CN101225080A - Method for extracting flavone from sea-buckthorn leaves and feed stuff containing the same - Google Patents
Method for extracting flavone from sea-buckthorn leaves and feed stuff containing the same Download PDFInfo
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- CN101225080A CN101225080A CNA2008100639170A CN200810063917A CN101225080A CN 101225080 A CN101225080 A CN 101225080A CN A2008100639170 A CNA2008100639170 A CN A2008100639170A CN 200810063917 A CN200810063917 A CN 200810063917A CN 101225080 A CN101225080 A CN 101225080A
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Abstract
The invention relates to an extraction method and forage of flavone, in particular to a method of extracting flavone from sea buckthorn leaves and to the forage containing flavone, solving the complicated method, low yield, organic solvent residue and much addition when sea buckthorn leaves are taken as forage addition in the prior method of extracting flavone from sea buckthorn leaves. The method of the invention comprises 1 to wash, remove the impurity, dry and grind the sea buckthorn leaves; 2 to extract the flavone by CO<SUB>2</SUB> super-critical method; 3 elution and vacuum dry. The forage comprises corn, soybean meal, fish meal, soya-bean oil, table salt, calcium hydrogen phosphate, methionine, choline chloride, multi-dimensional, microelements, stone powder and flavone. The extraction method and forage of flavone has the advantages of having easy operation, completing the extraction at one time without organic solvent residue, with extraction rate up to 98%, total yield up to 5%, easily realizing industrialization, having high content of active ingredient of flavone over 50%, addition of flavone of 0.01% to 1% in the forage, increasing the utilization rate of protein and other advantages.
Description
Technical field
The present invention relates to a kind of extracting method and feed, specifically is the method for Folium Hippophae extraction flavones and the feed that contains flavones.
Background technology
Sea-buckthorn belongs to the Elaeangnaceae hippophae plant, is comprehensive wild bush of a kind of nutritive ingredient or dungarunga, contains abundant biologically active substance, multivitamin and trace element, and does not have chemical pollution, has edible widely and pharmaceutical use.
Yet the complex process of extracts active ingredients in the existing Folium Hippophae, active constituent content is no more than 10% in the extract that is obtained, and yield only is 1.05%, and has problems such as organic substance is residual.In addition, sea-buckthorn is as in the applied research process of fodder additives in herding is produced, and addition is greater than 5%, and the specific aim of application is not strong.
Summary of the invention
The present invention is low for flavones extracting method complexity, the yield that solves in the Folium Hippophae, and organic solvent residual and Folium Hippophae are as the excessive problem of fodder additives addition, and a kind of feed that from Folium Hippophae, extracts the method for flavones and contain flavones that proposes.The present invention adopts CO
2Supercritical methanol technology has solved the extraction process complexity, yield is low, and solvent has residual, and the excessive problem of fodder additives addition.
The present invention makes by following step: one, Folium Hippophae is cleaned impurity elimination, drying and crushing is also crossed 30~60 mesh sieves; Two, adopt CO
2Supercritical methanol technology extracting flavone, wherein processing parameter: extracting pressure is 10~50MPa, and extraction temperature is 10~70 ℃, and separating pressure is 1~10MPa, and separation temperature is 15~75 ℃, control CO
2Flow is 100~200L/min, and the extraction time is 0.5~5h; Three, the fluent meterial after will extracting with the X-5 resin absorption after, use ethanol elution again, be dry 1~6h under 0.002~0.1MPa, 30~70 ℃ the condition in vacuum tightness.
The present invention is easy and simple to handle, and extraction process is disposable to be finished and the organic solvent-free residue problem.The present invention extracts flavones from Folium Hippophae extraction rate reached is more than 98%, and total yield is easy to realize industrialization up to 5%.
Containing the feed that the present invention extracts flavones is made up of 50~65 parts of corns, 30~40 parts of dregs of beans, 1~5 part of fish meal, 2~5 parts of soya-bean oil, 0.2~0.5 portion of salt, 1~2 part of secondary calcium phosphate, 0.05~0.5 part of methionine(Met), 0.1~0.3 part of choline chloride 60,0.01~0.04 part of compound vitamin, 0.1~0.5 part of trace element, 1~6 part of stone flour and 0.01~1 part of flavones by ratio of weight and the number of copies.
