting solutions were applied to HEMA Q columns activated as described (29). Columns were then washed with 5 mL of doubly distilled water, and excess water was removed by centrifugation (5 min at 200 g), followed by washing with 1 mL of methanol and 1 mL of ethyl acetate.…”

Section: Jv-acetyl-s-[2-(butoxycarbonyl)-2-hydroxyethyl]cysteine (2-bhc)mentioning

confidence: 99%

Metabolic pathways of 1-butyl [3-13C]acrylate. Identification of urinary metabolites in rat using nuclear magnetic resonance and mass spectroscopy

Linhart

Hrabal²,

Šmejkal³

et al. 1994

Chem. Res. Toxicol.

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1-Butylacrylate, an industrial monomer, is rapidly metabolized by carboxylesterase-catalyzed hydrolysis to acrylic acid and 1-butanol. Acrylic acid enters the intermediary metabolism and is efficiently degraded to carbon dioxide as the metabolic end product. To obtain a virtually complete metabolic pattern, rats were dosed by a single intraperitoneal dose of 1 mmol/kg 1-butyl [3-13C]acrylate. The urine was then analyzed by a one-dimensional 1H-detected and two-dimensional 1H-13C shift-correlated heteronuclear multiple-quantum NMR experiment. In this experiment, three urinary metabolites, namely, 3-hydroxypropanoic acid, N-acetyl-S-(2-carboxyethyl)cysteine, and N-acetyl-S-(2-carboxyethyl)cysteine sulfoxide, were identified comparing their 1H and 13C chemical shifts with those of authentic standards. In another experiment, to enhance minor metabolic pathways, rats were dosed with 0.25 mmol/kg of a carboxylesterase inhibitor, tri-o-tolyl phosphate, prior to 0.5 mmol/kg butyl [3-13C]acrylate. Under these conditions, N-acetyl-S-(2-carboxyethyl)cysteine, N-acetyl-S-[2-(butoxycarbonyl)-ethyl]cysteine, and N-acetyl-S-(2-carboxyethyl)cysteine sulfoxide were found in urine. No metabolites which would arise from a possible metabolic activation of 1-butyl acrylate to 1-butyl oxiranecarboxylate and its subsequent hydrolysis or glutathione conjugation were found. It is estimated that any metabolite amounting to more than 1% of the dose should be detected under these conditions. To study the routes by which BA enters the intermediary metabolism, incorporation of the label into urinary carboxylic acids was followed by GC/MS. Significant enrichment was found in 3-hydroxypropanoic acid and citric and isocitric acid but not in lactic acid.(ABSTRACT TRUNCATED AT 250 WORDS)

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“…Solid-phase extractions (SPEs) are widely used in sample preparation and new methods and materials were developed over the last decades [20]. When targeting OAs, anionic exchange sorbents are often chosen [21][22][23]. However, most methods utilizing SPE to gain quantitative data on OAs focus on food and clinical research [23,24].…”

Section: Introductionmentioning

confidence: 99%

Method development and validation for the quantification of organic acids in microbial samples using anionic exchange solid-phase extraction and gas chromatography-mass spectrometry

et al. 2020

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Organic acids play a key role in central metabolic functions of organisms, are crucial for understanding regulatory processes and are ubiquitous inside the cell. Therefore, quantification of these compounds provides a valuable approach for studying dynamics of metabolic processes, in particular when the organism faces changing environmental conditions. However, the extraction and analysis of organic acids can be challenging and validated methods available in this field are limited. In this study, we developed a method for the extraction and quantification of organic acids from microbial samples based on solid-phase extraction on a strong anionic exchange cartridge and gas chromatographic-mass spectrometric analysis. Full method validation was conducted to determine quality parameters of the new method. Recoveries for 12 of the 15 aromatic and aliphatic acids were between 100 and 111% and detection limits between 3 and 272 ng/mL. The ranges for the regression coefficients and process standard deviations for these compound classes were 0.9874–0.9994 and 0.04–0.69 μg/mL, respectively. Limitations were encountered when targeting aliphatic acids with hydroxy, oxo or enol ester functions. Finally, we demonstrated the applicability of the method on cell extracts of the bacterium Escherichia coli and the dinoflagellate Prorocentrum minimum.

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Solid-phase extraction with strong anion-exchange columns for selective isolation and concentration of urinary organic acids.

Cited by 27 publications

References 0 publications

Chemical derivatization and mass spectral libraries in metabolic profiling by GC/MS and LC/MS/MS

Chemical derivatization and mass spectral libraries in metabolic profiling by GC/MS and LC/MS/MS

Metabolic pathways of 1-butyl [3-13C]acrylate. Identification of urinary metabolites in rat using nuclear magnetic resonance and mass spectroscopy

Method development and validation for the quantification of organic acids in microbial samples using anionic exchange solid-phase extraction and gas chromatography-mass spectrometry

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