Determination of chemical purity and isotopic composition of natural and carbon-13-labeled arsenobetaine bromide standards by quantitative1H-NMR

Le, Phuong-Mai; Ding, Jianfu; Leek, Donald M.; Mester, Zoltán; Robertson, Gilles P.; Windust, Anthony; Meija, Juris

doi:10.1007/s00216-016-9827-y

Cited by 11 publications

(8 citation statements)

References 19 publications

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“…The chemical purity of vanillin in VANA-1 and VANB-1 was determined by quantitative 1 H-NMR on a Bruker-NMR 400 spectrometer (Bruker Optics Inc; MA, USA) operating at 400.13 MHz for proton ( 1 H) resonance frequency equipped with a 5 mm ID NMR probe controlled at 298 K, following a method adapted from Le et al [ 26 ]. In brief, three replicate samples of each vanillin sample (15 mg) and maleic acid (8 mg) as an internal calibrator were weighed on an analytical microbalance (UMT-2; Mettler-Toledo) and co-dissolved in 2 mL DMSO- d 6 in a 20-mL vial.…”

Section: Methodsmentioning

confidence: 99%

Site-specific carbon isotope measurements of vanillin reference materials by nuclear magnetic resonance spectrometry

Martineau

Akoka

et al. 2022

Anal Bioanal Chem

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Vanillin, one of the world’s most popular flavor used in food and pharmaceutical industries, is extracted from vanilla beans or obtained (bio)-synthetically. The price of natural vanillin is considerably higher than that of its synthetic alternative which leads increasingly to counterfeit vanillin. Here, we describe the workflow of combining carbon isotope ratio combustion mass spectrometry with quantitative carbon nuclear magnetic resonance spectrometry (13C-qNMR) to obtain carbon isotope measurements traceable to the Vienna Peedee Belemnite (VPDB) with 0.7‰ combined standard uncertainty (or expanded uncertainty of 1.4‰ at 95% confidence level). We perform these measurements on qualified Bruker 400 MHz instruments to certify site-specific carbon isotope delta values in two vanillin materials, VANA-1 and VANB-1, believed to be the first intramolecular isotopic certified reference material (CRMs). Graphical abstract

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Section: Methodsmentioning

confidence: 99%

Site-specific carbon isotope measurements of vanillin reference materials by nuclear magnetic resonance spectrometry

Martineau

Akoka

et al. 2022

Anal Bioanal Chem

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“…Natural abundance arsenobetaine bromide was synthesized inhouse [19] and its purity of 0.9930 ± 0.0025 g/g (expanded uncertainty, k ¼ 2) was established by quantitative 1 H NMR with traceability to NIST SRM 350b benzoic acid [32]. This natural isotopic composition AsBet is available as CRM ABET-1 from NRC.…”

Section: Reagents and Solutionsmentioning

confidence: 99%

“…The purity of natural abundance arsenobetaine bromide primary standard was determined by quantitative 1 H NMR as detailed in a recent study [32]. Similarly, the purity of natural isotopic abundance methyl mercury chloride (MeHgCl), purchased from Sigma-Aldrich Canada Ltd. (Oakville, ON, Canada), was determined using the same technique.…”

Section: Sample Preparation For the Determination Of Purity Of Naturamentioning

confidence: 99%

“…Thus, efforts were made for the determination of purity of MeHgCl by 1 H-NMR, similar to the determination of purity of AsBet in a previous study [32]. The determination of purity of the MeHgCl primary standard using 1 H-NMR is based on NIST SRM 350b benzoic acid as a calibrator, which is co-dissolved with MeHg in a known mass ratio.…”

Section: Determination Of Purity Of Natural Abundance Mehgcl Primary mentioning

confidence: 99%

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Species specific isotope dilution for the accurate and SI traceable determination of arsenobetaine and methylmercury in cuttlefish and prawn

