WO2021180117A1 - 一种包含槲皮万寿菊素的组合物 - Google Patents
一种包含槲皮万寿菊素的组合物 Download PDFInfo
- Publication number
- WO2021180117A1 WO2021180117A1 PCT/CN2021/079963 CN2021079963W WO2021180117A1 WO 2021180117 A1 WO2021180117 A1 WO 2021180117A1 CN 2021079963 W CN2021079963 W CN 2021079963W WO 2021180117 A1 WO2021180117 A1 WO 2021180117A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- marigold
- composition
- feed
- quercetin
- hydroxykaempferol
- Prior art date
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- KBPHJBAIARWVSC-XQIHNALSSA-N trans-lutein Natural products CC(=C/C=C/C=C(C)/C=C/C=C(C)/C=C/C1=C(C)CC(O)CC1(C)C)C=CC=C(/C)C=CC2C(=CC(O)CC2(C)C)C KBPHJBAIARWVSC-XQIHNALSSA-N 0.000 description 1
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Images
Classifications
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Definitions
- This application relates to an active additive, which can be applied to the fields of feed, food, health care products, medicines, cosmetics and the like.
- Feed additives refer to small or trace substances added in the process of feed production, processing and use. The amount of feed additives is small but the effect is significant. Feed additives are inevitable raw materials used in the modern feed industry. They have obvious effects on strengthening the nutritional value of basic feeds, improving animal production performance, ensuring animal health, saving feed costs, and improving the quality of livestock products. Feed additives are usually divided into nutritional additives and non-nutritive additives.
- Nutritional additives include mineral trace element additives, vitamin additives, amino acid additives, non-protein nitrogen compound additives, etc.
- Non-nutritive additives mainly include growth-promoting additives, feed preservation additives, appetite promotion and quality improvement additives, etc.
- Common appetite promotion and quality improvement additives are sodium glutamate, amaranth, carmine, lemon yellow, sunset yellow, gardenia yellow, ⁇ -carotene, amino sugars and some flavors and phagostimulants.
- Such additives can stimulate the receptors of livestock and poultry through methods such as seasoning, flavoring, and coloring, and significantly increase their appetite. They can also improve the hue of livestock and poultry products, so that poultry and egg yolks have a beautiful color.
- Antioxidants in feed are commonly used butylated hydroxytoluene, butylated hydroxymethoxybenzene, ethoxyquinoline, propyl gallate, etc.
- antioxidants can prevent fat, protein, carbohydrates and fat-soluble vitamins in feed from being Oxidation decomposes, resulting in spoilage and deterioration. Due to price and other reasons, the antioxidant used in feed is mainly ethoxyquin (Ethoxyquin or EQ). This product is currently the most widely used feed antioxidant variety at home and abroad, with good effect, low price and safe use. However, the anti-oxidant effect of ethoxyquin on oil is not ideal, and the color of the product will become darker and darker during storage. The large amount of use in the premix will affect the color of the feed.
- ethoxyquin ethoxyquin
- Querce Marigold the chemical name is 3,3,4,5,6,7-hexahydroxyflavone. It has anti-inflammatory, anti-allergic, anti-hypertensive, anti-arrhythmic, anti-platelet aggregation, anti-oxidation, anti-tumor, etc. Pharmacological effects.
- the main plant source of quercetin marigold is the extraction of compositae plants.
- Compositae plants containing quercetin marigold include marigold, maidenhair, marigold, artemisia annua, artemisia annua, yellow-top chrysanthemum, and helichrysum , Matricaria, Threadleaf chrysanthemum and Inula, etc.
- the research of quercetin marigold mainly focuses on its pharmacological activity, and it has not yet been applied in the field of food and feed additives.
- composition containing quercetin marigold has excellent antioxidant properties.
- the antioxidant performance of the composition of the present application when the amount of 2ppm-100ppm is added to the oil is equivalent to 150ppm of ethoxyquinoline (EQ) resistance. Oxidation performance.
- the feed added with the composition of the present application not only greatly improves the antioxidant effect, but also has the effects of promoting the growth of livestock and poultry and improving the meat quality of livestock and poultry.
- This application provides a composition that can be used as an additive for food, medicine, health care products, cosmetics, and feed.
- the composition is a composition containing quercetin marigold, which contains quercetin marigold and 6-hydroxykaempferol.
- the content ratio of quercetin marigold: 6-hydroxykaempferol is 100:1-43; the content ratio is preferably from 100:1-40, 100:1-35, 100:1-30 , 100:1-25, 100:1-20, 100:1-15; can be further preferably selected from 100:1-10, 100:1-9, 100:1-8, 100:1-7, 100: 1-6, 100:1-5, 100:1-4, 100:1-3, 100:1-2; 100:2-10, 100:2-9, 100:2-8, 100:2- 7,100:2-6, 100:2-5, 100:2-4, 100:2-3; 100:3-10, 100:3-9, 100:3-8, 100:3-7, 100: 3-6, 100: 3-5, 100, 3-4; 100: 4-10, 100: 4-9, 100: 4-8, 100: 4-7, 100: 4-6, 100: 4-5; 100:5-10, 100:5-9, 100:5-8, 100:5-7, 100:5-6; 100:6-10, 100:6-9, 100:6- 8,100:6-7
- compositions containing quercetin marigold which is characterized in that it contains quercetin marigold, and also contains 6-hydroxykaempferol and marigold.