Described compound vitamin is by vitamin A, vitamins D, vitamin-E, vitamin K, vitamins B
12, a kind of or wherein several combination in the vitamin H, folic acid, nicotinic acid, pantothenic acid, pyridoxol, riboflavin, VitB1.Described trace element is by combination a kind of or wherein several in copper, iodine, iron, manganese, selenium and the zinc.
The active constituent content of the flavones in the feed of the present invention is up to more than 50%, and the flavones addition is 0.01%~1%.Contrast according to experiment: feed feed of the present invention after 8 weeks, the average growth rate of fryer has improved 4.5%~7.69%; Protein utilization has on average improved 14.12%~21.65%; Calcium utilization has on average improved 11.3%~32.7%; Dressing percentage has on average improved 11.91%~23.85%; Abdomen fat rate has on average reduced by 41.6%~30.4%; Yellowish pink has on average improved 36.3%~82.6%; Drip loss has on average reduced by 60.53%~34.32%; Shearing force has on average reduced by 25.4%~42.8%; Diameter of muscle fiber has on average reduced by 32.78%~66.3%; Muscle protein has on average improved 10.6%~13.08%.
Embodiment
Embodiment one: present embodiment is extracted flavones from Folium Hippophae method is: one, Folium Hippophae is cleaned impurity elimination, drying and crushing is crossed 30~60 mesh sieves; Two, adopt CO
2Supercritical methanol technology extracting flavone, wherein processing parameter: extracting pressure is 10~50MPa, and extraction temperature is 10~70 ℃, and separating pressure is 1~10MPa, and separation temperature is 15~75 ℃, control CO
2Flow is 100~200L/min, and the extraction time is 0.5~5h; Three, the fluent meterial after will extracting with the X-5 resin absorption after, use ethanol elution again, be dry 1~6h under 0.002~0.1MPa, 30~70 ℃ the condition in vacuum tightness.
Embodiment two: the difference of present embodiment and embodiment one is that drying and crushing is also crossed 40~50 mesh sieves in the step 2.Other is identical with embodiment one.
Embodiment three: the difference of present embodiment and embodiment one is that drying and crushing is also crossed 45 mesh sieves in the step 2.Other is identical with embodiment one.
Embodiment four: the difference of present embodiment and embodiment one is that extracting pressure is 20~40MPa in the step 2, and extraction temperature is 20~60 ℃.Other is identical with embodiment one.
Embodiment five: the difference of present embodiment and embodiment one is that extracting pressure is 25~35MPa in the step 2, and extraction temperature is 35~50 ℃.Other is identical with embodiment one.
Embodiment six: the difference of present embodiment and embodiment one is that extracting pressure is 35MPa in the step 2, and extraction temperature is 45 ℃.Other is identical with embodiment one.
Embodiment seven: the difference of present embodiment and embodiment one is that the step 2 separating pressure is 1~10MPa, and separation temperature is 15~75 ℃.Other is identical with embodiment one.
Embodiment eight: the difference of present embodiment and embodiment one is that separating pressure is 3~7MPa in the step 2, and separation temperature is 30~60 ℃.Other is identical with embodiment one.
Embodiment nine: the difference of present embodiment and embodiment one is that extracting pressure is 5MPa in the step 2, and extraction temperature is 45 ℃.Other is identical with embodiment one.
Embodiment ten: the difference of present embodiment and embodiment one is CO in the step 2
2Flow is 120~170L/min.Other is identical with embodiment one.
Embodiment 11: the difference of present embodiment and embodiment one is CO in the step 2
2Flow is 130~150L/min.Other is identical with embodiment one.
Embodiment 12: the difference of present embodiment and embodiment one is CO in the step 2
2Flow is 145L/min.Other is identical with embodiment one.
