Fast methodology for the reliable determination of nonylphenol in water samples by minimal labeling isotope dilution mass spectrometry

Fabregat-Cabello, Neus; Castillo, Ángel; Sancho, Juan V.; González, F.; Roig-Navarro, A.F.

doi:10.1016/j.chroma.2013.05.033

Cited by 19 publications

(18 citation statements)

References 24 publications

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“…18,19 It has also been reported that data obtained through the use of the “minimal labeling approach” require corrections by an isotope pattern deconvolution algorithm. 16,17 On the other hand, the limited availability and/or high price of other than d -labeled analogues may be a practical hurdle that prevents their widespread applications.…”

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confidence: 99%

Application of Screening Experimental Designs to Assess Chromatographic Isotope Effect upon Isotope-Coded Derivatization for Quantitative Liquid Chromatography–Mass Spectrometry

2014

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Isotope effect may cause partial chromatographic separation of labeled (heavy) and unlabeled (light) isotopologue pairs. Together with a simultaneous matrix effect, this could lead to unacceptable accuracy in quantitative liquid chromatography–mass spectrometry assays, especially when electrospray ionization is used. Four biologically relevant reactive aldehydes (acrolein, malondialdehyde, 4-hydroxy-2-nonenal, and 4-oxo-2-nonenal) were derivatized with light or heavy (d3-, 13C6-, 15N2-, or 15N4-labeled) 2,4-dinitrophenylhydrazine and used as model compounds to evaluate chromatographic isotope effects. For comprehensive assessment of retention time differences between light/heavy pairs under various gradient reversed-phase liquid chromatography conditions, major chromatographic parameters (stationary phase, mobile phase pH, temperature, organic solvent, and gradient slope) and different isotope labelings were addressed by multiple-factor screening using experimental designs that included both asymmetrical (Addelman) and Plackett–Burman schemes followed by statistical evaluations. Results confirmed that the most effective approach to avoid chromatographic isotope effect is the use of 15N or 13C labeling instead of deuterium labeling, while chromatographic parameters had no general influence. Comparison of the alternate isotope-coded derivatization assay (AIDA) using deuterium versus 15N labeling gave unacceptable differences (>15%) upon quantifying some of the model aldehydes from biological matrixes. On the basis of our results, we recommend the modification of the AIDA protocol by replacing d3-2,4-dinitrophenylhydrazine with 15N- or 13C-labeled derivatizing reagent to avoid possible unfavorable consequences of chromatographic isotope effects.

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confidence: 99%

Application of Screening Experimental Designs to Assess Chromatographic Isotope Effect upon Isotope-Coded Derivatization for Quantitative Liquid Chromatography–Mass Spectrometry

2014

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“…Therefore, isocratic conditions were also tested. Based on our previous work 18,23 different percentages of methanol-water combinations, with and without ammonia and ammonium acetate as modiers, were evaluated. The best sensitivity was reached with a mobile phase consisting of 97% methanol-water with 0.01% ammonia since the presence of NH 4 Ac negatively affected the signal of BPA.…”

Section: Resultsmentioning

confidence: 99%

“…The ubiquitous presence of the selected compounds in all the laboratory material, included solvents, is probably the main challenge during the determination of EDCs at very low concentration levels. For this reason, and according to our previous experience, 18,23 all of the glass material was rinsed with acetone, methanol and hexane. Compared with previous work, rinsing with hexane was also added to the cleaning procedure due to some contamination observed aer rinsing only with the other two solvents.…”

Section: Cleaning Proceduresmentioning

confidence: 99%

Method development and validation for the determination of selected endocrine disrupting compounds by liquid chromatography mass spectrometry and isotope pattern deconvolution in water samples. Comparison of two extraction techniques

et al. 2016

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“…Finally, the experimentally measured isotope distributions for the labelled compound were compared with the 100 convoluted distributions by linear regression analysis . Then, the ‘right’ isotope enrichment was selected as to that giving the minimum in the square sum of residuals (SSR) between the calculated and observed distributions.…”

Section: Methodsmentioning

confidence: 99%

Determination of the enrichment of isotopically labelled molecules by mass spectrometry

2014

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A general method for the determination of the enrichment of isotopically labelled molecules by mass spectrometry (MS) is described. In contrast to other published procedures, the method described here takes into account and corrects for measurement errors such as the contribution at M - 1 due to loss of hydrogen or lack of spectral resolution and provides an uncertainty value for the determined enrichment. The general procedure requires the following steps: (1) evaluation of linearity in the mass spectrometer by injecting the natural abundance compound at different concentration levels, (2) determination of the purity of the mass cluster using the natural abundance analogue, (3) calculation of the theoretical isotope composition of the labelled compound using different tentative isotope enrichments, (4) calculation of 'convoluted' isotope distributions for the labelled compound taking into account the purity of the mass cluster determined with the natural abundance analogue and (5) comparison of the isotope distributions measured for the labelled compound with those calculated for different isotope enrichments using linear regression. The method was applied to a series of commercially available (13)C- and (2)H-labelled compounds and to a suite of singly (13)C-labelled β2-agonist prepared in-house both by gas chromatography (GC)-MS, GC-tandem MS (MS/MS) and liquid chromatography-MS/MS with satisfactory results. It was observed that the main uncertainty source for the isotope enrichment was the uncertainty in the purity of the measured cluster as determined with the natural abundance compound.

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Fast methodology for the reliable determination of nonylphenol in water samples by minimal labeling isotope dilution mass spectrometry

Abstract: "B H<=G

Cited by 19 publications

References 24 publications

Application of Screening Experimental Designs to Assess Chromatographic Isotope Effect upon Isotope-Coded Derivatization for Quantitative Liquid Chromatography–Mass Spectrometry

Application of Screening Experimental Designs to Assess Chromatographic Isotope Effect upon Isotope-Coded Derivatization for Quantitative Liquid Chromatography–Mass Spectrometry

Method development and validation for the determination of selected endocrine disrupting compounds by liquid chromatography mass spectrometry and isotope pattern deconvolution in water samples. Comparison of two extraction techniques

Determination of the enrichment of isotopically labelled molecules by mass spectrometry

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