ABSTRACT
Chinese medicinal injection, made of active components extracted from Chinese medicine or Chinese medicinal compound, is a novel dosage form of Chinese patent medicine in China and is pivotal in the traditional Chinese medicine(TCM) industry. The quality control standard of Chinese medicinal injection determines its safety and efficacy. The quantitative nuclear magnetic resonance(qNMR) spectroscopy is a non-targeted, non-invasive, and non-destructive technique with high reproducibility, short measurement time, convenient sample preparation, a broad range of linearity, and no requirement on the reference substance of tested components, which is advantageous as compared with traditional chromatographic methods, and it can provide information about the molecular composition of the tested samples. Therefore, in light of multiple challenges in the quality control of Chinese medicinal injection, such as complex composition, difficulties in quantitative analysis, and the shortage of reference substances, the application of qNMR spectroscopy combined with chemometrics techniques was proposed for the quality evaluation of Chinese medicine reference substances, Chinese medicinal injection, and intermediates in the production process, as well as for the stability analysis of Chinese medicinal injection. This study is expected to provide references for the application of qNMR spectroscopy in the quality control of Chinese medicinal injection.
Subject(s)
Magnetic Resonance Spectroscopy , Medicine, Chinese Traditional , Quality Control , Reproducibility of ResultsABSTRACT
The inundation of Cordyceps sinensis counterfeits in the market makes it difficult to identify. In this study, 21 batches of wild C. sinensis from 3 different regions, 30 batches of naturally cultured C. sinensis and 4 kinds of counterfeits extracted by methanol and water were analyzed using NMR technology. 9 characteristic peaks were defined as quantitative criterion after comparison, and NMR fingerprints of C. sinensis were established. According to the result it is highly similar between naturally cultured C. sinensis and wild ones by comparing their NMR fingerprints. However, NMR spectra of four kinds of adulterants showed differences with C. sinensis. The result also showed that NMR fingerprint of C. sinensis are highly characteristic and specific. The NMR characteristic fingerprint of wild C. sinensis was consistent with the naturally cultured C. sinensis, and it indicated that the chemical constituents of wild C. sinensis and naturally cultured C. sinensis are nearly the same.
ABSTRACT
AIM: To establish ()~1H NMR fingerprint of Radix Daphne genkwa to disclose its chemical composition of the secondary metabolites and provide a quick and credible assay for the detoxicated extraction of the active constituents. METHODS: The ()~1H NMR spectrum of petrol-acetone-methanol extract from Radix Dephne genkwa was detected using CDCl_3/DMSO-d_6(1∶1) as the deuterium reagent. The resonance intensity of the proton in the spectrum was indicated in relative integral area of peaks referenced by the resonance intensity of methyl signal in DMSO. The ()~1H NMR of cascade extraction of Radix Dephne genkwa by the reagent in sequence of petrol→acetone→methanol or chloroform→aether→acetyl acetate→methanol was utilized for observing the variation on their chemical compositions. RESULTS: The ()~1H NMR of Radix Dephne genkwa clearly expressed the information of the protons from long chain aliphatics or genkwadaphnin derivatives, aromatic coumarins or flavonoids as well as glycosides with moiety(ies) of pyran saccharide, symbolizing the existence of aliphatics, genkwadaphnin derivatives, coumarins and flavonoids. Remarkable difference was observed in ()~1H NMR spectrum of the extract by different cascade reagent. As the increase in the polarity of reagent, the intensity of the proton signals in upper field was quickly reduced concomitantly with the rapid enhancement of active proton signals from hydroxyls and saccharides in glycosides in down field. CONCLUSION: The ()~1H NMR fingerprint of Radix Dephne genkwa possesses its own characteristics and can be used as a reliable assay for studying the extraction of active constituents with minimum content of toxic diterpenoids. (Key