- the content ratio of quercetin marigold: 6-hydroxykaempferol is 100:1-43; preferably from 100:1-40, 100:1-35, 100:1-30, 100:1 -25, 100:1-20, 100:1-15; can be further preferably selected from 100:1-10, 100:1-9, 100:1-8, 100:1-7, 100:1-6, 100:1-5, 100:1-4, 100:1-3, 100:1-2; 100:2-10, 100:2-9, 100:2-8, 100:2-7, 100: 2-6, 100:2-5, 100:2-4, 100:2-3; 100:3-10, 100:3-9, 100:3-8, 100:3-7, 100:3- 6,100:3-5,100,3-4; 100:4-10, 100:4-9, 100:4-8, 100:4-7, 100:4-6, 100:4-5; 100:5-10, 100:5-9, 100:5-8, 100:5-7, 100:5-6; 100:6-10, 100:6-9, 100:6-8, 100: 6-7; 100:7
- the present invention also relates to the application of the composition containing quercetin marigold, which is used as an additive component of food, medicine, health care products, cosmetics and feed.
- the composition is applied in feed.
- the composition enables the feed to have the effects of promoting the growth of livestock and poultry and reducing the feed-to-meat ratio.
- the present invention also relates to the application of the composition containing quercetin marigold, which is used as an additive component of food, medicine, health care products, cosmetics and feed.
- the composition is used as an antioxidant.
- the application also provides a feed.
- the raw materials of the feed include any one or more selected from the group consisting of oil, protein, vitamins, pigments, and carbohydrates, and the above-mentioned composition containing quercetin marigold.
- the oil is selected from vegetable oil or animal oil;
- the vegetable oil is selected from soybean oil, cottonseed oil, sunflower oil, peanut oil, olive oil, sesame oil, palm oil, corn oil, etc., and the animal oil is selected from lard, Butter, sheep oil, fish oil, etc.;
- the protein is vegetable protein or animal protein, including but not limited to fish meal, soy protein, and gluten;
- the pigment raw materials include, but are not limited to, lutein, lycopene, capsanthin, and carrot Vitamins, curcumin, etc.;
- the vitamin raw materials include, but are not limited to, vitamin A, vitamin B, vitamin C, vitamin D, vitamin E, and their derivative esters.
- the feed is animal feed, and the animal feed includes but is not limited to chicken feed,
- the present invention also relates to an oil composition, which contains a composition containing quercetin marigold.
- the present invention also relates to a pigment composition, which contains a composition containing quercetin marigold.
- the present invention also relates to a vitamin composition, which contains a composition containing quercetin marigold.
- the present invention also relates to a protein composition, which contains a composition containing quercetin marigold.
- the present invention also relates to a carbohydrate composition, which contains a composition containing quercetin marigold.
- composition containing quercetin marigold described in this application can be used as an additive component of any food, feed, cosmetics, health care product, and medicine, as an antioxidant, growth promoter and/or quality improver.
- the application provides the use of the composition containing quercetin marigold, which includes using the composition as a feed additive, which has the effects of anti-oxidation, promoting animal growth, and reducing the ratio of animal feed to meat.
- the animals include but are not limited to broilers, laying hens, pigs, rabbits, sheep, cows, fish, cats, dogs and the like.
- composition containing quercetin marigold is obtained by extracting natural raw materials, or obtained by the ratio of each component.
- composition containing quercetin marigold described in the present application can be obtained by extracting Compositae plants, such as marigold, maidenhair, marigold, artemisia annua, artemisia annua, yellow-top chrysanthemum, helichrysum, matricaria, clematis and Xuanfuhua and so on.
- Compositae plants such as marigold, maidenhair, marigold, artemisia annua, artemisia annua, yellow-top chrysanthemum, helichrysum, matricaria, clematis and Xuanfuhua and so on.
- the flowers of the above-mentioned Compositae plants, or other processed forms of flowers, or flower meal are preferred. Other processing forms of the flowers include, but are not limited to, fermentation treatment, or granulation treatment, or drying treatment, or crushing treatment.
- the flower meal refers to flower residue after degreasing treatment.
- composition containing quercetin marigold described in the present application can be obtained by extraction by solvent extraction method, ultrasonic assisted extraction, microwave assisted extraction, supercritical carbon dioxide extraction and the like.
- the extraction solvent is selected from ethanol solvent, methanol solvent, acetone solution, ethyl acetate, methyl ethyl ketone, n-hexane, chloroform, dichloromethane and the like.
- composition containing quercetin marigold described in the present application can be obtained by further separation and purification after extraction, and the purification method includes: macroporous resin separation method, liquid-liquid extraction method, column chromatography separation method, solid-liquid separation, centrifugation Separation and so on.
- the conditions of HPLC detection are as follows: mobile phase: phase A is 1 ⁇ formic acid solution, phase B is acetonitrile, and gradient elution is used for analysis (the conditions of gradient elution are shown in Table 1); the flow rate is controlled during the elution process :0.3ml/min; Column temperature: 40°C; Chromatographic column: BEH C18 column (2.1mm ⁇ 50mm, particle size 1.7 ⁇ m); UV detector wavelength: 210-500nm; Injection volume: 0.6 ⁇ L.
- the retention time of quercetin marigold is about 4-5 min
- the retention time of 6-hydroxykaempferol is about 6-7 min
- the retention time of marigold is about 7.7-8.2 min.