Embodiment 13: the feed that contains flavones in the present embodiment is made up of 50~65 parts of corns, 25~40 parts of dregs of beans, 1~5 part of fish meal, 2~5 parts of soya-bean oil, 0.2~0.5 portion of salt, 1~2 part of secondary calcium phosphate, 0.05~0.5 part of methionine(Met), 0.1~0.3 part of choline chloride 60,0.01~0.04 part of compound vitamin, 0.1~0.5 part of trace element, 1~6 part of stone flour and 0.01~1 part of flavones by ratio of weight and the number of copies.
Compound vitamin is by vitamin A, vitamins D, vitamin-E, vitamin K, vitamins B in the present embodiment
12, a kind of or wherein several combination in the vitamin H, folic acid, nicotinic acid, pantothenic acid, pyridoxol, riboflavin, VitB1.Trace element is by combination a kind of or wherein several in copper, iodine, iron, manganese, selenium and the zinc.
The feed making method of present embodiment is as follows: with flavones divide 3~10 times with dregs of beans or stone flour according to above-mentioned ratio of weight and number mixing, make feed pre-mixing material; Again with feed pre-mixing material and other feedstuff raw material mixings.
Embodiment 14: the difference of present embodiment and embodiment 13 is that feed is made up of 53~62 parts of corns, 28~38 parts of dregs of beans, 2.5~4.5 parts of fish meal, 2.5~4 parts of soya-bean oil, 0.25~0.4 portion of salt, 1.2~1.8 parts of secondary calcium phosphates, 0.1~0.45 part of methionine(Met), 0.15~0.25 part of choline chloride 60,0.02~0.03 part of compound vitamin, 0.2~0.45 part of trace element, 1.5~5.5 parts of stone flours and 0.03~0.9 part of flavones by ratio of weight and the number of copies.Other is identical with embodiment 13.
Embodiment 15: the difference of present embodiment and embodiment 13 is that feed is made up of 55~60 parts of corns, 30~34 parts of dregs of beans, 3~4 parts of fish meal, 2.8~3.6 parts of soya-bean oil, 0.28~0.36 portion of salt, 1.65~1.74 parts of secondary calcium phosphates, 0.25~0.4 part of methionine(Met), 0.18~0.24 part of choline chloride 60,0.028 part of compound vitamin, 0.3~0.4 part of trace element, 3~5 parts of stone flours and 0.04~0.8 part of flavones by ratio of weight and the number of copies.Other is identical with embodiment 13.
Embodiment 16: present embodiment compares test, and feed and described two kinds of concrete components of feed that contain flavones of not containing flavones are as shown in table 1.
Table 1
Composition | Broiler fodder 1 | Broiler fodder 2 | Broiler fodder 3 |
Corn | 57 | 57 | 57 |
Dregs of beans | 34.5 | 34.5 | 34.5 |
Fish meal | 2 | 2 | 2 |
Soya-bean oil | 2 | 2 | 2 |
Salt | 0.3 | 0.3 | 0.3 |
Secondary calcium phosphate | 1.7 | 1.7 | 1.7 |
Methionine(Met) | 0.2 | 0.2 | 0.2 |
Choline chloride 60 | 0.1 | 0.1 | 0.1 |
Compound vitamin | 0.03 | 0.03 | 0.03 |
Trace element | 0.3 | 0.3 | 0.3 |
Stone flour | 1.87 | 1.82 | 1.37 |
Flavones | 0 | 0.05 | 0.5 |
Every part of compound vitamin is by 1500IU vitamin A, 3200IU vitamins D, 10IU vitamin-E, 0.5mg vitamin K, 0.01mg vitamins B in the present embodiment
12, 0.15mg vitamin H, 0.55mg folic acid, 30mg nicotinic acid, 10mg pantothenic acid, 3.5mg pyridoxol, 3.6mg riboflavin and 1.8mg VitB1 form; Every part of trace element is made up of 8mg copper, 0.35mg iodine, 80mg iron, 60mg manganese, 0.15mg selenium and 40mg zinc.
Adopt the feed in the present embodiment, the results are shown in Table 2 with the feed contrast effect that does not contain fodder additives of the present invention.
