CN105639653A - oil-tea camellia flower granule with antioxidant activity and preparation method and application thereof - Google Patents
oil-tea camellia flower granule with antioxidant activity and preparation method and application thereof Download PDFInfo
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- CN105639653A CN105639653A CN201510992977.0A CN201510992977A CN105639653A CN 105639653 A CN105639653 A CN 105639653A CN 201510992977 A CN201510992977 A CN 201510992977A CN 105639653 A CN105639653 A CN 105639653A
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Classifications
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L2/00—Non-alcoholic beverages; Dry compositions or concentrates therefor; Their preparation
- A23L2/385—Concentrates of non-alcoholic beverages
- A23L2/39—Dry compositions
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
- A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs
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- Health & Medical Sciences (AREA)
- Nutrition Science (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Food Science & Technology (AREA)
- Polymers & Plastics (AREA)
- Medicines Containing Plant Substances (AREA)
- Medicinal Preparation (AREA)
Abstract
The invention discloses an oil-tea camellia flower granule with antioxidant activity and a preparation method and application thereof. The method optimizes an extraction process and is as below: extracting dry oil-tea camellia flower to obtain an oil-tea camellia flower antioxidant active stock solution; concentrating the stock solution; and blending the stock solution with soluble starch, Arabic gum, glucose powder and citric acid scientifically, so as to prepar the oil-tea camellia flower granule with antioxidant activity. The product has good particle size, taste and brewing performance, is rich in polyphenols, flavonoids, polysaccharides and anthocyanins, activity high antioxidant, and has clearance rate of DPPH., OH. and O2-. over 95 %. The present invention develops a new technical scheme for the effective use of oil-tea camellia; and compared to the prior art, the present invention significantly improves the nutritional health care function of oil-tea camellia; and the processed oil-tea camellia antioxidant granule avoids seasonal restrictions, and the product production can be carried out all-year long. The invention is conducive to the promotion of industrialization, and has good economic and social benefits.
Description
Technical field
The present invention relates to oil tea processing technique field, more specifically, it relates to a kind of oil tea medicinal granules and its preparation method with anti-oxidant activity.
Background technology
Oil tea is as the reproductive organ of tea oil tree, concentrate the nutritive substance in oil tea, the various active compositions such as rich in proteins, amino acid, reducing sugar, polysaccharide, polyphenol, flavones, anthocyanidin, VITAMIN, have anti-oxidant, antitumor, the well health-care effect such as raising immunizing power, adjusting blood lipid, nourishing, beauty treatment to human body. Through practical proof, the anti-oxidant function of oil tea can match in excellence or beauty with internationally recognized oxidation resistant plant Rosmarinus officinalis, has stronger radical scavenging activity and antioxygenation, is a kind of good natural anti-oxidation plant resources.
From the eighties in last century, China's oil tea cultivated area progressively expands, and in order to solve need of production, the research of oil tea is dropped into a large amount of financial resources and material resources by industries, universities and research institutors circle, and obtains and develop faster. But it is for a long time that the exploitation of its by product resource oil tea are obviously delayed. Except possessing ornamental value, its overwhelming majority is naturally withered, rotten, causes the serious wasting of resources. Therefore, it is that the medicinal granules that raw material development has an anti-oxidant activity has certain theoretical and practical significance taking oil tea.
The applicant is devoted for years to the recycling research in oil tea resource and oil tea, it is that the Chinese patent of CN201310673162.7 provides a kind of oil tea flower extract and the application in preparation nourishing drink thereof at publication number, using green oil camellia or dry oil tea as raw material, using water as Extraction solvent, extraction obtains oil tea flower extract, prepared nourishing drink, effectively utilize and ignored discarded oil tea, filled up the blank that oil tea develops. But this technology does not have fully to be extracted by the activeconstituents of oil tea, make oil tea activeconstituents to make full use of aspect not enough to some extent, moreover, this technology is by oil tea flower extract application preparation nourishing drink, application product is single, nourishing drink is not easy to preserve, and carries and also there is inconvenient part.
