食品分析の信頼性確保における定量NMRに基づく相対モル感度の役割―分析種の定量用標品不要なクロマトグラフィーの開発

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タイトル別名
  • Role of Relative Molar Sensitivity Based on Quantitative NMR in Ensuring Reliability of Food Analysis: Development of Chromatography without Need for Analyte Reference Material
  • ショクヒン ブンセキ ノ シンライセイ カクホ ニ オケル テイリョウ NMR ニ モトズク ソウタイ モル カンド ノ ヤクワリ : ブンセキシュ ノ テイリョウヨウヒョウヒン フヨウ ナ クロマトグラフィー ノ カイハツ

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説明

Measuring content values such as functional compounds, food additives, and residual pesticides are important parameters for quality assessments of foods. In many cases, the sample extracts consist of multiple components and analytes should be determined under conditions that separate individual components. Chromatographic methods such as HPLC and GC are particularly widely used for such analyses. One concern is that the content values of analytes depend on the purity of each standard. To improve the reliability of the standards, we had developed 1H quantitative NMR (1H-qNMR) with an internal standard (IS) for the purity measurement of each standard. Since signal areas between a standard (analyte) and an IS correspond to numbers of nuclei of each, if a certified reference material (CRM) is used as the IS, the purity of the standard can be accurately determined by comparing the signal area of the analyte with that of the IS. The obtained purity can be used to correct the concentrations of the calibration standards for the analyte using chromatography. However, there is still a problem; not everyone has an NMR instrument. Therefore, we really expect reagent companies having NMR to supply reference materials (RMs) having an authentic purity value for all analytes. However, since there are huge numbers of analytes to be analyzed in the field of food analysis, this expectation is not realistic.<br> 　Therefore, we focused on how to develop chromatography without a need for RMs for analytes. We decided to use a suitable RM of another compound which is available from reagent market. This has led to designing an off-line combination of chromatography and 1H-qNMR for determination of relative molar sensitivity (RMS) of each analyte to a suitable RM. The RMS is calculated as follows: (1) artificial mixture of the analyte and the RM are subjected to 1H-qNMR and chromatography; (2) the response ratio of the analyte and the RM, obtained by chromatography, is corrected using the molar ratio, as obtained by 1H-qNMR. Then, using chromatography, analyte content can be determined from the RMS value, the peak area of the analyte and the RM, and the amount of the RM precisely added to the sample solution. In this review, the chromatography using RMS is introduced as a versatile tool for ensuring the reliability of food analysis. Furthermore, we also introduce the example of evaluating the reliability of quantitative values obtained by HPLC/UV and GC/FID using RMSs (Analytical chemistry, 2017, 89 (13), pp6963–6968), and the example applied to quality assessments of natural food coloring, cochineal extract (Food Additives & Contaminants: Part A, 2018, 35 (5), pp838–847).

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  • FFIジャーナル

    FFIジャーナル 224 (2), 123-130, 2019-04-01

    FFIジャーナル編集委員会

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