Table 2
Index | Broiler fodder 1 | Broiler fodder 2 | Broiler fodder 3 |
The beginning body weight | 0.42±0.01 | 0.44±0.01 | 0.44±0.02 |
8 all mean body weights | 12.20±0.57 | 12.76±0.97 | 13.09±0.42 |
Protein utilization | 47.16±5.28 | 54.01±5.34 | 57.18±6.72 |
Calcium utilization | 52.13±9.06 | 58.23±10.09 | 69.05±11.08 |
Dressing percentage | 85.17±1.97 | 94.89±2.47 | 105.10±2.95 |
Abdomen fat rate | 2.50±0.34 | 1.74±0.25 | 1.46±0.21 |
Yellowish pink | 13.87±5.27 | 18.89±6.01 | 25.19±6.22 |
Drip loss | 6.03±2.15 | 3.96±1.94 | 2.38±1.05 |
Shearing force | 3.51±0.99 | 2.63±0.57 | 2.01±0.26 |
Diameter of muscle fiber | 35.24±5.38 | 23.76±3.90 | 11.95±2.03 |
Muscle protein | 73.87±4.89 | 81.70±2.15 | 83.53±2.98 |
Associative list 2 is analyzed, and as seen the feed feed that does not contain fodder additives of the present invention and the feed experiment contrast of the present invention of feeding: feed feed of the present invention after 8 weeks, the average growth rate of fryer has improved 4.5%~7.69%; Protein utilization has on average improved 14.12%~21.65%; Calcium utilization has on average improved 11.3%~32.7%; Dressing percentage has on average improved 11.91%~23.85%; Abdomen fat rate has on average reduced by 41.6%~30.4%; Yellowish pink has on average improved 36.3%~82.6%; Drip loss has on average reduced by 60.53%~34.32%; Shearing force has on average reduced by 25.4%~42.8%; Diameter of muscle fiber has on average reduced by 32.78%~66.3%; Muscle protein has on average improved 10.6%~13.08%.
Claims (10)
1. a method of extracting flavones from Folium Hippophae is characterized in that extracting method is prepared by following step: one, Folium Hippophae is cleaned impurity elimination, drying and crushing and mistake 30~60 mesh sieves; Two, adopt CO
2Supercritical methanol technology extracting flavone, wherein processing parameter: extracting pressure is 10~50MPa, and extraction temperature is 10~70 ℃, and separating pressure is 1~10MPa, and separation temperature is 15~75 ℃, control CO
2Flow is 100~200L/min, and the extraction time is 0.5~5h; Three, the fluent meterial after will extracting with the X-5 resin absorption after, use ethanol elution again, be dry 1~6h under 0.002~0.1MPa, 30~70 ℃ the condition in vacuum tightness.
2. the method for extracting flavones from Folium Hippophae according to claim 1 is characterized in that extracting pressure is 20~40MPa in the step 2, and extraction temperature is 20~60 ℃.
3. the method for extracting flavones from Folium Hippophae according to claim 1 is characterized in that separating pressure is 3~7MPa in the step 2, and separation temperature is 30~60 ℃.
4. the method for extracting flavones from Folium Hippophae according to claim 1 is characterized in that CO in the step 2
2Flow is 120~170L/min.
5. the method for extracting flavones from Folium Hippophae according to claim 1 is characterized in that CO in the step 2
2Flow is 135~150L/min.
6. contain right and require 1 described method to extract the feed of flavones, it is characterized in that the feed that contains flavones is made up of 50~65 parts of corns, 25~40 parts of dregs of beans, 1~5 part of fish meal, 2~5 parts of soya-bean oil, 0.2~0.5 portion of salt, 1~2 part of secondary calcium phosphate, 0.05~0.5 part of methionine(Met), 0.1~0.3 part of choline chloride 60,0.01~0.04 part of compound vitamin, 0.1~0.5 part of trace element, 1~6 part of stone flour and 0.01~1 part of flavones by ratio of weight and the number of copies.