Summary of the invention
One of the technical problem to be solved in the present invention is that the reutilization technology for existing oil tea is not enough, especially to the deficiency of its effective active components utilising, it is provided that a kind of oil tea anti-oxidant activity stoste. Optimize extraction process to the property of the present invention is directed to, the effective constituent in oil tea fully must be extracted, obtain containing abundant polyphenol, flavones, polysaccharide and anthocyanidin, anti-oxidant activity height, to DPPH, OH and O2 -Clearance rate all oil tea anti-oxidant activity stoste more than 95%.
Another technical problem that the present invention to be solved is to provide a kind of oil tea medicinal granules, science is equipped with auxiliary material, ensure that oil tea activeconstituents is not suffered a loss and can have been played its anti-oxidation efficacy, but also there is the feature of easy preservation, easy to carry, instant.
The also technical problem that the present invention to be solved is to provide the preparation method of described oil tea medicinal granules.
The object of the present invention is achieved by the following technical programs:
The present invention provides a kind of oil tea anti-oxidant activity stoste, prepares by the following method:
S1. taking green oil camellia as raw material, dry after selected removal of impurities, pulverize, obtain oil tea pollen;
S2. by step S1 gained oil tea pollen using alcohol-water as Extraction solvent, oil tea anti-oxidant activity stoste is obtained through vacuum aided extraction or ultra-high voltage two assisted extraction;
Wherein, described in step S2, the condition of vacuum couplings ultrasonic-assisted extraction is: the granularity of oil tea pollen is 20��120 orders, ethanol-water solution taking volume fraction as 20%��90% is for Extraction solvent, according to 1g oil tea pollen: the mixing of the feed liquid ratio of 10��50mL Extraction solvent, Extracting temperature be 30��90 DEG C, vacuum tightness be 0.1��0.9MPa when extract 10��50min;
Or, described in step S2, the condition of ultra-high voltage two assisted extraction is: the granularity of oil tea pollen is 20��120 orders, ethanol-water solution taking volume fraction as 20%��90% is for Extraction solvent, according to 1g oil tea pollen: the ratio mixing of the solid-liquid ratio of 10��50mL Extraction solvent, extracting, pressure is 100��700MPa, intermittent pressurized extracts 2 times under Extracting temperature is 20��80 DEG C of conditions, extracts 2��10min altogether.
When extracting method of the present invention, not only remain the activeconstituents of oil tea to greatest extent, and obtained active stoste and remain oil tea fragrance of a flower gas largely, be the organoleptic quality offer powerful guarantee of follow-up preparation oil tea medicinal granules.
Preferably, fresh described in step S1 oil tea is for Thistle oil camellia or common spends oil tea in vain.
Preferably, selecting removal of impurities described in step S1 is select wherein without the oil tea of disease and pest, nothing breakage, and removes the impurity such as the blade being mingled with, careless bits;
Preferably, drying described in step S1 adopts the drying modes such as microwave hot air combined drying, microwave vacuum combined drying, vacuum freezing combined drying or cryogenic vacuum combined drying to carry out composite drying stage by stage, oil tea is dried to moisture content lower than 8%, such drying mode and extent control are conducive to retaining the original color and luster of oil tea and fragrance, are also convenient to following process. The processing condition of described drying are with reference to existing routine techniques.
Further preferably, adopting microwave hot air combined drying process, drying conditions is: microwave power 350W, and microwave time 30S carries out completing, the activity of deactivating enzyme, after under 50 DEG C of conditions warm air drying 12h, dried oil tea water content is less than 8%;Then adopt medicinal herb grinder to pulverize, sieve, obtain dry oil tea pollen.
Preferably, in step S2, when adopting vacuum aided to extract, the granularity of oil tea pollen is 60��80 orders; When adopting ultra-high voltage two assisted extraction, the granularity of oil tea pollen is 80��100 orders.
Further preferably, in step S2, when adopting vacuum aided to extract, the ethanol-water solution taking volume fraction as 60%��70% is for Extraction solvent; Solid-liquid ratio is 1g oil tea pollen: 30��40mL Extraction solvent; Extraction time is 30��40min; Extracting temperature is 70��80 DEG C; Vacuum tightness is 0.6��0.7MPa.
Further preferably, when adopting ultra-high voltage two assisted extraction, adopting grinding particle size to be 80��100 dry oil tea pollen of objects is raw material, and the ethanol-water solution taking volume fraction as 50%��60% is for Extraction solvent; Solid-liquid ratio is 1g oil tea pollen: 30��40mL Extraction solvent; Extraction pressure is 300��400Mpa; Extraction time is 6��8min; Extracting temperature is 40��50 DEG C.