Kumkrong

et al. 2016

Analytica Chimica Acta

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READ THESE TERMS AND CONDITIONS CAREFULLY BEFORE USING THIS WEBSITE.http://nparc.cisti-icist.nrc-cnrc.gc.ca/eng/copyright Vous avez des questions? Nous pouvons vous aider. Pour communiquer directement avec un auteur, consultez la première page de la revue dans laquelle son article a été publié afin de trouver ses coordonnées. Si vous n'arrivez pas à les repérer, communiquez avec nous à PublicationsArchive-ArchivesPublications@nrc-cnrc.gc.ca. Questions? Contact the NRC Publications Archive team atPublicationsArchive-ArchivesPublications@nrc-cnrc.gc.ca. If you wish to email the authors directly, please see the first page of the publication for their contact information. NRC Publications Archive Archives des publications du CNRCThis publication could be one of several versions: author's original, accepted manuscript or the publisher's version. / La version de cette publication peut être l'une des suivantes : la version prépublication de l'auteur, la version acceptée du manuscrit ou la version de l'éditeur. NRC Publications Record / Notice d'Archives des publications de CNRC:http://nparc.cisti-icist.nrc-cnrc.gc.ca/eng/view/object/?id=31e489cf-7228-467b-ba7c-d3e5ee9917b8 http://nparc.cisti-icist.nrc-cnrc.gc.ca/fra/voir/objet/?id=31e489cf-7228-467b-ba7c-d3e5ee9917b8 Methods based on species specific isotope dilution were developed for the accurate and SI traceable determination of arsenobetaine (AsBet) and methylmercury (MeHg) in prawn and cuttlefish tissues by LC-MS/MS and SPME GC-ICPMS. Quantitation of AsBet and MeHg were achieved by using a Contents lists available at ScienceDirectAnalytica Chimica Acta whereas MeHg in PRON-1 was found to be < 0.015 mg kg À1. It was found that AsBet comprised 69.7% and 99.0% of total As in the prawn and cuttlefish, respectively, whereas MeHg comprised 94.5% of total Hg in cuttlefish.

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“…These are independent of sample preparation and may contain contributions arising from data acquisition, postacquisition processing, and signal quantification strategy. It is common for all errors to be declared alongside their estimates in an uncertainty budget from which the overall uncertainty of a quantitative measurement may be calculated using generally accepted error propagation techniques. , There is rich literature detailing the breakdown, analysis, and estimation of uncertainty within the context of various qNMR applications. ,,− Yet, while it is common for each component of uncertainty to be estimated either experimentally or computationally on the basis of repeated measurements, the uncertainty contributions due to the actual qNMR measurement process should, in principle, be faithfully simulated based on the analysis of a single acquired spectrum. This is due to the well-developed theories underlying the physics of NMR, discrete Fourier Transform (FT), NMR signal processing, and noise therein, as well as the stability and reliability of modern high-field spectroscopic setups.…”

Section: Introductionmentioning

confidence: 99%

A Monte Carlo Method for Analyzing Systematic and Random Uncertainty in Quantitative Nuclear Magnetic Resonance Measurements

Khirich¹

2021

Anal. Chem.

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Quantitative nuclear magnetic resonance (qNMR) is a powerful analytical technology that is capable of quantifying the concentration of any analyte with exquisite accuracy and precision so long as it contains at least one nonlabile nuclear magnetic resonance (NMR)-active nucleus. Unlike with traditional analytical technologies, the concentrations of analytes do not directly influence the uncertainty in the quantification of NMR signals because an ideal NMR response depends only on the nature and amount of the nucleus being observed. Rather, in the absence of spectral artifacts and under favorable experimental conditions, the measurement uncertainty may be influenced by the following factors: (1) spectroscopic parameters such as the spectral width, number of time domain points, and acquisition time; (2) postacquisition data processing, such as apodization and zero-filling; (3) the signal-to-noise ratios (SNRs) and lineshapes of the two signals being used in a qNMR measurement; and (4) the method of signal quantification employed, such as numerical integration or lineshape fitting (LF). Here, a general Monte Carlo (MC) method that considers these factors is presented, with which the random and systematic contributions to qNMR measurement uncertainty may be calculated. Autocorrelation analysis of synthetic and experimental noise is used in a fingerprint-like approach to demonstrate the validity of the simulations. The MC method allows for a general quantitative assessment of measurement uncertainty without the need to acquire spectral replicates and without reference to the molecular structures and concentrations of analytes. Representative examples of qNMR measurement uncertainty simulations are provided in which the metrological performances of integration and LF are contrasted for signal pairs obtained using various acquisition and processing schemes in the low-SNR regimean area where application of the proposed MC method may prove to be particularly salient.

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Determination of chemical purity and isotopic composition of natural and carbon-13-labeled arsenobetaine bromide standards by quantitative1H-NMR

Cited by 11 publications

References 19 publications

Site-specific carbon isotope measurements of vanillin reference materials by nuclear magnetic resonance spectrometry

Site-specific carbon isotope measurements of vanillin reference materials by nuclear magnetic resonance spectrometry

Species specific isotope dilution for the accurate and SI traceable determination of arsenobetaine and methylmercury in cuttlefish and prawn

A Monte Carlo Method for Analyzing Systematic and Random Uncertainty in Quantitative Nuclear Magnetic Resonance Measurements

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