Quantification of Clitidine in <i>Paralepistopsis acromelalga</i> Using Quantitative NMR Method

Because one toxic component of Paralepistopsis acromelalga, clitidine, is not commercially available as a reagent and because standards are difficult to obtain, a quantitative NMR method that requires no standard was investigated for this study. To compare the quantitative values obtained using the two methods, the absolute purity of the standard used for the LC-MS/MS method was calculated using quantitative NMR. The result was calculated as 89.8±1.5%: more than 10% lower than the result obtained using conventional HPLC purity. This finding is presumably attributable to the presence of water in the crystals. Calculating the absolute purity of the product before use is crucially important. The values of the Paralepistopsis acromelalga fruit extract were quantified and compared using conventional LC-MS/MS and quantitative NMR. The quantitative values did not differ significantly, suggesting that, in most cases, they were within a 5% margin of error. Furthermore, quantitative NMR provides several benefits not obtained using conventional methods, including its rapid measurement capability and its obviation of the need for a reference material for the measured substance. By virtue of these benefits, quantitative NMR is an extremely useful tool for natural toxin analysis where sudden outbreaks occur and for which rapid calculation of results is necessary.

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Publication Details

Journal
Food Hygiene and Safety Science (Shokuhin Eiseigaku Zasshi)
Published
2024-08-25
DOI
https://doi.org/10.3358/shokueishi.65.84
Primary Topic
Analytical Chemistry and Chromatography
Type
article
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article

Quantification of Clitidine in Paralepistopsis acromelalga Using Quantitative NMR Method

Yuka Nagaoka, Yoshitaka Ishida
Food Hygiene and Safety Science (Shokuhin Eiseigaku Zasshi)
Analytical Chemistry and Chromatography
article

Quantification of Clitidine in Paralepistopsis acromelalga Using Quantitative NMR Method

Yuka Nagaoka, Yoshitaka Ishida
article en

Abstract

Because one toxic component of Paralepistopsis acromelalga, clitidine, is not commercially available as a reagent and because standards are difficult to obtain, a quantitative NMR method that requires no standard was investigated for this study. To compare the quantitative values obtained using the two methods, the absolute purity of the standard used for the LC-MS/MS method was calculated using quantitative NMR. The result was calculated as 89.8±1.5%: more than 10% lower than the result obtained using conventional HPLC purity. This finding is presumably attributable to the presence of water in the crystals. Calculating the absolute purity of the product before use is crucially important. The values of the Paralepistopsis acromelalga fruit extract were quantified and compared using conventional LC-MS/MS and quantitative NMR. The quantitative values did not differ significantly, suggesting that, in most cases, they were within a 5% margin of error. Furthermore, quantitative NMR provides several benefits not obtained using conventional methods, including its rapid measurement capability and its obviation of the need for a reference material for the measured substance. By virtue of these benefits, quantitative NMR is an extremely useful tool for natural toxin analysis where sudden outbreaks occur and for which rapid calculation of results is necessary.

Food Hygiene and Safety Science (Shokuhin Eiseigaku Zasshi)Vol. 65(4)
Yamagata Prefectural Institute of Public Health (JP)
Openalex Percentile: Top 86%
Analytical Chemistry and Chromatography
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