Preparation method of polyphyllin II and polyphyllin VII
A technology of Chonglou saponin and Yunnan Chonglou, applied in steroids, organic chemistry, etc., can solve the problems of separation and purification of Chonglou steroidal saponin monomer compounds, difficulty in purification, and limitation of new drug research and development potential.
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Embodiment 1
[0027] The extraction method of papaya saponin II and VII of the present invention:
[0028] After the dry peel (0.50 g) of Paprika dianthus is crushed, it is extracted with water, 90% ethanol or absolute ethanol, and ultrasonically extracted. The extraction time is 30-120 minutes, and the extraction temperature is 25°C-60°C. Under different extraction conditions, the detected contents of papaya saponin II and papaya saponin VII are shown in Table 1. After filtering the extract, evaporate to dryness below 60°C to obtain the crude extract (0.14-0.27 g) of the pericarp of Papaya dianthus.
[0029] Table 1. Content comparison of papaya saponin II and papaya saponin VII in different extraction methods
[0030]
[0031] Note: The content of papaya saponin II and papaya saponin VII is calculated according to the dry matter of the extracted raw materials
Embodiment 2
[0033] The enrichment method of papaya saponin II and VII of the present invention:
[0034] Method 1: Take 6.85g of the crude extract of the pericarp of Parisia diangi, add 100mL of water to make a suspension, and extract it with 100mL of ethyl acetate and n-butanol for 5 times respectively. After the extract was concentrated, an ethyl acetate extract (0.41 g) and an n-butanol extract (3.22 g) were obtained, respectively. The fraction extracted with n-butanol was chromatographed on a Sephadex LH-20 gel column and eluted with methanol to obtain fractions (1.50 g) rich in saponins II and VII.
[0035] Method 2: take 500 g of the crude extract of the pericarp of Pachyphyllum yunnanensis, go through D101 macroporous resin chromatography, and elute with water, 80% ethanol, 95% ethanol and acetone, respectively. Among them, 80% ethanol eluted part was concentrated to obtain 150 g of eluate. Take 10 g of 80% ethanol eluent, add 100 mL of water to make a suspension, and sequentiall...
Embodiment 3
[0037] Separation and purification method of papaya saponin II and VII of the present invention:
[0038] Method 1: Take 1.50 g of the part rich in papaya saponin II and VII in method 1 of Example 2, and pass it through preparative HPLC (YMC-Pack, ODS-A chromatographic column, diameter 250×20mm, 5μm; flow rate v=8.0mL / min; eluent: 0~15min, methanol-water, 87:13; 15~30min, methanol-water, 90:10) to prepare the compound papaya saponin VII (156.0mg, t R =12.943min) and papaya saponin II (145.8mg, t R = 24.010 min).
[0039] Method 2: Take 164.6 mg of the part rich in papaya saponin II and VII in method 2 of Example 2, and pass through preparative HPLC (YMC-Pack, ODS-A chromatographic column, diameter 250×20mm, 5μm; flow rate v=8.0mL / min; the eluent is methanol-water, 90:10) to prepare compound saponin VII (24.4mg, t R =11.520min) and papaya saponin II (27.1mg, t R = 21.320 min).
[0040] Method 3: Take 150.3 mg of the part rich in papaya saponin II and VII in method 2 of Exa...
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