A kind of preparation method of ambrette lactone
A technology of ambride and bacterial strain, applied in the field of flavors and fragrances, can solve the problems of harsh synthesis conditions, difficulty in mass production of ambride, long synthesis steps, etc., and achieves simple and convenient preparation process, low product cost, Source-rich effects
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Embodiment 1
[0027] Embodiment 1: the cultivation of Sophora japonica for many years
[0028] Strain: The medicinal fungus Perenniporia robiniophila (Murrill) Rvarden is isolated and purified from the fruiting body of the wild Robinia pseudoacacia growing on the living tree of Robinia pseudoacacia, belonging to the fungus Higher fungi of the genus Perenniporia in the polyporaceae Polyporaceae.
[0029] Culture conditions: Based on the comprehensive potato medium (CPDA medium) as the base medium, the carbon source (glucose, sucrose, maltose, soluble starch and corn starch), nitrogen source (yeast extract , peptone, beef extract, urea and ammonium sulfate), potassium dihydrogen phosphate, magnesium sulfate, vitamin B1, pH value, culture time and culture temperature, etc. The best culture conditions are: 200 grams of potatoes, 20 grams of sucrose, 20 grams of yeast extract, 15 grams of agar, 2 grams of magnesium sulfate, 3 grams of potassium dihydrogen phosphate, 0.01 grams of vitamin B1, ad...
Embodiment 2
[0031] Embodiment 2: the preparation of Sophora japonica Absolute Oil
[0032] Under stirring at room temperature, the total culture material obtained in Example 1 was fully extracted with 5 times of ethanol for 3 times, each time for 24 hours, and filtered. The filtrates were combined, cooled to about 0°C, filtered off after the precipitation was complete, and the filtrate was concentrated under reduced pressure below 50°C to recover ethanol to obtain a crude paste.
[0033] After dissolving the crude paste with petroleum ether, wash away free acid with 5% aqueous sodium bicarbonate solution or 5% aqueous sodium carbonate solution or 1% aqueous sodium hydroxide solution, then wash with saturated saline until neutral, separate the water layer to obtain petroleum ether extraction liquid.
[0034] The petroleum ether extract is dehydrated and dried with anhydrous sodium sulfate or anhydrous magnesium sulfate, and concentrated under reduced pressure below 50°C to recover petrole...
Embodiment 3
[0036] Embodiment 3: the separation and purification of ambrette lactone
[0037] The absolute oil was purified by silica gel column chromatography, petroleum ether-ethyl acetate (100:0-90:10, v / v) gradient elution, traced by thin-layer chromatography, and a colorless oily ambrette lactone was obtained. Its spectral data are as follows:
[0038] 1 H NMR (400MHz, CDCl 3 ): δ5.32(t, 2H, J=4.6Hz, H-8, 9), 4.13(t, 2H, J=5.4Hz, H-17), 2.32(t, 2H, J=6.4Hz, H -3), 2.05(m, 4H, H-7, 10), 1.63(m, 4H, H-6, 11), 1.33(m, 14H, H-4, 5, 12, 13, 14, 15, 16).
[0039] 13 C NMR (100MHz, CDCl 3 ): δ174.05 (s, C-2), 130.31 (d, C-8 or C-9), 130.15 (d, C-9 or C-8), 63.82 (t, C-17), 34.64 ( t, C-3), 29.52(t, C-7 or C-10), 28.90(t, C-10 or C-7), 28.81(t), 28.62(t), 28.56(t), 28.47( t), 27.76(t), 27.05(t), 26.91(t), 25.43(t), 25.37(t) (C-4, 5, 12, 13, 14, 15, 16).
[0040] EI-MS (m / z): 252[M] + .
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