Adopt the inventive method to extract the oil tea anti-oxidant activity stoste that obtains and compare other extracting method existing, remain activeconstituents contained by it to greatest extent, and adopt ethanol as Extraction solvent, also significantly increase the anti-oxidant activity of extracting solution, to DPPH, OH and O2 -Clearance rate more than 95%. After testing, in the experimental example that the present invention is a large amount of for a long time, in the oil tea anti-oxidant activity stoste that different batches prepares, polyphenol content is 350��400mg/100mL, flavones content is 400��500mg/mL, and polysaccharide content is 700��800mg/100mL, and anthocyanidin content is 50��60mg/100mL. And there is very strong anti-oxidant activity, to DPPH, OH and O2 -Clearance rate more than 95%.
Based on described oil tea anti-oxidant activity stoste, the present invention also provides a kind of oil tea medicinal granules with anti-oxidant activity, is made up of each component of following weight percent: the concentrated solution of oil tea anti-oxidant activity stoste, 10%��70%; Zulkovsky starch, 1%��5%; Gum arabic, 10%��40%; Icing Sugar, 10%��70%; Citric acid, 0.5%��3%; Wherein, the concentrated solution of described oil tea anti-oxidant activity stoste is concentrated to wherein soluble solid mass percent by oil tea anti-oxidant activity stoste and reaches 35��40% and get final product.
Preferably, the concentrated solution of described oil tea anti-oxidant activity stoste adopts cryogenic vacuum to concentrate to obtain, the concentrated condition of preferred cryogenic vacuum is 45��50 DEG C, 10��13Kpa, so process the concentrated solution obtained, maintain to maximum degree effective constituent and the local flavor of oil tea anti-oxidant activity stoste. After testing, in enriched material, polyphenol content is 4500��5000mg/100mL, and flavones content is 6000��6500mg/mL, and polysaccharide content is 7000��8000mg/100mL, and anthocyanidin content is 600��800mg/100mL.
Preferably, described medicinal granules adopt gum arabic (powder shape) as vehicle. Gum arabic is a kind of carbohydrate polymer, does not substantially produce heat, and is good water-soluble dietary fibre.
Preferably, described oil tea medicinal granules is made up of each component of following weight percent: the concentrated solution of oil tea anti-oxidant activity stoste, 30%��50%; Zulkovsky starch, 1%��2%; Gum arabic, 10%��20%; Icing Sugar, 30%��50%; Citric acid, 0.5%��1.5%.
Further preferably, described oil tea medicinal granules is made up of each component of following weight percent: the concentrated solution of oil tea anti-oxidant activity stoste, 40%; Zulkovsky starch, 1.5%; Gum arabic, 18%; Icing Sugar, 40%; Citric acid, 0.5%. Preferably, described Icing Sugar can adopt glucose powder. Glucose powder sugariness is the 60��70% of cane sugar powder, is added in product of the present invention and is possible not only to the mouthfeel improving product, and can not affect the oil tea extraction original local flavor of concentrated solution, brings out the best in each other.
The preparation method described in invention also provides with the oil tea medicinal granules of anti-oxidant activity takes each component by the weight percent of composition of raw materials, through allotment, mixing, granulation, is drying to obtain.
The present invention provides preferred oil tea medicinal granules preparation method as follows: first added by Zulkovsky starch in the concentrated solution of oil tea anti-oxidant activity stoste, add citric acid again to dissolve, then deployed mixture is slowly added with spray pattern in the gum arabic mixed and glucose powder, then all materials are dropped in mixing machine, fully mix, then granulating and forming. Specifically, it is put into the described raw material mixed Pendulargranulator carries out granulation. The aforementioned wet granular prepared being placed in boiling drier dry, dry terminal is that pellet moisture is down to about 3%. The processing condition of described granulating and forming are: net sieve 14��20 order, drying temperature 70��80 DEG C.
