Objective: To establish a quantitative nuclear magnetic resonance hydrogen spectroscopy(1H qNMR) method for determining the moisture content in several pharmaceutical excipients. Methods: Using sodium benzenesulfonate as the internal standard and heavy water as the solvent, the water content in the blank sample was determined by absolute quantification using nuclear magnetic resonance spectroscopy. By comparing with the blank value, a quantitative calculation formula for the water content in the sample was established, and the water content in the sample was tested and calculated. Results: Methodological studies had shown that this method had a good linear relationship(r=0.999 1), with a linear range of 0.032-0.561 mg absolute water content in the sample, the precision RSD was 0.039%, repeatability RSD was 0.43%, and the average recovery was 98.7%. The 1H qNMR method measured the water content in DMSO-1, DMSO-2, sodium benzenesulfonate, and sodium acetate to be 0.23%, 0.28%, 0.46%, and 0.28%, respectively, which were essentially consistent with the results obtained from the method described in the Chinese Pharmacopoeia(2020). Conclusion: The 1H qNMR method established is fast, simple to operate, with a small sample size and accurate results. It can be used for the determination of water content in some pharmaceutical excipients.
CHEN Xin-qi
,
WEN Jing
,
LIU Hao-hui-ling
,
ZHANG Mei
,
JIAO Xiao-lin
,
WANG Wei
. Rapid determination of water content in certain pharmaceutical excipients by 1H qNMR method*[J]. Chinese Journal of Pharmaceutical Analysis, 2024
, 44(11)
: 1992
-1996
.
DOI: 10.16155/j.0254-1793.2024-0258
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