- the detection conditions are as follows:
- the content of each component in the composition containing quercetin marigold described in this application is calculated by the area normalization method, and the ratio of the peak area of each component to the percentage of the total peak area is the content ratio of each component.
- composition containing quercetin marigold described in the present application when its content in oil is 2-100 ppm, has an antioxidant performance equivalent to 150 ppm of ethoxyquinoline (EQ) antioxidant performance.
- composition containing quercetin marigold has the effects of promoting animal growth, reducing the ratio of animal feed to meat, and improving meat quality.
- composition containing quercetin marigold described in the present application can be used as an additive component of any food or feed, as an antioxidant, a growth promoter and/or a quality improver.
- Example 1 is a HPLC detection chromatogram of Composition 9 prepared in Example 9;
- Example 2 is a HPLC detection chromatogram of the composition 10 prepared in Example 10;
- Figure 3 is a high performance liquid phase detection chromatogram of the composition 11 prepared in Example 11;
- Figure 4 is a high performance liquid phase detection chromatogram of the composition 12 prepared in Example 12;
- Figure 5 of the drawings is a high performance liquid phase detection chromatogram of the composition 13 prepared in Example 13;
- Figure 6 of the accompanying drawings of the specification shows the color protection effect diagram of composition 9-composition 11 on lycopene, in which (a) is a blank control group, (b) a control group after high temperature treatment, and (c) contains after high temperature treatment A sample of composition 9, (d) a sample containing composition 10 after high temperature treatment, and (e) a sample containing composition 11 after high temperature treatment.
- composition products of Examples 1-8 were prepared according to the raw materials and parts by weight in the following table
- Example 1 To Querce Marigold (parts by weight) 6-hydroxykaempferol (parts by weight) Marigold (parts by weight) Example 1 100 10 1 Example 2 100 11 3 Example 3 100 11 4 Example 4 100 12 4 Example 5 100 10 3 Example 6 100 7 3 Example 7 100 5 1 Example 8 100 5 0
- Example 6 Take 5 portions of chicken fat and butter, 100 grams each. Set the chicken oil experimental group and the butter experimental group each with 3 groups, and add the composition of Example 6 according to the addition amount of 4, 6, and 8ppm respectively; set each group of the chicken oil control group and the butter control group, with the addition amount of 150ppm Add ethoxyquin; set a blank group of chicken butter and one blank group of butter, without adding any additives. Mix each group of additives and grease evenly, place them in a 40°C thermostat, and take samples at 0, 3, 7, 14, 21, and 28 days to determine the peroxide value. The results show that Example 6 can significantly reduce the peroxidation value of fats and oils and delay the oxidation loss process of fats and oils. The antioxidant effect is equivalent to that of ethoxyquinoline 150ppm.
- Example 6 Set up experimental groups I-VI, a total of six groups, add Example 6 to the feed at 1.25, 2.5, 3.75, 5, 10, and 20 ppm, and set up a control group.
- the control group uses the same feed as the experimental group, but not The composition of Example 6 was added.
- 147 1-day-old Rose healthy broilers (half male and half female, average weight 46.7 ⁇ 2.34g) were randomly divided into 7 groups, 21 chickens in each group, fed separately according to the above supplements, and the above 7 groups of broiler chickens were studied for the whole period ( 1-42 days old) average daily feed intake, average daily weight gain, feed to meat ratio. The results show that when Example 6 is added to the feed, the feed to meat ratio can be reduced. At the same time, when the additive dosage is 3.75ppm, the feed-to-meat ratio is the lowest.
- Example 9 Use acetone to extract marigold flowers, then add water and n-hexane phase for liquid-liquid separation, acetone water phase is concentrated and filtered, the filter cake is extracted and removed with a 1:0.5 mixed solvent of n-hexane and ethyl acetate to obtain The composition of quercetin marigold, in which the quercetin marigold:6-hydroxykaempferol is 100:3, which is the composition 9.
- Example 10 Extracting maidenhair with acetone, then adding water and n-hexane for liquid-liquid separation, the acetone water phase was concentrated and filtered, the filter cake was extracted with a 1:1 mixed solvent of n-hexane and ethyl acetate to obtain a The composition of the skin marigold, in which the quercetin marigold:6-hydroxykaempferol is 100:9, which is the composition 10.
- Example 11 Using n-hexane to extract maidenhair for degreasing, the obtained maidenhair residue was extracted with methanol, concentrated and filtered, the filter cake was extracted with ethyl acetate, the extract was concentrated and dried, and then washed repeatedly with pure water 3 times to obtain The composition of quercetin marigold, wherein the ratio of quercetin marigold:6-hydroxykaempferol is 100:17, which is composition 11.
- Example 12 Using n-hexane to extract maidenhair for degreasing, the obtained maidenhair residue was extracted with ethyl acetate, the extract was concentrated and filtered, the filter cake was purified with n-hexane, and solid phase dried to obtain a combination containing quercetin marigold
- the ratio of quercetin marigold to 6-hydroxykaempferol is 100:22, and the ratio of quercetin marigold to marigold is 100:5, which is composition 12.
