Purity Assessment of Aryltetralin Lactone Lignans by Quantitative 1H Nuclear Magnetic Resonance
Yan-Jun Sun,
Yan-Li Zhang,
Yu Wang,
Jun-Min Wang,
Xuan Zhao,
Jian-Hong Gong,
Wei Gao,
Yan-Bin Guan
Affiliations
Yan-Jun Sun
Collaborative Innovation Center for Respiratory Disease Diagnosis, Treatment & Chinese Medicine Development of Henan Province, Henan University of Traditional Chinese Medicine, Zhengzhou 450046, China
Yan-Li Zhang
Collaborative Innovation Center for Respiratory Disease Diagnosis, Treatment & Chinese Medicine Development of Henan Province, Henan University of Traditional Chinese Medicine, Zhengzhou 450046, China
Yu Wang
School of Pharmacy, China Medical University, Shenyang 110122, China
Jun-Min Wang
Collaborative Innovation Center for Respiratory Disease Diagnosis, Treatment & Chinese Medicine Development of Henan Province, Henan University of Traditional Chinese Medicine, Zhengzhou 450046, China
Xuan Zhao
Collaborative Innovation Center for Respiratory Disease Diagnosis, Treatment & Chinese Medicine Development of Henan Province, Henan University of Traditional Chinese Medicine, Zhengzhou 450046, China
Jian-Hong Gong
Collaborative Innovation Center for Respiratory Disease Diagnosis, Treatment & Chinese Medicine Development of Henan Province, Henan University of Traditional Chinese Medicine, Zhengzhou 450046, China
Wei Gao
Collaborative Innovation Center for Respiratory Disease Diagnosis, Treatment & Chinese Medicine Development of Henan Province, Henan University of Traditional Chinese Medicine, Zhengzhou 450046, China
Yan-Bin Guan
Collaborative Innovation Center for Respiratory Disease Diagnosis, Treatment & Chinese Medicine Development of Henan Province, Henan University of Traditional Chinese Medicine, Zhengzhou 450046, China
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.
