A preparation method of ebony extract and its quality detection method
A quality detection method and extract technology, which is applied in the field of preparation of ebony extract, can solve problems such as difficult to unify limits, inconsistent expression of content determination limits, uneven quality residuals, etc., and achieve the effect of stable preparation process
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Embodiment 1
[0046]The preparation method of ebony extract: S1, take 100g of ebony, weigh it, put it in a casserole, decoct the medicinal liquid 6 times the amount of water added, add it to the decoction pot, decoct for 30min, filter it while it is hot with a 300-mesh standard sieve, and put the filtrate in a water bath Cooling; adding 10 times the amount of water to the dregs and decocting for 20 minutes, filtering while hot with a standard sieve of 200 mesh, combining the two filtrates, cooling the filtrate in a water bath to 65°C and then concentrating; concentrating the filtrate to an appropriate amount under reduced pressure, and placing it in a freeze dryer. Freeze-dry to obtain the ebony extract.
[0047] Preferably, a rotary evaporator is used for concentration under vacuum and reduced pressure (vacuum degree: -0.085~-0.090MPa), the concentration temperature is 65°C, the concentration is 1 to 2 hours to a suitable volume, and the specific gravity of the concentrated solution is 1.04...
Embodiment 2
[0053] The preparation process of ebony extract, according to figure 2 (1) Weigh 3 parts of ebony plums, each about 100g, add 8 times of water for the first decoction, add 6 times of water for the second decoction, and start decocting after soaking for 30 minutes. The first frying is to turn on the strong fire (500w), after boiling, adjust to the slow fire and cook for 30 minutes. While hot, separate 200 mesh filter cloths. The second frying (200w), after boiling, adjust to a slow fire and cook for 25 minutes respectively. While hot, separate 200 mesh filter cloths. Combine the decoctions under the same mesh number, concentrate the decoction at 65°C, and then take samples to measure the yield of extract and the transfer rate of citric acid. The results are shown in the table: Take 100g of ebony plum, weigh it, put it in a casserole, add 8 times of water to soak for 30 minutes, and then start decocting. First boil on high fire (500W), then decoct on slow fire (200W) for 30...
Embodiment 3
[0062] The establishment of embodiment 3 citric acid content determination analytical method
[0063] (1) Source and purity check of reference substance
[0064] The citric acid reference substance (No. 100396-201603) was purchased from China National Institutes for Food and Drug Control for content determination. The content was calculated as 100%, and it was dried at 105°C for 2 hours before use. In the experiment, the full wavelength of citric acid was scanned, and its ultraviolet absorption diagram was recorded. The results can be seen from the figure: citric acid is the terminal absorption, and the detection wavelength is 210nm.
[0065] (2) Chromatographic conditions
[0066] Octadecylsilane-bonded silica gel was used as filler; acetonitrile-0.5% ammonium dihydrogen phosphate solution (3:97) (adjusted to pH 3.0 with phosphoric acid) was used as mobile phase. The number of theoretical plates calculated by citric acid should not be less than 7000.
[0067] (3) Preparati...
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