- Example 13 Using n-hexane to extract marigold flowers for degreasing, the obtained marigold flower meal was extracted with 67% methanol, the extract was concentrated and filtered, the filter cake was extracted and purified with ethyl acetate, the extract was concentrated and dried, and then the n-hexane was used to remove impurities , Solid-phase drying to obtain a composition containing quercetin marigold, wherein the ratio of quercetin marigold to 6-hydroxykaempferol is 100:31, and the ratio of quercetin marigold to marigold is 100:10, which is Composition 13.
- Example 14 Mix the high-purity reference substance of quercetin marigold and 6-hydroxykaempferol in proportion to obtain a composition with a ratio of quercetin marigold and 6-hydroxykaempferol of 100:32, which is the composition 14.
- Example 15 The high-purity reference substance of quercetin marigold and 6-hydroxykaempferol was mixed in proportion to obtain a composition with a ratio of quercetin marigold and 6-hydroxykaempferol of 100:42, which is the composition 15.
- Example 16 The high-purity reference substance of quercetin marigold, 6-hydroxykaempferol, and marigold was mixed in proportion to obtain a ratio of quercetin marigold and 6-hydroxykaempferol of 100:10, and quercetin marigold A composition with a ratio of chrysanthemum to marigold of 100:5 is composition 16.
- Example 17 The high-purity reference substance of quercetin marigold, 6-hydroxykaempferol, and marigold was mixed in proportions to obtain a ratio of quercetin marigold and 6-hydroxykaempferol of 100:10, and quercetin marigold A composition with a ratio of chrysanthemum to marigold of 100:28 is composition 17.
- Quercetin marigold, 6-hydroxykaempferol, marigold, composition 9-17 were prepared with absolute ethanol to prepare sample solutions with concentrations of 1, 2, 3, 4, 5, and 6 ⁇ g/ml. Then mix DPPH with absolute ethanol into a 2 ⁇ 10-4mol/L solution, accurately pipette 2 mL of blank and sample solution and mix with 2 mL of DPPH solution, and place in a water bath at 30°C in the dark for 30 minutes, and measure at a wavelength of 517 nm. Absorbance A (blank) and A sample (sample).
- Quercetin marigold, 6-hydroxykaempferol, marigold, composition 9-17 were prepared with absolute ethanol to prepare sample solutions with concentrations of 100, 150, 200, 250, and 300 ⁇ g/ml. Prepare 9mmoI/L salicylic acid-ethanol solution, 9mmol/L FeSO4 solution, 8.8mmol/L H2O2 solution. Then add different samples according to the order in the table below, and measure the absorbance at 37°C for 15 min at 510nm. Calculation method:
- Type A A background Salicylic acid-ethanol solution 1ml 1ml 1ml FeSO 4 solution 1ml 1ml 1ml Sample solution To 1ml 1ml water 12ml 11ml 12ml H 2 O 2 solution 1ml 1ml To
- composition 9 and composition 14 were added to the feed at 2, 6, 10, 100 ppm (based on active ingredients) as the experimental group, and a blank control group was set.
- 189 1-day-old Ross healthy broilers half male and half female, average weight 46.7 ⁇ 2.34g were randomly divided into 9 groups, 21 chickens in each group, fed with the same amount of feed for each of the above groups, and the above 9 groups of broilers were studied. Feed-to-weight ratio for the whole period (1-42 days old). The results are shown in Table 6 below.
- compositions 9, 10, and 11 can all delay the high temperature loss of pigment.
- the present application relates to a composition containing quercetin marigold, which contains quercetin marigold, 6-hydroxykaempferol, and can further contain marigold.
- the composition has excellent antioxidant effects and can be used as an active additive ingredient for food, medicine, health care products, cosmetics and feed. At the same time, it can play a role in promoting animal growth, reducing feed-to-meat ratio and improving meat quality in feed.
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Abstract
一种包含槲皮万寿菊素的组合物,其中包含槲皮万寿菊素、6-羟基山奈酚,进一步还可包含万寿菊素。该组合物具有优异的抗氧化效果,可作为食品、药品、保健品、化妆品和饲料的活性添加成分。同时,其在饲料中能够发挥促进动物生长,降低料肉比,改善肉质的作用。
Description
交叉引用
本申请要求2020年3月10日提交的专利名称为“一种包含槲皮万寿菊素的组合物”的第202010160134.5号中国专利申请和2021年2月26日提交的专利名称为“一种包含槲皮万寿菊素的组合物”的第202110216085.7号中国专利申请的优先权,其全部公开内容通过引用整体并入本文。
本申请涉及一种活性添加剂,可应用于饲料、食品、保健品、药品、化妆品等领域。
饲料添加剂是指在饲料生产加工、使用过程中添加的少量或微量物质,在饲料中用量很少但作用显著。饲料添加剂是现代饲料工业必然使用的原料,对强化基础饲料营养价值,提高动物生产性能,保证动物健康,节省饲料成本,改善畜产品品质等方面有明显的效果。饲料添加剂通常分为营养性添加剂和非营养性添加剂。营养性添加剂包括矿物质微量元素添加剂、维生素添加剂、氨基酸添加剂、非蛋白氮化合物添加剂等。非营养性添加剂主要包括助生长添加剂、饲料保藏添加剂、食欲促进和品质改良添加剂等。常见的食欲促进和品质改良添加剂有谷氨酸钠、苋菜红、胭脂红、柠檬黄、日落黄、栀子黄、β-胡萝卜素、氨基糖类及一些香精、诱食剂等。这类添加剂通过对饲料调味、增香、着色等方法,刺激畜禽的感受器官,显著提高其食欲,又可改进畜禽产品的色调,使禽肉、蛋黄具有美观的色泽。饲料中的抗氧化常用的有丁羟基甲苯、丁羟甲氧基苯、乙氧基喹啉、没食子酸丙酯等,这些抗氧化剂能防止饲料中的脂肪、蛋白、碳水化合物及脂溶性维生素被氧化分解以致腐败变质。由于价格等原因用于饲料的抗氧化剂主要是乙氧基喹啉(Ethoxyquin或缩写EQ),该产品是目前 国内外使用最广泛的饲料抗氧化剂品种,效果好、价格低、使用安全。但乙氧基喹啉对油脂的抗氧化效果不甚理想,并且产品在储存过程中其色泽会愈变愈深,在预混料中大量使用会影响到饲料的色泽。
槲皮万寿菊素,化学名称为3,3,4,5,6,7-六羟基黄酮,具有抗炎、抗过敏,降血压、抗心律失常、抗血小板凝聚,抗氧化,抗肿瘤等重要的药理作用。此外,槲皮万寿菊素的主要植物来源为菊科植物的提取,含有槲皮万寿菊素的菊科植物包括万寿菊、孔雀草、金盏花、黄花蒿、万年蒿、黄顶菊、蜡菊、母菊、线叶菊和旋复花等。目前槲皮万寿菊素的研究主要集中在其药理活性方面,还尚未被应用于食品、饲料添加剂领域。
