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浅析乙醇提取龙眼核总黄酮及鉴别新研究
to, lays aside in the 250ml measuring flask, dilutes with 60% ethyl alcohol to the scale division, results in the sample fluid.
2.2 Determinations methods restOn take the grass cutter as the comparison determination longan seed in the total flavanone content, joins the aluminum ion reagent, at the same time controls is suitable the pH value, causes the flavanone compound and the aluminum salt forms the complex compound, can obtain the stable characteristic absorption peak in the visible light area.
2.3 Quantitative experiments total flavanone content determination
2.3.1 Wave lengths choiceSample fluids right amount, in under the 0.30ml 5% sodium nitrite solution existence alkalinity condition, after the aluminium nitrate coloration, attracts the luminosity take the reagent as the spatial dried ginseng compared to the fluid in the 420~700nm wavelength range determination chelate, the chelate has the biggest absorption in the 510nm wave length place, when determines selects this wave length.
2.3.2 Standard curves plan distinctionsPrecisely absorb the grass cutter to compare the fluid (0.10mg/ml) 0.00, 0.50, 1.00, 2.00, 3.00, 4.00, 5.00ml in the 10.00ml measuring flask, joins 5% sodium nitrite solution 0.30ml separately, swings uniform, settles 6min; Again adds 10% aluminium nitrate solution 0.30ml, swings uniform, settles 6min; Again adds 4% caustic soda solution 4.00ml, dilutes with 60% ethyl alcohol to the scale division, swings uniform, settles 12min, makes the blank by the reagent, absorbance was determinated at 510nm place. determination result of absorbance to see Table 1.
Table 1 determination of absorbance by ultraviolet visible spectrophotometer （略）
Results in the regression equation according to on table: A=-2.208×10-2+13.7578C，r=0.9999.
2.3.3 Withdrawing content determinationPrecise absorption sample fluid 1.00ml, sets at the 10.00ml measuring flask, absorbance A=1.102, according to the standard curve preparation method determination, according to regression equation: A=-2.208×10-2+13.7578C, in computation sample total flavanone content C=1.634mg/ml.
2.3.4 Recyclings experimentsPrecise quantity sample fluid 1.00ml, joins standard grass cutter comparison 2.00ml (0.10mg/ml), attracts the luminosity with the front sample determination method operation determination, extracts the returns-ratio is 99.65%.
2.4 Qualitative experimental total flavanone distinction
2.4.1 Colors respondedUnder the ultraviolet ray assumes the color response: Takes this sample solution on the filter paper, assumes the yellow under the visible light, assumes the dust color under the ultraviolet ray and has the fluorescence spot.Strong ammonia water response that, Takes this sample solution on the filter paper, smokes the filter paper above the ammonia water 0.5min, observes immediately under the ultraviolet ray, assumes the extremely obvious tan fluorescence spot.Aluminum trichloride response that, The sample solution on the filter paper, adds by drops 1% aluminum trichloride ethyl alcohol solution, air-dries. Assumes the yellow under the visible light, assumes the decadent fluorescence spot under the ultraviolet ray.Magnesium acetate response that, The sample solution on the filter paper, adds by drops 1% magnesium acetate methyl alcohol solution, air-dries, under the ultraviolet ray assumes the decadent spot.The hydrochloric acid - magnesium powder responded that, Takes the ethyl alcohol to extract 1ml to add the magnesium powder in the test tube, again joins the thick hydrochloric acid number drop (1 time to join), assumes the purple red in the froth place.
2.4.2 Paper chromatographicAnalyses sample solution 10 ml on filter paper. With normal butyl alcohol: Acetic acid: Water =4: 1: 5 for launches the medicinal preparation, previous line launches 5h, takes out air dries. Spurts 1% aluminum chloride ethyl alcohol solution. After air-dries under the ultraviolet ray, obviously fluorescence spot.
3 Discussions
3.1 Experimental results indicated that, this experimental technique craft simple, the returns-ratio is 99.65%, the extraction efficiency is higher than the traditional method, the ultrasonic wave which use this article provides withdraws, yellow ketones matter its purity which the purification method but obtains is high. The ultrasonic wave may strengthen the ethyl alcohol to soak the formulation, achieved time-saving, is highly effective, the energy conservation goal, this method uses the entire physical process, does not have any pollution, is ideal withdraws the yellow ketones matter the way, has the broad application prospect.
3.2 Flavonoid are big kind of natural products, widely exists in the vegetable kingdom, is many Chinese medicine effective components, has the very high for medicinal purposes value. In the nature most common is the flavanone and the flavonol, other yellow (are mellow), the isoflavone including the double hydrogen, the double flavanone, the flavanol, looks up your alkone, the orange alkone, the variety glucoside and the new yellow ketones and so on［6］. The natural origin biological flavanone molecular weight is small, can by the human body rapid absorption, be able through the blood brain barrier, to be able to enter the fatty tissue, then manifests the following function: Eliminates weary, protects the blood vessel, guards against the arteriosclerosis, the expansion blood capillary, dredges the microcycle, the anti-fat oxidation, anti-is senile, activates the cerebrum and other internal organs cells functions.The flavonoid has the anti-cancer, the anti-tumor, anti-heart blood vessel of brain disease, the anti- inflammation analgesia, the immunity adjustment, falls the blood sugar, treatment osteoporosis, the bacteriostasis anti-virus
2.2 Determinations methods restOn take the grass cutter as the comparison determination longan seed in the total flavanone content, joins the aluminum ion reagent, at the same time controls is suitable the pH value, causes the flavanone compound and the aluminum salt forms the complex compound, can obtain the stable characteristic absorption peak in the visible light area.
