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.
Highlights
Nuclear magnetic resonance spectroscopy (NMR), as a well-known analytical technique, has been routinely used for the structure elucidation of organic compounds, especially of newly synthesized and natural products
QHNMR was developed and validated for the purity test of aryltetralin lactone lignans. 1,4dinitrobenzene was used as internal standard
The results investigated by the high performance liquid chromatography (HPLC)-UV analytic system were in good agreement with those assessed by the quantitative 1H Nuclear Magnetic Resonance (qHNMR) method, with differences of less than 1.3%
Summary
Nuclear magnetic resonance spectroscopy (NMR), as a well-known analytical technique, has been routinely used for the structure elucidation of organic compounds, especially of newly synthesized and natural products. QHNMR was firstly published in 1963, for measuring the intra-molecular proton ratios in organic compounds [1]. Due to the wide use of NMR spectrometers with high magnetic fields and the improvements in the probes, gradient shimming techniques, and efficient signal treatment methods, qHNMR has been ameliorated continually in sensitivity, resolution, and precision [4]. Numerous applications of qHNMR have been reported in the fields of phyto-preparations [5,6], agricultural products [7], natural products [8], disease diagnosis, environmental toxicity, metabolomics, pharmaceutics [2], and so on. It was confirmed that qHNMR was a reliable and accurate technique for quantitative analysis
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