In the present invention, the anti-oxidant stoste of oil tea is containing bitter taste material, if can not effectively embed, the mouthfeel bitter taste of gained medicinal granules is heavier, agreeable to the taste not. So the present invention is through summing up discovery in a large number, under the concentrated solution part by weight of oil tea anti-oxidant activity stoste is 10%��70% condition, preferred Zulkovsky starch adds with the part by weight of 1%��5%, fully stir under keeping the temperature condition of 50 DEG C��60 DEG C, it is possible to successfully embed the bitter taste material in the anti-oxidant stoste of oil tea. Preferably, for ensureing the best effect of electuary, described gum arabic and glucose powder need to add after pulverizing, sieving in advance again, it is preferable that granularity is 100��120 orders.
Being sieved by described dry rear oil tea medicinal granules, it is preferable that electuary particle fineness is sieved by 10��50 orders, the fine particle by 10 orders sieves and by 60 orders sieves is no more than the 8% of particle total amount. Obtaining described oil tea medicinal granules, in particulate state, evenly unanimously, inclusion-free, nothing caking, brew is good, containing oxidation-resistant active ingredients such as polyphenol, flavones, polysaccharide and anthocyanidin. Preferably described oil tea medicinal granules is reconstituted according to 1g:20mL boiling water.
The present invention has following useful effect: the recycling that the present invention is oil tea provides more technical scheme, and that has widened oil tea effectively utilizes product scope. After oil tea flower extract is made particle, it is possible to better as the application such as nutritional additive of electuary, pastry foodstuff, beverage, Application Areas is convenient, wide.
Extracting method, in preparation oil tea flower extract, has been carried out specific aim optimization by the present invention. Oil tea material quality is tender and lovely, and in leaching process, easy color, smell and taste are lost to the greatest extent. The present invention adopts vacuum aided to extract and ultra-high voltage two assisted extraction methods, summarize Extraction solvent kind pointedly and concentration, raw material granularity, ultrasonic wave or pressure range, Extracting temperature and time etc. have been carried out global optimization, not only remain the activeconstituents of oil tea to greatest extent, in obtained product, not only polyphenol, flavones, polysaccharide and anthocyanidin content are abundant, and anti-oxidant activity is higher, to DPPH, OH and O2 -Clearance rate more than 95%, achievement in research previous relative to prior art and the applicant all demonstrates bigger advantage, and obtained active stoste and remain oil tea fragrance of a flower gas largely, it is the organoleptic quality offer powerful guarantee of follow-up preparation oil tea medicinal granules.Specifically, the present invention adopts combined drying mode to be completed by green oil camellia drying treatment, retains the original color and luster of oil tea and fragrance largely; Ethanol is adopted to extract as Extraction solvent, extraction time length when compensate for using water as Extraction solvent, temperature height, the deficiency that fluid volume is big, extract the prerequisite of oil tea activeconstituents in maximum degree under, the price of Extraction solvent (ethanol) is not high, recovery process simple, efficiency height, and the pollution produced by environment is considerably less; Especially the vacuum aided based on specific aim processing condition is adopted to extract or ultra-high voltage assisted extraction, accelerate the effective constituent diffusion stripping of oil tea and fully mix with Extraction solvent, the accurate restriction of extraction conditions remains to very high degree again the nutritive ingredient in oil tea, shorten extraction time, improve extraction yield, for the suitability for industrialized production of product provides a scientific basis. Invention further provides a kind of oil tea medicinal granules, auxiliary material is optimized configuration, the oil tea medicinal granules bitter taste prepared alleviates, and overall organoleptic quality is good, microbiological indicator conformance with standard. Described oil tea medicinal granules outward appearance drying, uniform particles, color and luster are consistent, make moist phenomenon without caking. After described oil tea medicinal granules boiling water is reconstituted, comparatively fast dissolve, without impurity such as burnt bits, after testing, the antioxidant components such as polyphenol, flavones, polysaccharide, anthocyanidin are basic and stoste is consistent, and have good anti-oxidant activity, reducing power is relatively strong, to DPPH, OH and O2 -Clearance rate higher. Oranoleptic indicator, the microbiological indicator of oil tea medicinal granules entirety have been measured by the present invention, after being reconstituted by oil tea medicinal granules, wherein antioxidant component, anti-oxidant activity have been studied. After testing, the present invention has that the outward appearance of the oil tea medicinal granules product of anti-oxidant activity is dry, uniform particles, in light brown, color and luster consistent, makes moist phenomenon without caking, the particle proportion of granularity between 14��30 orders is more than 95%. Having the peculiar fragrance of oil tea, brew is good, can comparatively fast dissolve, and the impurity such as considers to be worth doing without Jiao. Product total plate count (cfu/g)��100/g of the present invention, intestinal bacteria (MPN/100g)��30, without pathogenic bacterium detection. Oil tea medicinal granules product of the present invention contains abundant antioxidant component, and especially polyphenol, flavones, polysaccharide and anthocyanidin content are abundant, and anti-oxidant activity is relatively strong, to DPPH, OH and O2 -There is very high clearance rate. Oil tea Raw material processing is made medicinal granules by the present invention, avoids restriction in season so that product can be produced throughout the year, is conducive to industrialization promotion, has good economic benefit and social benefit.
