Collaborative Study to Validate Purity Determination by 1H quantitative NMR Spectroscopy by Using Internal Calibration Methodology.

Collaborative Study to Validate Purity Determination by 1H quantitative NMR Spectroscopy by Using Internal Calibration Methodology. Chem Pharm Bull (Tokyo). 2020 Jun 19;: Authors: Miura T, Sugimoto N, Bhavaraju S, Yamazaki T, Nishizaki Y, Liu Y, Bzhelyansky A, Amezcua C, Ray J, Zailer E, Diehl B, Gallo V, Todisco S, Ofuji K, Fujita K, Higano T, Geletneky C, Hausler T, Singh N, Yamamoto K, Kato T, Sawa R, Watanabe R, Iwamoto Y, Goda Y Abstract Nuclear Magnetic Resonance (NMR) spectroscopy has recently been utilized to determine the absolute amounts of organic molecules with metrological traceability since signal intensity is directly proportional to the number of each nucleus in a molecule. The NMR methodology that uses hydrogen nucleus (1H) to quantify chemicals is called quantitative 1H NMR (1H qNMR). The quantitative method using 1H qNMR for determining the purity or content of chemicals has been adopted into some compendial guidelines and official standards. However, there are still few reports in the literature regarding validation of 1H qNMR methodology. Here, we coordinated an international collaborative study to validate a 1H qNMR based on the use of an internal calibration methodology. Thirteen laboratories participated in this study, and the purities of three samples were individually measured using 1H qNMR method. The three samples were all certified via conventional primary methods of measurement, such as butyl p-hydroxybe...
Source: Chemical and Pharmaceutical Bulletin - Category: Drugs & Pharmacology Authors: Tags: Chem Pharm Bull (Tokyo) Source Type: research