Accéder au contenu
Merck

A quantitative ¹H nuclear magnetic resonance (qHNMR) method for assessing the purity of iridoids and secoiridoids.

Fitoterapia (2014-12-17)
Zeyun Li, Edward Welbeck, Li Yang, Chunyong He, Haijun Hu, Ming Song, Kaishun Bi, Zhengtao Wang
RÉSUMÉ

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.

MATÉRIAUX
Référence du produit
Marque
Description du produit

Sigma-Aldrich
Acétonitrile, suitable for HPLC, gradient grade, ≥99.9%
Sigma-Aldrich
Acétonitrile, HPLC Plus, ≥99.9%
Sigma-Aldrich
Méthanol-d4, ≥99.8 atom % D
Sigma-Aldrich
Acide phosphorique, ACS reagent, ≥85 wt. % in H2O
Sigma-Aldrich
Acétonitrile, ACS reagent, ≥99.5%
Sigma-Aldrich
Acide phosphorique, 85 wt. % in H2O, 99.99% trace metals basis
Sigma-Aldrich
Acide phosphorique, ACS reagent, ≥85 wt. % in H2O
Sigma-Aldrich
Acétonitrile, suitable for HPLC, gradient grade, ≥99.9%
Sigma-Aldrich
Méthanol-d4, ≥99.8 atom % D
Sigma-Aldrich
Acétonitrile, anhydrous, 99.8%
Sigma-Aldrich
Acide phosphorique, crystalline, ≥99.999% trace metals basis
Sigma-Aldrich
Méthanol-d4, ≥99.8 atom % D, contains 0.03 % (v/v) TMS
Sigma-Aldrich
Acide phosphorique, 85 wt. % in H2O, FCC, FG
Sigma-Aldrich
Méthanol-d4, 99 atom % D
Sigma-Aldrich
Acide phosphorique, BioUltra, ≥85% (T)
Sigma-Aldrich
Acétonitrile, biotech. grade, ≥99.93%
Sigma-Aldrich
Méthanol-d4, ≥99.8 atom % D, contains 0.05 % (v/v) TMS
Sigma-Aldrich
Acide phosphorique, ≥85 wt. % in H2O, ≥99.999% trace metals basis
Sigma-Aldrich
Acétonitrile, ReagentPlus®, 99%
Sigma-Aldrich
Acide phosphorique, BioReagent, suitable for insect cell culture, 85%
Sigma-Aldrich
Acétonitrile, electronic grade, 99.999% trace metals basis
Sigma-Aldrich
Acétonitrile, suitable for DNA synthesis, ≥99.9% (GC)
Supelco
Acétonitrile, Pharmaceutical Secondary Standard; Certified Reference Material
Sigma-Aldrich
Méthanol-d4, "100%", 99.96 atom % D
Sigma-Aldrich
Méthanol-d4, anhydrous, ≥99.8 atom % D
Sigma-Aldrich
Acide phosphorique solution, NMR reference standard, 85% in D2O (99.9 atom % D), NMR tube size 4.2 mm × 8 in. , WGS-5BL Coaxial NMR tube
USP
Residual Solvent Class 2 - Acetonitrile, United States Pharmacopeia (USP) Reference Standard
Supelco
Acétonitrile, analytical standard
Sigma-Aldrich
Méthanol-d4, ≥99.8 atom % D, contains 0.1 % (v/v) TMS
Sigma-Aldrich
Acide phosphorique solution, NMR reference standard, 85% in D2O (99.9 atom % D), NMR tube size 5 mm × 8 in.