Accompanying drawing explanation
Fig. 1 the present invention has preparation technology's schematic flow sheet of the oil tea medicinal granules of anti-oxidant activity; Fig. 2 vacuum tightness is on the impact of antioxidant component content in oil tea extracting solution; Fig. 3 Extracting temperature is on the impact of antioxidant component content in oil tea extracting solution; Fig. 4 extraction time is on the impact of antioxidant component content in oil tea extracting solution; Fig. 5 Extraction solvent (ethanol) concentration is on the impact of antioxidant component content in oil tea extracting solution; Fig. 6 solid-liquid ratio is on the impact of antioxidant component content in oil tea extracting solution; The dry oil tea grinding particle size of Fig. 7 is on the impact of antioxidant component content in oil tea extracting solution; Fig. 8 ultra high pressure extraction pressure is on the impact of antioxidant component content in oil tea extracting solution;Fig. 9 ultra high pressure extraction temperature is on the impact of antioxidant component content in oil tea extracting solution; Figure 10 ultra-high voltage action time is on the impact of antioxidant component content in oil tea extracting solution; The reducing power experimental result of Figure 11 oil tea medicinal granules; Figure 12 oil tea medicinal granules removes the effect of DPPH free radical; Figure 13 oil tea medicinal granules removes the effect of OH free radical; Figure 14 oil tea medicinal granules removes O2 -The effect of free radical.
Embodiment
Below in conjunction with the drawings and specific embodiments, the invention will be further described, and cited embodiment is only the experimental example of representativeness of the present invention, does not therefore limit the scope of the invention. Unless stated otherwise, the present invention adopts raw material and equipment are raw material and the equipment of the art routine.
The preparation of embodiment 1 oil tea anti-oxidant activity stoste
The present embodiment provides a kind of oil tea anti-oxidant activity stoste, prepares by the following method:
S1. taking green oil camellia as raw material, dry after selected removal of impurities, pulverize, obtain oil tea pollen;
S2. being sieved by step S1 gained oil tea pollen makes its granularity be 20��50 orders, ethanol-water solution taking volume fraction as 20% is for Extraction solvent, according to 1g oil tea pollen: the feed liquid ratio mixing of 10mL Extraction solvent, adopting the method that vacuum aided is extracted, vacuum aided extraction conditions is: Extracting temperature 30 DEG C, vacuum tightness 0.1MPa, extraction time 10min.
Described fresh oil tea is Thistle oil camellia. Select wherein without the complete oil tea of disease and pest, nothing breakage, and remove the impurity such as the blade being mingled with, careless bits. Described drying adopts microwave hot air combined drying process, and drying conditions is: microwave power 350W, microwave time 30S, temperature 50 DEG C, dry 12h, and dried oil tea water content is 6.2%; Then adopt medicinal herb grinder to pulverize, sieve, obtain dry oil tea pollen. Gained oil tea anti-oxidant activity stoste outward appearance clear, in orange-yellow, has the distinctive fragrance of oil tea.
The preparation of embodiment 2 oil tea anti-oxidant activity stoste
The present embodiment provides a kind of oil tea anti-oxidant activity stoste, prepares by the following method:
S1. taking green oil camellia as raw material, dry after selected removal of impurities, pulverize, obtain oil tea pollen;
S2. being sieved by step S1 gained oil tea pollen makes its granularity be 80��120 orders, ethanol-water solution taking volume fraction as 70% is for Extraction solvent, according to 1g oil tea pollen: the feed liquid ratio mixing of 50mL Extraction solvent, adopting the method that vacuum aided is extracted, vacuum aided extraction conditions is: Extracting temperature 30 DEG C, vacuum tightness 0.6MPa, extraction time 20min.