2.3 Quantitative experiments total flavanone content determination
2.3.1 Wave lengths choiceSample fluids right amount, in under the 0.30ml 5% sodium nitrite solution existence alkalinity condition, after the aluminium nitrate coloration, attracts the luminosity take the reagent as the spatial dried ginseng compared to the fluid in the 420~700nm wavelength range determination chelate, the chelate has the biggest absorption in the 510nm wave length place, when determines selects this wave length.
2.3.2 Standard curves plan distinctionsPrecisely absorb the grass cutter to compare the fluid (0.10mg/ml) 0.00, 0.50, 1.00, 2.00, 3.00, 4.00, 5.00ml in the 10.00ml measuring flask, joins 5% sodium nitrite solution 0.30ml separately, swings uniform, settles 6min; Again adds 10% aluminium nitrate solution 0.30ml, swings uniform, settles 6min; Again adds 4% caustic soda solution 4.00ml, dilutes with 60% ethyl alcohol to the scale division, swings uniform, settles 12min, makes the blank by the reagent, absorbance was determinated at 510nm place. determination result of absorbance to see Table 1.
Table 1 determination of absorbance by ultraviolet visible spectrophotometer （略）
Results in the regression equation according to on table: A=-2.208×10-2+13.7578C，r=0.9999.
2.3.3 Withdrawing content determinationPrecise absorption sample fluid 1.00ml, sets at the 10.00ml measuring flask, absorbance A=1.102, according to the standard curve preparation method determination, according to regression equation: A=-2.208×10-2+13.7578C, in computation sample total flavanone content C=1.634mg/ml.
2.3.4 Recyclings experimentsPrecise quantity sample fluid 1.00ml, joins standard grass cutter comparison 2.00ml (0.10mg/ml), attracts the luminosity with the front sample determination method operation determination, extracts the returns-ratio is 99.65%.
2.4 Qualitative experimental total flavanone distinction
2.4.1 Colors respondedUnder the ultraviolet ray assumes the color response: Takes this sample solution on the filter paper, assumes the yellow under the visible light, assumes the dust color under the ultraviolet ray and has the fluorescence spot.Strong ammonia water response that, Takes this sample solution on the filter paper, smokes the filter paper above the ammonia water 0.5min, observes immediately under the ultraviolet ray, assumes the extremely obvious tan fluorescence spot.Aluminum trichloride response that, The sample solution on the filter paper, adds by drops 1% aluminum trichloride ethyl alcohol solution, air-dries. Assumes the yellow under the visible light, assumes the decadent fluorescence spot under the ultraviolet ray.Magnesium acetate response that, The sample solution on the filter paper, adds by drops 1% magnesium acetate methyl alcohol solution, air-dries, under the ultraviolet ray assumes the decadent spot.The hydrochloric acid - magnesium powder responded that, Takes the ethyl alcohol to extract 1ml to add the magnesium powder in the test tube, again joins the thick hydrochloric acid number drop (1 time to join), assumes the purple red in the froth place.
2.4.2 Paper chromatographicAnalyses sample solution 10 ml on filter paper. With normal butyl alcohol: Acetic acid: Water =4: 1: 5 for launches the medicinal preparation, previous line launches 5h, takes out air dries. Spurts 1% aluminum chloride ethyl alcohol solution. After air-dries under the ultraviolet ray, obviously fluorescence spot.
3 Discussions
3.1 Experimental results indicated that, this experimental technique craft simple, the returns-ratio is 99.65%, the extraction efficiency is higher than the traditional method, the ultrasonic wave which use this article provides withdraws, yellow ketones matter its purity which the purification method but obtains is high. The ultrasonic wave may strengthen the ethyl alcohol to soak the formulation, achieved time-saving, is highly effective, the energy conservation goal, this method uses the entire physical process, does not have any pollution, is ideal withdraws the yellow ketones matter the way, has the broad application prospect.
3.2 Flavonoid are big kind of natural products, widely exists in the vegetable kingdom, is many Chinese medicine effective components, has the very high for medicinal purposes value. In the nature most common is the flavanone and the flavonol, other yellow (are mellow), the isoflavone including the double hydrogen, the double flavanone, the flavanol, looks up your alkone, the orange alkone, the variety glucoside and the new yellow ketones and so on［6］. The natural origin biological flavanone molecular weight is small, can by the human body rapid absorption, be able through the blood brain barrier, to be able to enter the fatty tissue, then manifests the following function: Eliminates weary, protects the blood vessel, guards against the arteriosclerosis, the expansion blood capillary, dredges the microcycle, the anti-fat oxidation, anti-is senile, activates the cerebrum and other internal organs cells functions.The flavonoid has the anti-cancer, the anti-tumor, anti-heart blood vessel of brain disease, the anti- inflammation analgesia, the immunity adjustment, falls the blood sugar, treatment osteoporosis, the bacteriostasis anti-virus
