Detection method of related substances in vegetable drug extract-scutellarin
A technology for detection of scutellarin and its detection method, which is applied in the field of detection of related substances in the botanical extract scutellarin, and can solve the problems of no identification of substances and determination of content limits of related substances, etc.
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Embodiment 1
[0059] Embodiment 1. Separation and identification of four related substances:
[0060] The scutellarin APIs provided by 7 companies and the scutellarin tablets provided by 11 companies were used for high performance liquid chromatography detection, and the APIs with higher content of related substances were selected for the separation and identification of related substances. Take 20g of breviscapine API, dissolve it in DMF, and separate it by high performance liquid chromatography. The chromatographic column is Shimadzu Hedera ODS-P 30×250mm, 50ml / min, and the detection wavelength is 335nm. Using 26% methanol-0.05% formic acid aqueous solution as the eluent, four related substances were received according to UV light. Compounds 1, 2, 3, 4 were isolated. Compounds 1, 2, 3 and 4 were subjected to NMR spectra and high-resolution mass spectrometry, respectively. Compounds 1, 2, 3 and 4 were identified as: 6-hydroxykaempferol-7-O-β-glucuronic acid, scutellarin, scutellarin and ...
Embodiment 2
[0063] Embodiment 2. Separation and identification of four related substances:
[0064] The scutellarin APIs provided by 7 companies and the scutellarin tablets provided by 11 companies were used for high performance liquid chromatography detection, and the APIs with higher content of related substances were selected for the separation and identification of related substances. Take 20g of breviscapine API, dissolve it in DMF, and separate it by high performance liquid chromatography. The chromatographic column is Shimadzu Hedera ODS-P 30×250mm, 50ml / min, and the detection wavelength is 335nm. Using 12% acetonitrile-0.05% formic acid aqueous solution as the eluent, four related substances were received according to ultraviolet. Compounds 1, 2, 3, 4 were isolated. Compounds 1, 2, 3 and 4 were subjected to NMR spectra and high-resolution mass spectrometry, respectively. Compounds 1, 2, 3 and 4 were identified as: 6-hydroxykaempferol-7-O-β-glucuronic acid, scutellarin, scutellar...
Embodiment 3
[0067] Embodiment 3. Separation and identification of four related substances:
[0068] The scutellarin APIs provided by 7 companies and the scutellarin tablets provided by 11 companies were used for high performance liquid chromatography detection, and the APIs with higher content of related substances were selected for the separation and identification of related substances. Take 20g of breviscapine API, dissolve it in DMF, and separate it by high performance liquid chromatography. The chromatographic column is Shimadzu Hedera ODS-P 30×250mm, 50ml / min, and the detection wavelength is 335nm. Using 26% methanol-0.05% formic acid aqueous solution as the eluent, four related substances were received according to UV light. After purification by semi-preparative high performance liquid chromatography, compounds 1, 2, 3, and 4 were isolated. Compounds 1, 2, 3 and 4 were subjected to NMR spectra and high-resolution mass spectrometry, respectively. Compounds 1, 2, 3 and 4 were iden...
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