Described fresh oil tea is Thistle oil camellia. Select wherein without the complete oil tea of disease and pest, nothing breakage, and remove the impurity such as the blade being mingled with, careless bits; Described drying adopts microwave hot air combined drying process, and drying conditions is: microwave power 350W, microwave time 30S, temperature 50 DEG C, dry 12h, and dried oil tea water content is 6.2%; Then adopt medicinal herb grinder to pulverize, sieve, obtain dry oil tea pollen. Gained oil tea anti-oxidant activity stoste outward appearance clear, in orange red, has the distinctive fragrance of oil tea.
The preparation of embodiment 3 oil tea anti-oxidant activity stoste
The present embodiment provides a kind of oil tea anti-oxidant activity stoste, prepares by the following method:
S1. taking green oil camellia as raw material, dry after selected removal of impurities, pulverize, obtain oil tea pollen;
S2. being sieved by step S1 gained oil tea pollen makes its granularity be 60��80 orders, ethanol-water solution taking volume fraction as 90% is for Extraction solvent, according to 1g oil tea pollen: the feed liquid ratio mixing of 40mL Extraction solvent, adopting the method that vacuum aided is extracted, vacuum aided extraction conditions is: Extracting temperature 90 DEG C, vacuum tightness 0.9MPa, extraction time 30min.
Described fresh oil tea is Thistle oil camellia. Select wherein without the oil tea of disease and pest, nothing breakage, and remove the impurity such as the blade being mingled with, careless bits; Described drying adopts microwave hot air combined drying process, and drying conditions is: microwave power 350W, microwave time 30S, temperature 50 DEG C, and being dried to oil tea water content is 7%; Then adopt medicinal herb grinder to pulverize, sieve, obtain dry oil tea pollen. The clarification of gained oil tea anti-oxidant activity stoste outward appearance is bright, and color and luster is relatively dark, in sorrel, has the distinctive fragrance of oil tea.
The preparation of embodiment 4 oil tea anti-oxidant activity stoste
The present embodiment provides a kind of oil tea anti-oxidant activity stoste, prepares by the following method:
S1. taking green oil camellia as raw material, dry after selected removal of impurities, pulverize, obtain oil tea pollen;
S2. being sieved by step S1 gained oil tea pollen makes its granularity be 60��80 orders, ethanol-water solution taking volume fraction as 60% is for Extraction solvent, according to 1g oil tea pollen: the feed liquid ratio mixing of 30mL Extraction solvent, adopting the method that vacuum aided is extracted, vacuum aided extraction conditions is: Extracting temperature 80 DEG C, vacuum tightness 0.6MPa, extraction time 40min.
Described fresh oil tea spends oil tea in vain for common. Select wherein without disease and pest, without the oil tea damaged, pattern is pure white, and remove the impurity such as the blade being mingled with, careless bits; Described drying adopts microwave hot air combined drying process, and drying conditions is: microwave power 350W, microwave time 30S, temperature 50 DEG C, and being dried to oil tea water content is 6.8%; Then adopt medicinal herb grinder to pulverize, sieve, obtain dry oil tea pollen. Gained oil tea anti-oxidant activity stoste outward appearance clear, in orange-yellow, has the distinctive fragrance of oil tea.
The preparation of embodiment 5 oil tea anti-oxidant activity stoste
The present embodiment provides a kind of oil tea anti-oxidant activity stoste, prepares by the following method:
S1. taking green oil camellia as raw material, dry after selected removal of impurities, pulverize, obtain oil tea pollen;
S2. being sieved by step S1 gained oil tea pollen makes its granularity be 60��80 orders, ethanol-water solution taking volume fraction as 70% is for Extraction solvent, according to 1g oil tea pollen: the feed liquid ratio mixing of 35mL Extraction solvent, adopting the method that vacuum aided is extracted, vacuum aided extraction conditions is: Extracting temperature 70 DEG C, vacuum tightness 0.7MPa, extraction time 35min.
