title: A quantitative ¹H nuclear magnetic resonance (qHNMR) method for assessing the purity of iridoids and secoiridoids.
abstract: This paper utilized a quantitative (1)H nuclear magnetic resonance (qHNMR) method for assessing the purity of iridoids and secoiridoids. The method was fully validated, including specificity, linearity, accuracy, precision, reproducibility, and robustness. For optimization of experimental conditions, several experimental parameters were investigated, including relaxation delay (D1), scan numbers (NS) and power length (PL1). The quantification was based on the area ratios of H-3 from analytes relative to aromatic protons from 1,4-dinitrobenzene (internal standard) with methanol-d4 as solvent. Five iridoids and secoiridoids (sweroside, swertiamarin, gentiopicroside, geniposide, genipin) were analyzed. Furthermore, the results were validated by the high performance liquid chromatography coupled with ultraviolet detection (HPLC-UV) method. It can be concluded that the qHNMR method was simple, rapid, and accurate, providing a reliable and superior method for assessing the purity of iridoids and secoiridoids.
authors.affiliation: Institute of Chinese Materia Medica, Shanghai University of Traditional Chinese Medicine, Shanghai 201203, China; School of Pharmacy, Shenyang Pharmaceutical University, Shenyang 110016, China.
authors.forename: Zeyun
authors.initials: Z
authors.lastname: Li
authors.affiliation: Institute of Chinese Materia Medica, Shanghai University of Traditional Chinese Medicine, Shanghai 201203, China.
authors.forename: Edward
authors.initials: E
authors.lastname: Welbeck
authors.affiliation: Institute of Chinese Materia Medica, Shanghai University of Traditional Chinese Medicine, Shanghai 201203, China.
authors.forename: Li
authors.initials: L
authors.lastname: Yang
authors.affiliation: Institute of Chinese Materia Medica, Shanghai University of Traditional Chinese Medicine, Shanghai 201203, China.
authors.forename: Chunyong
authors.initials: C
authors.lastname: He
authors.affiliation: Institute of Chinese Materia Medica, Shanghai University of Traditional Chinese Medicine, Shanghai 201203, China.
authors.forename: Haijun
authors.initials: H
authors.lastname: Hu
authors.affiliation: Institute of Chinese Materia Medica, Shanghai University of Traditional Chinese Medicine, Shanghai 201203, China.
authors.forename: Ming
authors.initials: M
authors.lastname: Song
authors.affiliation: School of Pharmacy, Shenyang Pharmaceutical University, Shenyang 110016, China. Electronic address: kaishunbi.syphu@gmail.com.
authors.forename: Kaishun
authors.initials: K
authors.lastname: Bi
authors.affiliation: Institute of Chinese Materia Medica, Shanghai University of Traditional Chinese Medicine, Shanghai 201203, China. Electronic address: ztwang@shutcm.edu.cn.
authors.forename: Zhengtao
authors.initials: Z
authors.lastname: Wang
mesh_terms: D002851:Chromatography, High Pressure Liquid / Q000379:methods; D057888:Iridoid Glucosides / Q000737:chemistry*; D039823:Iridoids / Q000737:chemistry; D009682:Magnetic Resonance Spectroscopy / Q000379:methods*; D015394:Molecular Structure; D011753:Pyrones / Q000737:chemistry; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity
chemical_list: D057888:Iridoid Glucosides; D039823:Iridoids; D011753:Pyrones; C012997:gentiopicroside; C007835:geniposide; C013270:swertiamarin; C007834:genipin; C049412:sweroside
keywords: 1,4-Dinitrobenzene (PubChem CID: 7492); Genipin (PubChem CID: 442424); Geniposide (PubChem CID: 107848); Gentiopicroside (PubChem CID: 88708); HPLC-UV; Iridoids and secoiridoids; Purity; Sweroside (PubChem CID: 161036); Swertimarin (PubChem CID: 442435); qHNMR