High accuracy isotope dilution analysis for the determination of ethanol using gas chromatography-combustion-isotope ratio mass spectrometry

Briche, Céline S. J. Wolff; Hernández, Helena; O’Connor, Gavin; Webb, Ken; Catterick, Tim

doi:10.1039/b005878p

Cited by 18 publications

(8 citation statements)

References 9 publications

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“…While the oxygen isotopic composition of the spike could be measured and used to determine an appropriate correction for the presence of 17 O in the CO 2 resulting from chemical oxidation of the spike, a simpler option is to ensure that the oxygen isotopic composition of all peaks in chromatograms is identical. In other words, the aim “is to try to ‘reproduce’ the same oxygen isotopic composition in the different blends measured so that it can compensate for the effects of the oxygen contribution [32]. ” This approach has previously been applied during the analysis and certification of a steroid reference material and for exact-matching ID-IRMS analysis of ethanol [33, 34].…”

Section: Resultsmentioning

confidence: 99%

Systematic comparison of post-column isotope dilution using LC-CO-IRMS with qNMR for amino acid purity determination

et al. 2019

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Determination of the purity of a substance traceable to the International System of Units (SI) is important for the production of reference materials affording traceability in quantitative measurements. Post-column isotope dilution using liquid chromatography-chemical oxidation-isotope ratio mass spectrometry (ID-LC-CO-IRMS) has previously been suggested as a means to determine the purity of organic compounds; however, the lack of an uncertainty budget has prevented assessment of the utility this approach until now. In this work, the previously published ID-LC-CO-IRMS methods have not only been improved by direct gravimetric determination of the mass flow of 13C-labelled spike but also a comprehensive uncertainty budget has been established. This enabled direct comparison of the well-characterised ID-LC-CO-IRMS method to quantitative nuclear magnetic resonance spectroscopy (qNMR) for purity determination using valine as the model compound. The ID-LC-CO-IRMS and qNMR methods provided results that were in agreement within the associated measurement uncertainty for the purity of a sample of valine of (97.1 ± 4.7)% and (99.64 ± 0.20)%, respectively (expanded uncertainties, k = 2). The magnitude of the measurement uncertainty for ID-LC-CO-IRMS determination of valine purity precludes the use of this method for determination of purity by direct analysis of the main component in the majority of situations; however, a mass balance approach is expected to result in significantly improved measurement uncertainty.Electronic supplementary materialThe online version of this article (10.1007/s00216-019-02116-2) contains supplementary material, which is available to authorized users.

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Section: Resultsmentioning

confidence: 99%

Systematic comparison of post-column isotope dilution using LC-CO-IRMS with qNMR for amino acid purity determination

et al. 2019

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“…It is worth noting that the isotopic pattern of an alcoholic beverage is a very common feature which is employed for establishment of the alcohol origin . Thus, if synthetic ethanol is added to the drink, eg, in order to reduce the price of the final product, the isotopic pattern analysis would probably reveal this adulteration.…”

Section: Introductionmentioning

confidence: 99%

“…The first one is It is worth noting that the isotopic pattern of an alcoholic beverage is a very common feature which is employed for establishment of the alcohol origin. [27][28][29][30][31] Thus, if synthetic ethanol is added to the drink, eg, in order to reduce the price of the final product, the isotopic pattern analysis would probably reveal this adulteration. Ethanol of different origin has a different δ 13 C which can be detected by gas chromatography isotope ratio mass spectrometry (GC-IRMS).…”

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confidence: 99%

The perspectives of ethanol usage as an internal standard for the quantification of volatile compounds in alcoholic products by GC‐MS

et al. 2020

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The potential use of ethanol as an internal standard (IS) for GC‐MS analysis was studied. The paper describes the analysis of spirit drinks and other alcoholic products which consist of a mixture of water, ethanol, and volatile compounds. In the suggested method, ethanol was employed as an IS for the common procedure of volatile compounds quantification. A number of standard solutions of nine compounds with different concentrations was prepared in a water‐ethanol matrix and measured with GC‐MS in the SIM mode. Two possible approaches were suggested to avoid detector saturation during ethanol detection. The first one consisted in using less abundant m/z 47 as quantifiers. These ions mainly correspond to unfragmented heavy ethanol molecules containing one 13C isotope. The second method consisted in reduction of the voltage of MS electron multiplier. The experiment also included the preparation and subsequent dilution of the standard solution and ethanol with water, which determined the linearity of the modified MS response relative to the ethanol content. Analysis of the obtained results revealed that volatile compounds can be successfully accurately determined with GC‐MS by employing ethanol as an IS. Application of the suggested method is not limited to the reported volatile compounds and alcoholic products.

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“…A variant of the IDMS equation was developed by Henrion 14 and modified by Catterick et al 15,16 as a tool for inorganic analysis. In this revised equation a primary standard diluted to simulate the sample is doped with an equal amount of spike.…”

Section: Introductionmentioning

confidence: 99%

A high accuracy primary ratio method for the determination of iodine in complex matrices by double isotope dilution using MC-ICPMS and 129I spike

Santamaría-Fernández¹,

Evans²,

Wolff-Briche³

et al. 2006

J. Anal. At. Spectrom.

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Iodine is an essential element and yet is poorly represented in matrix reference materials. In this paper a novel development of the double IDMS equation using 129 I spike is presented which is ideally suited for the provision of primary measurements of iodine in complex matrices. Tolerances of the double IDMS method for iodine determination using a multi-collector ICPMS have been explored. The results indicate that even early approximates of the iodine concentration in the sample will give accurate results. The method is therefore potentially applicable to accurate one-off measurements where an iterative matching of samples and standards is not necessary. In addition, by limiting the procedure to only using standards that do not exceed at any point a maximum activity of 0.4 Bq g À1 (61 ng g À1 129 I) then the samples and standards can be handled outside of radiological control. The new methodology has been applied to the measurement of iodine in established reference materials BCR 063R, NIST SRM1846, NIST SRM1549, a FAPAS s (Food Analysis Performance Assessment Scheme) material C300 6994 and a candidate reference material in manufacture at LGC (LGC7163). The digestion procedure involved the addition of TMAH 5% and 129 I spike to 0.5 g of sample and heating to 100 1C in an oven for 2 hours. Data obtained for the reference materials showed excellent agreement with the reference values for iodine. Expanded relative uncertainties at the 95% confidence level in the different materials for iodine recoveries relative to gravimetric standards varied from 1.4 to 5.7% (k = 2).

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High accuracy isotope dilution analysis for the determination of ethanol using gas chromatography-combustion-isotope ratio mass spectrometry

Cited by 18 publications

References 9 publications

Systematic comparison of post-column isotope dilution using LC-CO-IRMS with qNMR for amino acid purity determination

Systematic comparison of post-column isotope dilution using LC-CO-IRMS with qNMR for amino acid purity determination

The perspectives of ethanol usage as an internal standard for the quantification of volatile compounds in alcoholic products by GC‐MS

A high accuracy primary ratio method for the determination of iodine in complex matrices by double isotope dilution using MC-ICPMS and 129I spike

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