Described fresh oil tea spends oil tea in vain for common. Select wherein without the oil tea of disease and pest, nothing breakage, and remove the impurity such as the blade being mingled with, careless bits; Drying described in the present embodiment adopts microwave hot air combined drying process, and drying conditions is: microwave power 350W, microwave time 30S, temperature 50 DEG C, and being dried to oil tea water content is 7.2%; Then adopt medicinal herb grinder to pulverize, sieve, obtain dry oil tea pollen. Gained oil tea anti-oxidant activity stoste outward appearance clear, in deep yellow, has the distinctive fragrance of oil tea.
The preparation of embodiment 6 oil tea anti-oxidant activity stoste
The present embodiment provides a kind of oil tea anti-oxidant activity stoste, prepares by the following method:
S1. taking green oil camellia as raw material, dry after selected removal of impurities, pulverize, obtain oil tea pollen;
S2. being sieved by step S1 gained oil tea pollen makes its granularity be 60��80 orders, ethanol-water solution taking volume fraction as 70% is for Extraction solvent, according to 1g oil tea pollen: the feed liquid ratio mixing of 35mL Extraction solvent, adopting the method that vacuum aided is extracted, vacuum aided extraction conditions is: Extracting temperature 70 DEG C, vacuum tightness 0.7MPa, extraction time 35min.
Described fresh oil tea is for Thistle oil camellia and common spends oil tea (mix, ratio is not limit) in vain. Select wherein without the oil tea of disease and pest, nothing breakage, and remove the impurity such as the blade being mingled with, careless bits; Drying adopts microwave hot air combined drying process, and drying conditions is: microwave power 350W, microwave time 30S, temperature 50 DEG C, and being dried to oil tea water content is 6.5%; Then adopt medicinal herb grinder to pulverize, sieve, obtain dry oil tea pollen. Gained oil tea anti-oxidant activity stoste outward appearance clear, in orange-yellow, has the distinctive fragrance of oil tea.
The preparation of embodiment 7 oil tea anti-oxidant activity stoste
The present embodiment provides a kind of oil tea anti-oxidant activity stoste, prepares by the following method:
S1. taking green oil camellia as raw material, dry after selected removal of impurities, pulverize, obtain oil tea pollen;
S2. being sieved by step S1 gained oil tea pollen makes its granularity be 100��120 orders, ethanol-water solution taking volume fraction as 90% is for Extraction solvent, according to 1g oil tea pollen: the feed liquid ratio mixing of 40mL Extraction solvent, ultra-high voltage two assisted extraction methods are adopted to extract, ultra-high voltage assisted extraction condition is: extraction pressure 700MPa, Extracting temperature 20 DEG C, intermittent pressurized extract 2 times, extract 2min altogether.
Described fresh oil tea is Thistle oil camellia. Select wherein without the complete oil tea of disease and pest, nothing breakage, and remove the impurity such as the blade being mingled with, careless bits; Drying means described in the present embodiment is with embodiment 1. Gained oil tea anti-oxidant activity stoste outward appearance clear, in light yellow, has the distinctive fragrance of oil tea.
The preparation of embodiment 8 oil tea anti-oxidant activity stoste
The present embodiment provides a kind of oil tea anti-oxidant activity stoste, prepares by the following method:
S1. taking green oil camellia as raw material, dry after selected removal of impurities, pulverize, obtain oil tea pollen;
S2. being sieved by step S1 gained oil tea pollen makes its granularity be 20��80 orders, ethanol-water solution taking volume fraction as 20% is for Extraction solvent, according to 1g oil tea pollen: the feed liquid ratio mixing of 50mL Extraction solvent, ultra-high voltage two assisted extraction methods are extracted, ultra-high voltage assisted extraction condition is: extraction pressure 100MPa, Extracting temperature 80 DEG C, intermittent pressurized extract 2 times, extract 10min altogether.
Described green oil camellia is Thistle oil camellia. Select wherein without the oil tea of disease and pest, nothing breakage, and remove the impurity such as the blade being mingled with, careless bits; Drying means described in the present embodiment is with embodiment 1. Gained oil tea anti-oxidant activity stoste outward appearance clear, in orange-yellow, has the distinctive fragrance of oil tea.
