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Quantitative determination of febrifugine by proton nuclear magnetic resonance spectroscopy with internal standard method / 中国中药杂志
China Journal of Chinese Materia Medica ; (24): 134-138, 2018.
Article in Chinese | WPRIM | ID: wpr-776412
ABSTRACT
A quantitative nuclear magnetic resonance method(qNMR) was established for determination of the absolute content of febrifugine. Proton nuclear magnetic resonance spectroscopy of febrifugine was obtained in DMSO-d₆ with hydroquinone as the internal standard substance on a Bruker Ascend 600 MHz superconducting nuclear resonance spectrometer at 298 K. The specific parameters were as follows the observing frequency was 600 MHz,spectra width was 7 211 Hz, pulse width was 9.70 μs, pulse sequence was zg30,scan times was 32 and relaxation time was 2 s. The proton signal peaked at δ 7.71 for febrifugine and δ 6.55 for hydroquinone were selected as the quantification peaks. Linear regression of quantitative peak area ratio of febrifugine-hydroquinone versus their mass ratio yielded a correlation coefficient of 0.999 6 and a regression equation of +0.008 6.The linear range of febrifugine was 2.17-17.07 g·L⁻¹,the precision RSD was 0.78%(=6),the repeatability RSD was 1.2%(=6),and the contents of three batches of febrifugine sample were 94.91%,95.09% and 95.52%,respectively. The content of febrifugine was 96.44% determined by high performance liquid chromatography(HPLC). The relative error of the content of febrigugine determinted by qNMR and HPLC methods was 1.27%. The results showed that the internal standard method of proton nuclear magnetic resonance spectroscopy could be used to determine the absolute content of febrifugine.
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Full text: Available Index: WPRIM (Western Pacific) Main subject: Piperidines / Protons / Quinazolines / Magnetic Resonance Spectroscopy Language: Chinese Journal: China Journal of Chinese Materia Medica Year: 2018 Type: Article

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Full text: Available Index: WPRIM (Western Pacific) Main subject: Piperidines / Protons / Quinazolines / Magnetic Resonance Spectroscopy Language: Chinese Journal: China Journal of Chinese Materia Medica Year: 2018 Type: Article