Steroid saponin compound in siberian fritillary bulb
A technology of irbe saponins and steroidal saponins, which is applied in the field of steroidal saponins, and can solve the problem of not finding non-alkaloid components
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Embodiment 1
[0076] Example 1: Isolation of Compounds
[0077] With 2 kg of dried bulbs of Igami (Fritillaria Pallidiflora Schrenk.), the ethanol with a volume fraction of 95% was extracted three times for 3 hours each time, and the solvent consumption was 10, 10, 8, and the combined filtrate was decompressed After recovering the solvent, 89.0 g of extract was obtained. The medicinal dregs extracted with 95% ethanol were extracted three times with 70% ethanol by volume fraction for 3 hours each time, the solvent consumption was 10, 10, 8, the filtrate was combined, and the solvent was recovered under reduced pressure to obtain 98.0 g of extractum. Add appropriate amount of 2L of water to disperse the obtained extract, and extract with equal volumes of petroleum ether, chloroform, ethyl acetate, and n-butanol in sequence (each solvent is extracted three times). After recovering the solvent, 2.2 g of petroleum ether layer extract, 3.5 g of chloroform layer, 5.1 g of ethyl acetate layer, and...
Embodiment 2
[0082] Embodiment 2: identification of chemical structure
[0083] The chemical structures of the nine isolated compounds were determined by 1-dimensional and 2-dimensional nuclear magnetic resonance (1D, 2D-NMR), mass spectrometry (MS), circular dichroism (CD) and other physical and chemical methods. Its chemical structure and identification means are shown in Table 1:
Embodiment 3
[0084] Embodiment 3: HPLC-TOF-MS analysis
[0085] Configuration of the reference solution: Ibeta saponin A, Ibeta saponin B, Ibeta saponin C, Ibeta saponin D, Ibeta saponin E, Ibeta saponin F, Ibeta saponin G, Ibeta saponin H, Ibeta saponin I Precisely weigh an appropriate amount of self-made chemical reference substance, and prepare a 5 μg / ml reference substance solution with methanol.
[0086] Configuration of sample solution: Precisely weigh 5g of each Fritillaria sample, extract with 100ml chloroform Sabouraud extractor for 3 hours, recover chloroform extract, dissolve in 10ml methanol, pretreat with SPE small chromatographic column filled with ODS, 95% acetonitrile Wash with 20ml, combine methanol and 95% acetonitrile eluent, dissolve in methanol, dilute to 5ml volumetric flask, filter with 0.2μm filter membrane, and obtain.
[0087] Test method: Inject 10 μl of sample, perform HPLC-TOF-MS analysis, use the M+H peak of each compound as the selected ion to obtain the chr...
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