Saltar al contenido
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
RESUMEN

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.

MATERIALES
Referencia del producto
Marca
Descripción del producto

Sigma-Aldrich
Acetonitrilo, suitable for HPLC, gradient grade, ≥99.9%
Sigma-Aldrich
Acetonitrilo, HPLC Plus, ≥99.9%
Sigma-Aldrich
Metanol-d4, ≥99.8 atom % D
Sigma-Aldrich
Ácido fosfórico, ACS reagent, ≥85 wt. % in H2O
Sigma-Aldrich
Acetonitrilo, ACS reagent, ≥99.5%
Sigma-Aldrich
Acetonitrilo, for HPLC, for UV, ≥99.9% (GC)
Sigma-Aldrich
Ácido fosfórico, 85 wt. % in H2O, 99.99% trace metals basis
Sigma-Aldrich
Ácido fosfórico, ACS reagent, ≥85 wt. % in H2O
Sigma-Aldrich
Acetonitrilo, suitable for HPLC, gradient grade, ≥99.9%
Sigma-Aldrich
Metanol-d4, ≥99.8 atom % D
Sigma-Aldrich
Ácido fosfórico, puriss. p.a., ACS reagent, reag. ISO, reag. Ph. Eur., ≥85%
Sigma-Aldrich
Ácido fosfórico, crystalline, ≥99.999% trace metals basis
Sigma-Aldrich
Ácido fosfórico, puriss. p.a., crystallized, ≥99.0% (T)
Sigma-Aldrich
Acetonitrilo, anhydrous, 99.8%
Sigma-Aldrich
Acetonitrilo, suitable for HPLC-GC, ≥99.8% (GC)
Sigma-Aldrich
Ácido fosfórico, puriss., meets analytical specification of Ph. Eur., BP, NF, FCC, 85.0-88.0%
Sigma-Aldrich
Metanol-d4, ≥99.8 atom % D, contains 0.03 % (v/v) TMS
Sigma-Aldrich
Metanol-d4, 99 atom % D
Sigma-Aldrich
Ácido fosfórico, 85 wt. % in H2O, FCC, FG
Sigma-Aldrich
Acetonitrilo, biotech. grade, ≥99.93%
Sigma-Aldrich
Ácido fosfórico, BioUltra, ≥85% (T)
Sigma-Aldrich
Metanol-d4, ≥99.8 atom % D, contains 0.05 % (v/v) TMS
Sigma-Aldrich
Ácido fosfórico, ≥85 wt. % in H2O, ≥99.999% trace metals basis
Sigma-Aldrich
Ácido fosfórico, BioReagent, suitable for insect cell culture, 85%
Sigma-Aldrich
Acetonitrilo, suitable for DNA synthesis, ≥99.9% (GC)
Sigma-Aldrich
Acetonitrilo, ReagentPlus®, 99%
Sigma-Aldrich
Acetonitrilo, electronic grade, 99.999% trace metals basis
Sigma-Aldrich
Metanol-d4, "100%", 99.96 atom % D
Supelco
Acetonitrilo, Pharmaceutical Secondary Standard; Certified Reference Material
Sigma-Aldrich
Acetonitrilo, ≥99.5% (GC)