Post-collection purity correction for internal standard correction-high performance liquid chromatography-quantitative nuclear magnetic resonance

Li, Xueyao; Zhang, Wei; Huang, Ting; Li, Ming; Su, Fuhai; Wu, Huaxin; Tang, Guangshi

doi:10.1039/d4ay00949e

Anal. Methods

2024

DOI: 10.1039/d4ay00949e

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Post-collection purity correction for internal standard correction-high performance liquid chromatography-quantitative nuclear magnetic resonance

Xueyao Li,

Wei Zhang,

Ting Huang

et al.

Abstract: The improved method enhances the accuracy of quantifying low-purity organic compounds by analyzing eluate components for correction factors, validated through oxytetracycline quantification, addressing qNMR challenges and ensuring purity.

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Comparison and Determination of the Content of Mosapride Citrate by Different qNMR Methods

Lian,

Li,

Zuo

et al. 2024

IJMS

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As a salt-type compound, mosapride citrate’s metabolism and side effects are correlated with its salt-forming ratio. Several techniques were developed in this work to compare various quantitative nuclear magnetic resonance (qNMR) methodologies and to quantitatively examine the content of raw materials. Among the qNMR techniques, methods for 1H NMR and 19F NMR were developed. Appropriate solvents were chosen, and temperature, number of scans, acquisition time, and relaxation delay parameter settings were optimized. Maleic acid was chosen as the internal standard in 1H NMR, and the respective characteristic signals of mosapride and citrate were selected as quantitative peaks. The internal standard in 19F NMR analysis was 4,4′-difluoro diphenylmethanone, and the distinctive signal peak at −116.15 ppm was utilized to quantify mosapride citrate. The precision, repeatability, linearity, stability, accuracy, and robustness of the qNMR methods were all validated according to the ICH guidelines. By contrasting the outcomes with those from high-performance liquid chromatography (HPLC), the accuracy of qNMR was assessed. As a result, we created a quicker and easier qNMR approach to measure the amount of mosapride citrate and evaluated several qNMR techniques to establish a foundation for choosing quantitative peaks for the qNMR method. Concurrently, it is anticipated that various selections of distinct quantitative objects will yield the mosapride citrate salt-forming ratio.

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Comparison and Determination of the Content of Mosapride Citrate by Different qNMR Methods

Lian,

Li,

Zuo

et al. 2024

IJMS

View full text Add to dashboard Cite

show abstract

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Post-collection purity correction for internal standard correction-high performance liquid chromatography-quantitative nuclear magnetic resonance

Abstract: The improved method enhances the accuracy of quantifying low-purity organic compounds by analyzing eluate components for correction factors, validated through oxytetracycline quantification, addressing qNMR challenges and ensuring purity.

Cited by 1 publication

References 16 publications

Comparison and Determination of the Content of Mosapride Citrate by Different qNMR Methods

Comparison and Determination of the Content of Mosapride Citrate by Different qNMR Methods

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