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

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
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.

MATERIALS
Product Number
Brand
Product Description

Sigma-Aldrich
Phosphoric acid solution, NMR reference standard, 85% in D2O (99.9 atom % D), NMR tube size 3 mm × 8 in.
Sigma-Aldrich
Phosphoric acid solution, NMR reference standard, 85% in D2O (99.9 atom % D), NMR tube size 5 mm × 8 in.
Sigma-Aldrich
Methanol-d4, ≥99.8 atom % D, contains 1 % (v/v) TMS
Sigma-Aldrich
Methanol-d4, "100%", 99.96 atom % D
Sigma-Aldrich
Phosphoric acid solution, 85 wt. % in H2O, FCC, FG
Sigma-Aldrich
Methanol-d4, "100%", ≥99.96 atom % D, contains 0.03 % (v/v) TMS
Sigma-Aldrich
Phosphoric acid solution, NMR reference standard, 85% in D2O (99.9 atom % D), NMR tube size 4.2 mm × 8 in. , WGS-5BL Coaxial NMR tube
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Methanol-d4, ≥99.8 atom % D, contains 0.05 % (v/v) TMS
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Methanol-d4, anhydrous, ≥99.8 atom % D
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Acetonitrile solution, contains 0.1 % (v/v) trifluoroacetic acid, suitable for HPLC
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Acetonitrile solution, contains 0.05 % (v/v) trifluoroacetic acid
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Acetonitrile solution, contains 0.1 % (v/v) formic acid, suitable for HPLC
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Methanol-d4, ≥99.8 atom % D, contains 0.1 % (v/v) TMS
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Methanol-d4, 99 atom % D
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Methanol-d4, ≥99.8 atom % D, contains 0.03 % (v/v) TMS
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Acetonitrile solution, contains 10.0% acetone, 0.05% formic acid, 40.0% 2-propanol
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Methanol-d4, ≥99.8 atom % D
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Methanol-d4, ≥99.8 atom % D
Supelco
Residual Solvent - Acetonitrile, Pharmaceutical Secondary Standard; Certified Reference Material
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Phosphoric acid, LR, 88-93%
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Phosphoric acid, AR, 88-93%
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Phosphoric acid, suitable for HPLC, ≥85%
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Ultrapure Acetonitrile
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Phosphoric acid, AR, ≥88%
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Acetonitrile, AR, ≥99.5%
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Acetonitrile, ReagentPlus®, 99%
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Acetonitrile, for preparative HPLC, ≥99.8% (GC)
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Phosphoric acid, puriss. p.a., ACS reagent, reag. ISO, reag. Ph. Eur., ≥85%
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Phosphoric acid, puriss., meets analytical specification of Ph. Eur., BP, NF, FCC, 85.0-88.0%
Sigma-Aldrich
Phosphoric acid, puriss. p.a., crystallized, ≥99.0% (T)