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

Molecules

Yan-Jun Sun¹  Yan-Li Zhang¹  Yu Wang²  Jun-Min Wang¹  Xuan Zhao¹  Jian-Hong Gong¹  Wei Gao¹  Yan-Bin Guan¹ 

[1] Collaborative Innovation Center for Respiratory Disease Diagnosis, Treatment & Chinese Medicine Development of Henan Province, Henan University of Traditional Chinese Medicine, Zhengzhou 450046, China; E-Mails:;School of Pharmacy, China Medical University, Shenyang 110122, China; E-Mail:

关键词: qHNMR;    HPLC-UV;    purity;    aryltetralin lactone lignan;   

DOI  :  10.3390/molecules20069671

来源: mdpi

【 摘 要 】

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.

【 授权许可】

CC BY   
© 2015 by the authors; licensee MDPI, Basel, Switzerland.