本申请发现包含槲皮万寿菊素的组合物具有优异的抗氧化性能,在油脂中本申请组合物加入量2ppm-100ppm时的抗氧化性能,相当于150ppm的乙氧基喹啉(EQ)抗氧化性能。添加本申请组合物的饲料,除了抗氧化效果大大提高外,还具有促进畜禽生长、改善畜禽肉质的作用。
发明内容
本申请提供了一种可作为食品、药品、保健品、化妆品和饲料等的添加剂的组合物。
所述组合物为含槲皮万寿菊素的组合物,该组合物中包含槲皮万寿菊素,还包含6-羟基山奈酚。
所述组合物中,槲皮万寿菊素:6-羟基山奈酚的含量比例为100:1-43;所述含量比例优选自100:1-40,100:1-35,100:1-30,100:1-25,100:1-20,100:1-15;还可进一步优选自100:1-10,100:1-9,100:1-8,100:1-7,100:1-6,100:1-5,100:1-4,100:1-3,100:1-2;100:2-10,100:2-9,100:2-8,100:2-7,100:2-6,100:2-5,100:2-4,100:2-3;100:3-10,100:3-9,100:3-8,100:3-7,100:3-6,100:3-5,100,3-4;100:4-10,100:4-9,100:4-8,100:4-7,100:4-6,100:4-5;100:5-10,100:5-9,100:5-8,100:5-7,100:5-6;100:6-10,100:6-9, 100:6-8,100:6-7;100:7-10,100:7-9,100:7-8;100:8-10,100:8-9;100:9-10。
本发明另一方面,涉及一种包含槲皮万寿菊素的组合物,其特征在于包含槲皮万寿菊素,还包含6-羟基山奈酚、万寿菊素。
所述组合物中,槲皮万寿菊素:6-羟基山奈酚的含量比例为100:1-43;优选自100:1-40,100:1-35,100:1-30,100:1-25,100:1-20,100:1-15;还可进一步优选自100:1-10,100:1-9,100:1-8,100:1-7,100:1-6,100:1-5,100:1-4,100:1-3,100:1-2;100:2-10,100:2-9,100:2-8,100:2-7,100:2-6,100:2-5,100:2-4,100:2-3;100:3-10,100:3-9,100:3-8,100:3-7,100:3-6,100:3-5,100,3-4;100:4-10,100:4-9,100:4-8,100:4-7,100:4-6,100:4-5;100:5-10,100:5-9,100:5-8,100:5-7,100:5-6;100:6-10,100:6-9,100:6-8,100:6-7;100:7-10,100:7-9,100:7-8;100:8-10,100:8-9;100:9-10。所述组合物中,槲皮万寿菊素:万寿菊素的含量比例为100:1-40;优选自100:1-35,100:1-30,100:1-25,100:1-20,100:1-15,100:1-10,100:1-5。
本发明还涉及包含槲皮万寿菊素的组合物的应用,该组合物作为食品、药品、保健品、化妆品和饲料的添加成分。优选的,所述组合物在饲料中应用。优选的,所述组合物使饲料具有促进畜禽生长,降低料肉比的作用。
本发明还涉及包含槲皮万寿菊素的组合物的应用,该组合物作为食品、药品、保健品、化妆品和饲料的添加成分。优选的,所述组合物作为抗氧化剂应用。
本申请还提供一种饲料,所述饲料的原料包含选自油脂、蛋白、维生素、色素、碳水化合物的中的任意一种或几种,以及上述包含槲皮万寿菊素的组合物。所述油脂选自植物油脂或动物油脂;所述植物油脂选自大豆油、棉籽油、葵花籽油、花生油、橄榄油、芝麻油、棕榈油、玉米油等,所述动物油脂选自猪油、牛油、羊油、鱼油等;蛋白为植物蛋白或动物蛋 白,包括但不限于鱼粉、大豆蛋白、谷蛋白;所述色素原料包含但不限于叶黄素、番茄红素、辣椒红素、胡萝卜素、姜黄素等;所述维生素原料包含但不限于维生素A、维生素B、维生素C、维生素D、维生素E以及它们的衍生酯类等。所述饲料为动物饲料,所述动物饲料包括但不限于鸡饲料、牛饲料、羊饲料、猪饲料、狗饲料、猫饲料等。
本发明还涉及一种油脂组合物,其中含有包含槲皮万寿菊素的组合物。
本发明还涉及一种色素组合物,其中含有包含槲皮万寿菊素的组合物。
本发明还涉及一种维生素组合物,其中含有包含槲皮万寿菊素的组合物。
本发明还涉及一种蛋白组合物,其中含有包含槲皮万寿菊素的组合物。
本发明还涉及一种碳水化合物组合物,其中含有包含槲皮万寿菊素的组合物。
本申请所述包含槲皮万寿菊素的组合物可作为任意食品、饲料、化妆品、保健品、药品的添加成分,作为抗氧化剂、生长促进剂和/或品质改良剂。
本申请提供所述包含槲皮万寿菊素组合物的用途,所述用途包括将所述组合物作为饲料的添加剂,具有抗氧化以及促进动物生长,降低动物料肉比的作用。所述动物包括但不限于肉鸡、蛋鸡、猪、兔子、羊、牛、鱼、猫、狗等。
所述包含槲皮万寿菊素的组合物由天然原料提取获得,或通过各成分配比得到。
本申请所述包含槲皮万寿菊素的组合物可通过提取菊科植物获得,例 如万寿菊、孔雀草、金盏花、黄花蒿、万年蒿、黄顶菊、蜡菊、母菊、线叶菊和旋复花等。优选上述菊科植物的花,或花的其它加工形式,或花粕。所述花的其它加工形式,包括但不限于发酵处理,或造粒处理,或烘干处理,或粉碎处理。所述花粕是指经脱脂处理后的花渣。
本申请所述包含槲皮万寿菊素的组合物可以采用溶剂提取物法、超声辅助提取、微波辅助提取、超临界二氧化碳提取法等进行提取获得。溶剂提取中,提取溶剂选自乙醇溶剂、甲醇溶剂、丙酮溶液、乙酸乙酯、丁酮、正己烷、氯仿、二氯甲烷等。
本申请所述包含槲皮万寿菊素的组合物可以通过提取后进一步分离纯化获得,所述纯化方法包括:大孔树脂分离法、液液萃取法、柱色谱分离法、固-液分离、离心分离等。
所述包含槲皮万寿菊素的组合物中各成分含量通过如下高效液相色谱法检测:
高效液相色谱检测的条件为,流动相:A相为1‰的甲酸溶液,B相为乙腈,采用梯度洗脱进行分析(梯度洗脱的条件如表1);洗脱的过程中控制流速:0.3ml/min;柱温:40℃;色谱柱:BEH C18柱(2.1mm×50mm,粒径1.7μm);紫外检测器波长:210-500nm;进样量:0.6μL。其中槲皮万寿菊素的保留时间约在第4-5min,6-羟基山奈酚的保留时间约在第6-7min,万寿菊素的保留时间约在第7.7-8.2min。
检测条件如下:
时间(min) | 流速(mL/min) | A相(%) | B相(%) |
初始 | 0.3 | 90.0 | 10.0 |
1 | 0.3 | 90.0 | 10.0 |
15 | 0.3 | 65.0 | 35.0 |
53 | 0.3 | 0.0 | 100.0 |
57 | 0.3 | 0.0 | 100.0 |
57.5 | 0.3 | 90.0 | 10.0 |
60 | 0.3 | 90.0 | 10.0 |
本申请所述包含槲皮万寿菊素的组合物中各成分含量通过面积归一化法计算得到,各成分的峰面积占总峰面积的百分率的比例即各成分含量比例。
本申请所述包含槲皮万寿菊素的组合物,当其在油脂中含量为2-100ppm时,其抗氧化性能相当于150ppm的乙氧基喹啉(EQ)抗氧化性能。
本申请提供所述包含槲皮万寿菊素组合物具有促进动物生长,降低动物料肉比,改善肉质的作用。
本申请所述包含槲皮万寿菊素的组合物可作为任意食品、饲料的添加剂成分,作为抗氧化剂、生长促进剂和/或品质改良剂。
说明书附图图1为实施例9制备获得的组合物9的高效液相检测色谱图;
说明书附图图2为实施例10制备获得的组合物10的高效液相检测色谱图;
说明书附图图3为实施例11制备获得的组合物11的高效液相检测色谱图;
说明书附图图4为实施例12制备获得的组合物12的高效液相检测色谱图;
说明书附图图5为实施例13制备获得的组合物13的高效液相检测色谱图;
说明书附图图6显示了组合物9-组合物11对番茄红素的护色效果 图,其中,(a)为空白对照组,(b)高温处理后对照组,(c)高温处理后含组合物9的样品,(d)高温处理后含组合物10的样品,(e)高温处理后含组合物11的样品。
为了使本发明的目的、技术方案及优点更加清楚明白,以下结合实施例,对本发明进行进一步详细说明。应当理解,此处所描述的具体实施例仅仅用以解释本发明,并不用于限定本发明。
一.包含槲皮万寿菊素的组合物的制备
按照如下表格中原料及重量份配制实施例1-8的组合物产品
槲皮万寿菊素(重量份) | 6-羟基山奈酚(重量份) | 万寿菊素(重量份) | |
实施例1 | 100 | 10 | 1 |
实施例2 | 100 | 11 | 3 |
实施例3 | 100 | 11 | 4 |
实施例4 | 100 | 12 | 4 |
实施例5 | 100 | 10 | 3 |
实施例6 | 100 | 7 | 3 |
实施例7 | 100 | 5 | 1 |
实施例8 | 100 | 5 | 0 |
二.第一批实验
(1)油脂中的抗氧化效果
分别取鸡油、牛油各5份,每份100克。设置鸡油实验组、牛油实验组各3组,分别按照4、6、8ppm的添加量加入实施例6组合物;设置鸡油对照组、牛油对照组各1组,以150ppm的添加量加入乙氧基喹啉;设置鸡油空白组、牛油空白组各1组,不添加任何添加剂。将各组添加物与油脂混合均匀,放置于40℃恒温箱中,分别于0,3,7,14,21,28天取样品,测定其过氧化值。结果表明,实施例6能够显著降低油脂的过氧 化值,延缓油脂氧化损失进程。抗氧化效果和乙氧基喹啉150ppm的添加量效果相当。
表1 实施例6对鸡油过氧化值的影响(mmol/g)
表2 实施例6对牛油过氧化值的影响单位:(mmol/g)
(2)肉鸡喂养
设置实验组Ⅰ-Ⅵ,共六组,分别按1.25、2.5、3.75、5、10、20ppm向饲料中添加实施例6,并设对照组一组,对照组使用饲料与实验组一致,但是未加入实施例6组合物。将147只1日龄罗斯健康肉鸡(公母各半,平均体重46.7±2.34g)随机分入7个组,每组21只鸡,按上述添加量分别喂食,研究上述7组肉鸡全期(1-42日龄)平均日采食量、平均日增重、料肉比。结果表明,向饲料中添加实施例6时,均能够降低料肉比。同时在添加剂量为3.75ppm时,料肉比最低。
表3 肉鸡喂养效果
三.第二批实验
制备实施例9-17
实施例9:利用丙酮提取万寿菊花,然后加入水和正己烷相进行液液分离,丙酮水相浓缩过滤,滤饼利用1:0.5的正己烷和乙酸乙酯混合溶剂进行萃取除杂,得到含有槲皮万寿菊素的组合物,其中槲皮万寿菊素:6-羟基山奈酚为100:3,即为组合物9。
实施例10:利用丙酮提取孔雀草,然后加入水和正己烷相进行液液分离,丙酮水相浓缩过滤,滤饼利用1:1的正己烷和乙酸乙酯混合溶剂萃取除杂,得到含有槲皮万寿菊素的组合物,其中槲皮万寿菊素:6-羟基山奈酚为100:9,即为组合物10。
实施例11:利用正己烷提取孔雀草进行脱脂,得到的孔雀草渣子用甲醇进行提取,浓缩过滤,滤饼利用乙酸乙酯萃取,萃取液浓缩干燥,然后利用纯水反复洗涤3次,得到含有槲皮万寿菊素的组合物,其中槲皮万寿菊素:6-羟基山奈酚为100:17,即为组合物11。
实施例12:利用正己烷提取孔雀草进行脱脂,得到的孔雀草渣子用乙酸乙酯进行提取,提取液浓缩过滤,滤饼利用正己烷除杂,固相干燥得到含有槲皮万寿菊素的组合物,其中槲皮万寿菊素和6-羟基山奈酚比为100:22,槲皮万寿菊素和万寿菊素比为100:5,即为组合物12。
实施例13:利用正己烷提取万寿菊进行脱脂,得到的万寿菊花粕用67%的甲醇提取,提取液浓缩过滤,滤饼利用乙酸乙酯萃取纯化,萃取液浓缩干燥,然后利用正己烷除杂,固相干燥得到含有槲皮万寿菊素的组合物,其中槲皮万寿菊素和6-羟基山奈酚比为100:31,槲皮万寿菊素和万寿菊素比为100:10,即为组合物13。
实施例14:将槲皮万寿菊素和6-羟基山奈酚的高纯对照品按比例混合,获得槲皮万寿菊素和6-羟基山奈酚比为100:32的组合物,即为组合物14。