7. according to the described feed that contains flavones of claim 6, it is characterized in that the feed that contains flavones is made up of 53~62 parts of corns, 28~38 parts of dregs of beans, 2.5~4.5 parts of fish meal, 2.5~4 parts of soya-bean oil, 0.25~0.4 portion of salt, 1.2~1.8 parts of secondary calcium phosphates, 0.1~0.45 part of methionine(Met), 0.15~0.25 part of choline chloride 60,0.02~0.03 part of compound vitamin, 0.2~0.45 part of trace element, 1.5~5.5 parts of stone flours and 0.03~0.09 part of flavones by ratio of weight and the number of copies.
8. according to the described feed that contains flavones of claim 6, it is characterized in that the feed that contains flavones is made up of 55~60 parts of corns, 30~34 parts of dregs of beans, 3~4 parts of fish meal, 2.8~3.6 parts of soya-bean oil, 0.28~0.36 portion of salt, 1.65~1.74 parts of secondary calcium phosphates, 0.25~0.4 part of methionine(Met), 0.18~0.24 part of choline chloride 60,0.028 part of compound vitamin, 0.3~0.4 part of trace element, 3~5 parts of stone flours and 0.04~0.08 part of flavones by ratio of weight and the number of copies.
9. according to claim 6, the 7 or 8 described feeds that contain flavones, it is characterized in that compound vitamin is by vitamin A, vitamins D, vitamin-E, vitamin K, vitamins B
12, a kind of or wherein several combination in the vitamin H, folic acid, nicotinic acid, pantothenic acid, pyridoxol, riboflavin, VitB1.
10. according to claim 6, the 7 or 8 described feeds that contain flavones, it is characterized in that trace element is by combination a kind of or wherein several in copper, iodine, iron, manganese, selenium and the zinc.
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Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
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CN102058634A (en) * | 2011-01-04 | 2011-05-18 | 鄂尔多斯市天骄资源发展有限责任公司 | Method for extracting and purifying total flavonoids of sea buckthorn |
CN102524562A (en) * | 2011-11-16 | 2012-07-04 | 淮南市施家湖水产养殖中心 | Feed additive for improving immunity of freshwater fish and preparation method thereof |
CN108434182A (en) * | 2018-04-09 | 2018-08-24 | 内蒙古宇航人高技术产业有限责任公司 | A kind of supercritical CO2The method that fluid extraction technology extracts Leaves of Hippophae L polyphenol |
CN109497288A (en) * | 2019-01-17 | 2019-03-22 | 中国农业科学院饲料研究所 | A kind of meat chicken feed and preparation method thereof |
CN111012807A (en) * | 2020-01-03 | 2020-04-17 | 内蒙古农业大学 | Extraction method and application of seabuckthorn flavone |
NL2029910B1 (en) * | 2021-11-25 | 2023-06-15 | Univ Gansu Agricultural | Extraction method of seabuckthorn leaves extract |
-
2008
- 2008-01-25 CN CNA2008100639170A patent/CN101225080A/en active Pending
Cited By (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102058634A (en) * | 2011-01-04 | 2011-05-18 | 鄂尔多斯市天骄资源发展有限责任公司 | Method for extracting and purifying total flavonoids of sea buckthorn |
CN102058634B (en) * | 2011-01-04 | 2012-08-29 | 鄂尔多斯市天骄资源发展有限责任公司 | Method for extracting and purifying total flavonoids of sea buckthorn |
CN102524562A (en) * | 2011-11-16 | 2012-07-04 | 淮南市施家湖水产养殖中心 | Feed additive for improving immunity of freshwater fish and preparation method thereof |
CN108434182A (en) * | 2018-04-09 | 2018-08-24 | 内蒙古宇航人高技术产业有限责任公司 | A kind of supercritical CO2The method that fluid extraction technology extracts Leaves of Hippophae L polyphenol |
CN109497288A (en) * | 2019-01-17 | 2019-03-22 | 中国农业科学院饲料研究所 | A kind of meat chicken feed and preparation method thereof |
CN111012807A (en) * | 2020-01-03 | 2020-04-17 | 内蒙古农业大学 | Extraction method and application of seabuckthorn flavone |
NL2029910B1 (en) * | 2021-11-25 | 2023-06-15 | Univ Gansu Agricultural | Extraction method of seabuckthorn leaves extract |
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Open date: 20080723 |