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Molecules 2015, 20(6), 9671-9685; doi:10.3390/molecules20069671

Purity Assessment of Aryltetralin Lactone Lignans by Quantitative 1H Nuclear Magnetic Resonance

1
Collaborative Innovation Center for Respiratory Disease Diagnosis, Treatment & Chinese Medicine Development of Henan Province, Henan University of Traditional Chinese Medicine, Zhengzhou 450046, China
2
School of Pharmacy, Henan University of Traditional Chinese Medicine, Zhengzhou 450046, China
3
School of Pharmacy, China Medical University, Shenyang 110122, China
*
Authors to whom correspondence should be addressed.
Academic Editor: Bruno Figadere
Received: 26 March 2015 / Accepted: 15 May 2015 / Published: 26 May 2015
(This article belongs to the Section Natural Products)
View Full-Text   |   Download PDF [1229 KB, uploaded 26 May 2015]   |  

Abstract

In the present work, a quantitative 1H Nuclear Magnetic Resonance (qHNMR) was established for purity assessment of six aryltetralin lactone lignans. The validation of the method was carried out, including specificity, selectivity, linearity, accuracy, precision, and robustness. Several experimental parameters were optimized, including relaxation delay (D1), scan numbers (NS), and pulse angle. 1,4-Dinitrobenzene was used as internal standard (IS), and deuterated dimethyl sulfoxide (DMSO-d6) as the NMR solvent. The purities were calculated by the area ratios of H-2,6 from target analytes vs. aromatic protons from IS. Six aryltetralin lactone lignans (deoxypodophyllotoxin, podophyllotoxin, 4-demethylpodophyllotoxin, podophyllotoxin-7′-O-β-d-glucopyranoside, 4-demethylpodophyllotoxin-7′-O-β-d-glucopyranoside, and 6′′-acetyl-podophyllotoxin-7′-O-β -d-glucopyranoside) were analyzed. The analytic results of qHNMR were further validated by high performance liquid chromatography (HPLC). Therefore, the qHNMR method was a rapid, accurate, reliable tool for monitoring the purity of aryltetralin lactone lignans. View Full-Text
Keywords: qHNMR; HPLC-UV; purity; aryltetralin lactone lignan qHNMR; HPLC-UV; purity; aryltetralin lactone lignan
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This is an open access article distributed under the Creative Commons Attribution License which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is properly cited. (CC BY 4.0).

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MDPI and ACS Style

Sun, Y.-J.; Zhang, Y.-L.; Wang, Y.; Wang, J.-M.; Zhao, X.; Gong, J.-H.; Gao, W.; Guan, Y.-B. Purity Assessment of Aryltetralin Lactone Lignans by Quantitative 1H Nuclear Magnetic Resonance. Molecules 2015, 20, 9671-9685.

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