实施例15:将槲皮万寿菊素和6-羟基山奈酚的高纯对照品按比例混合,获得槲皮万寿菊素和6-羟基山奈酚比为100:42的组合物,即为组合物15。
实施例16:将槲皮万寿菊素、6-羟基山奈酚、万寿菊素的高纯对照品按比例混合,获得槲皮万寿菊素和6-羟基山奈酚比为100:10、槲皮万寿菊素和万寿菊素比为100:5的组合物,即为组合物16。
实施例17:将槲皮万寿菊素、6-羟基山奈酚、万寿菊素的高纯对照品按比例混合,获得槲皮万寿菊素和6-羟基山奈酚比为100:10、槲皮万寿菊素和万寿菊素比为100:28的组合物,即为组合物17。
1、体外抗氧化能力测定
取实施例9-17各组合物,以及单一成分的槲皮万寿菊素、6-羟基山奈酚、万寿菊素、槲皮素,进行DPPH和羟自由基清除能力的检测,具体检测方法如下。
(1)DPPH自由基清除能力的测定
将槲皮万寿菊素、6-羟基山奈酚、万寿菊素、组合物9-17,用无水乙醇配制浓度为1、2、3、4、5、6μg/ml的样品溶液。然后将DPPH用无水乙醇配制成2×10-4mol/L的溶液,准确吸取空白和样品溶液2mL分别与2mL的DPPH溶液混匀,于30℃水浴下避光放置30min,于波长517nm处测定吸光度A(空白)和A样(样品)。
(2)羟自由基清除能力测定(水杨酸法)
将槲皮万寿菊素、6-羟基山奈酚、万寿菊素、组合物9-17,用无水乙醇配制浓度为100,150,200,250,300μg/ml的样品溶液。配制9mmoI/L水杨酸-乙醇溶液,9mmol/L FeSO4溶液,8.8mmol/L H2O2溶液。然后按照下表中顺序分别加入不同样品,37℃水浴15min,510nm测定吸光度。计算方法:
类别 | A0 | A样 | A本底 |
水杨酸-乙醇溶液 | 1ml | 1ml | 1ml |
FeSO 4溶液 | 1ml | 1ml | 1ml |
样品溶液 | 1ml | 1ml | |
水 | 12ml | 11ml | 12ml |
H 2O 2溶液 | 1ml | 1ml |
两项测试结果如下表4所示:
表4 DPPH和羟自由基的半数清除率
上表结果表明,在达到相同的抗氧化效果的情况下,本申请组合物的用量低于单一组分的产品。
2、在鱼油粉中的抗氧化作用
按照下表成分及含量(以活性成分计)制备含有槲皮万寿菊素、6-羟基山奈酚、万寿菊素或组合物9-17的鱼油粉及空白鱼油粉,将抗氧化剂与鱼油粉混合均匀后放置于40℃恒温箱中,于28天取样,测定其过氧化值,结果如下表5所示。
表5 鱼油粉中过氧化值的测定结果
上表结果表明,作为油脂类成分的添加剂,在达到相同的抗氧化效果的情况下,本申请组合物的用量低于单一组分的产品。
3、肉鸡实验
分别按2、6、10、100ppm(以活性成分计)向饲料中加入组合物9、组合物14作为实验组,并设置空白对照组。将189只1日龄罗斯健康肉鸡(公母各半,平均体重46.7±2.34g)随机分入9个组,每组21只鸡,分别喂食等量的上述各组饲料,研究上述9组肉鸡全期(1-42日龄)料重比。结果见下表6。
表6 肉鸡料重比结果
上表结果表明,向饲料中添加组合物9和组合物14时,均能够降低料肉比。同时在添加剂量大于6ppm时,料重比与空白对照组相比,明显降低。
4、护色效果
将番茄红油树脂与食用盐进行充分的混合分为4组,然后向其中3组中分别添加200ppm的组合物9、10、11,一组作为空白对比照组,以上4组样品放置于105℃恒温箱中2h后取出,观察其颜色变化,结果如说明书附图图1所示。
结果表明组合物9、10、11均能够延缓色素的高温损失。
本申请涉及一种包含槲皮万寿菊素的组合物,其中包含槲皮万寿菊素、6-羟基山奈酚,进一步还可包含万寿菊素。该组合物具有优异的抗氧化效果,可作为食品、药品、保健品、化妆品和饲料的活性添加成分。同时,其在饲料中能够发挥促进动物生长,降低料肉比,改善肉质的作用。
Claims (12)
- 一种包含槲皮万寿菊素的组合物,其特征在于包含槲皮万寿菊素,还包含6-羟基山奈酚。
- 根据权利要求1的组合物,所述槲皮万寿菊素:6-羟基山奈酚的含量比例为100:1-43;所述含量比例优选自100:1-35,更优选自100:1-30,100:1-25,更优选自100:1-20,100:1-15;
- 一种包含槲皮万寿菊素的组合物,其特征在于包含槲皮万寿菊素,还包含6-羟基山奈酚、万寿菊素。
- 根据权利要求3的组合物,所述槲皮万寿菊素:6-羟基山奈酚的含量比例为100:1-43;所述含量比例优选自100:1-35,更优选自100:1-30,100:1-25,更优选自100:1-20,100:1-15;所述槲皮万寿菊素:万寿菊素的含量比例选自100:1-40。
- 一种饲料,其中包含权利要求1-4任一项中所述的组合物。
- 一种食品,其中包含权利要求1-4任一项所述的组合物。
- 一种油脂组合物,其中包含权利要求1-4任一项所述的组合物。
- 一种色素组合物,其中包含权利要求1-4任一项所述的组合物。
- 一种维生素组合物,其中包含权利要求1-4任一项所述的组合物。
- 一种蛋白组合物,其中包含权利要求1-4任一项所述的组合物。
- 一种碳水化合物组合物,其中包含权利要求1-4任一项所述的组合物。
- 根据权利要求1-4任一项所述组合物的应用,该组合物作为食品、药品、保健品、化妆品和饲料的活性添加成分,优选的,所述应用是作为饲料活性添加剂。
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CN113367337B (zh) | 2023-02-24 |
US20230122252A1 (en) | 2023-04-20 |
CN113367337A (zh) | 2021-09-10 |
EP4118980A4 (en) | 2023-08-02 |
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