title: Purity Assessment of Aryltetralin Lactone Lignans by Quantitative 1H Nuclear Magnetic Resonance.
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.
authors.affiliation: Collaborative Innovation Center for Respiratory Disease Diagnosis, Treatment & Chinese Medicine Development of Henan Province, Henan University of Traditional Chinese Medicine, Zhengzhou 450046, China. sunyanjun2011@hactcm.edu.cn.|School of Pharmacy, Henan University of Traditional Chinese Medicine, Zhengzhou 450046, China. sunyanjun2011@hactcm.edu.cn.
authors.forename: Yan-Jun
authors.initials: YJ
authors.lastname: Sun
authors.affiliation: Collaborative Innovation Center for Respiratory Disease Diagnosis, Treatment & Chinese Medicine Development of Henan Province, Henan University of Traditional Chinese Medicine, Zhengzhou 450046, China. zyl2013hnzy@163.com.|School of Pharmacy, Henan University of Traditional Chinese Medicine, Zhengzhou 450046, China. zyl2013hnzy@163.com.
authors.forename: Yan-Li
authors.initials: YL
authors.lastname: Zhang
authors.affiliation: School of Pharmacy, China Medical University, Shenyang 110122, China. xiaowangyu21@163.com.
authors.forename: Yu
authors.initials: Y
authors.lastname: Wang
authors.affiliation: Collaborative Innovation Center for Respiratory Disease Diagnosis, Treatment & Chinese Medicine Development of Henan Province, Henan University of Traditional Chinese Medicine, Zhengzhou 450046, China. wjmhnzz@163.com.|School of Pharmacy, Henan University of Traditional Chinese Medicine, Zhengzhou 450046, China. wjmhnzz@163.com.
authors.forename: Jun-Min
authors.initials: JM
authors.lastname: Wang
authors.affiliation: Collaborative Innovation Center for Respiratory Disease Diagnosis, Treatment & Chinese Medicine Development of Henan Province, Henan University of Traditional Chinese Medicine, Zhengzhou 450046, China. lilas616@hotmail.com.|School of Pharmacy, Henan University of Traditional Chinese Medicine, Zhengzhou 450046, China. lilas616@hotmail.com.
authors.forename: Xuan
authors.initials: X
authors.lastname: Zhao
authors.affiliation: Collaborative Innovation Center for Respiratory Disease Diagnosis, Treatment & Chinese Medicine Development of Henan Province, Henan University of Traditional Chinese Medicine, Zhengzhou 450046, China. gongjianhong2009@126.com.|School of Pharmacy, Henan University of Traditional Chinese Medicine, Zhengzhou 450046, China. gongjianhong2009@126.com.
authors.forename: Jian-Hong
authors.initials: JH
authors.lastname: Gong
authors.affiliation: Collaborative Innovation Center for Respiratory Disease Diagnosis, Treatment & Chinese Medicine Development of Henan Province, Henan University of Traditional Chinese Medicine, Zhengzhou 450046, China. xiaojun801115@163.com.|School of Pharmacy, Henan University of Traditional Chinese Medicine, Zhengzhou 450046, China. xiaojun801115@163.com.
authors.forename: Wei
authors.initials: W
authors.lastname: Gao
authors.affiliation: Collaborative Innovation Center for Respiratory Disease Diagnosis, Treatment & Chinese Medicine Development of Henan Province, Henan University of Traditional Chinese Medicine, Zhengzhou 450046, China. guanyanbin96@126.com.|School of Pharmacy, Henan University of Traditional Chinese Medicine, Zhengzhou 450046, China. guanyanbin96@126.com.
authors.forename: Yan-Bin
authors.initials: YB
authors.lastname: Guan
mesh_terms: D002851:Chromatography, High Pressure Liquid; D004136:Dinitrobenzenes / Q000032:analysis; D004365:Drugs, Chinese Herbal; D007783:Lactones / Q000032:analysis*; D017705:Lignans / Q000032:analysis*; D011034:Podophyllotoxin / Q000031:analogs & derivatives* / Q000032:analysis*; D066244:Proton Magnetic Resonance Spectroscopy; D012015:Reference Standards
chemical_list: D004136:Dinitrobenzenes; D004365:Drugs, Chinese Herbal; D007783:Lactones; D017705:Lignans; C014451:deoxypodophyllotoxin; C053052:1,4-dinitrobenzene; D011034:Podophyllotoxin
keywords: HPLC-UV; aryltetralin lactone lignan; purity; qHNMR