The preparation of embodiment 9 oil tea anti-oxidant activity stoste
The present embodiment provides a kind of oil tea anti-oxidant activity stoste, prepares by the following method:
S1. taking green oil camellia as raw material, dry after selected removal of impurities, pulverize, obtain oil tea pollen;
S2. being sieved by step S1 gained oil tea pollen makes its granularity be 80��100 orders, ethanol-water solution taking volume fraction as 50% is for Extraction solvent, according to 1g oil tea pollen: the feed liquid ratio mixing of 30mL Extraction solvent, ultra-high voltage two assisted extraction methods are extracted, ultra-high voltage assisted extraction condition is: extraction pressure 300MPa, Extracting temperature 40 DEG C, intermittent pressurized extract 2 times, extract 6min altogether.
Described fresh oil tea spends oil tea in vain for common. It is described that to select removal of impurities be select wherein without disease and pest, without damaged complete oil tea, and remove the impurity such as the blade being mingled with, careless bits; Drying means is with embodiment 1.Gained oil tea anti-oxidant activity stoste outward appearance clear, in deep yellow, has the distinctive fragrance of oil tea.
The preparation of embodiment 10 oil tea anti-oxidant activity stoste
The present embodiment provides a kind of oil tea anti-oxidant activity stoste, prepares by the following method:
S1. taking green oil camellia as raw material, dry after selected removal of impurities, pulverize, obtain oil tea pollen;
S2. being sieved by step S1 gained oil tea pollen makes its granularity be 80��100 orders, ethanol-water solution taking volume fraction as 60% is for Extraction solvent, according to 1g oil tea pollen: the feed liquid ratio mixing of 40mL Extraction solvent, ultra-high voltage two assisted extraction methods are extracted, ultra-high voltage assisted extraction condition is: extraction pressure 400MPa, Extracting temperature 45 DEG C, intermittent pressurized extract 2 times, extract 8min altogether.
Described fresh oil tea spends oil tea in vain for common. It is described that to select removal of impurities be select wherein without disease and pest, without damaged complete oil tea, and remove the impurity such as the blade being mingled with, careless bits; Drying means is with embodiment 1. Gained oil tea anti-oxidant activity stoste outward appearance clear, in orange-yellow, has the distinctive fragrance of oil tea.
The preparation of embodiment 11 oil tea anti-oxidant activity stoste
The present embodiment provides a kind of oil tea anti-oxidant activity stoste, prepares by the following method:
S1. taking green oil camellia as raw material, dry after selected removal of impurities, pulverize, obtain oil tea pollen;
S2. being sieved by step S1 gained oil tea pollen makes its granularity be 80��100 orders, ethanol-water solution taking volume fraction as 55% is for Extraction solvent, according to 1g oil tea pollen: the feed liquid ratio mixing of 30mL Extraction solvent, ultra-high voltage two assisted extraction methods are extracted, ultra-high voltage assisted extraction condition is: extraction pressure 350MPa, Extracting temperature 45 DEG C, intermittent pressurized extract 2 times, extract 7min altogether.
Described fresh oil tea is for Thistle oil camellia and common spends oil tea (mixing) in vain. Select wherein without the oil tea of disease and pest, nothing breakage, and remove the impurity such as the blade being mingled with, careless bits; Drying means is with embodiment 1.
Gained oil tea anti-oxidant activity stoste outward appearance clear, orange red, there is the distinctive fragrance of oil tea.
The preparation of the concentrated solution of embodiment 12 oil tea anti-oxidant activity stoste
Arbitrary for embodiment 1 to 10 example gained oil tea anti-oxidant activity stoste is concentrated to after wherein soluble solid mass percent reaches 35��40%, obtaining the concentrated solution of oil tea anti-oxidant activity stoste respectively. Cryogenic vacuum concentration method can be adopted, it is preferable that the concentrated condition of cryogenic vacuum be 45��50 DEG C, 10��13Kpa, so processes the concentrated solution obtained, and maintains to maximum degree effective constituent and the local flavor of oil tea anti-oxidant activity stoste. After testing, polyphenol content 4500��5000mg/100mL in enriched material, flavones content is 6000��6500mg/mL, and polysaccharide content is 7000��8000mg/100mL, and anthocyanidin content is 600��800mg/100mL.
The preparation of embodiment 13 oil tea medicinal granules
The present embodiment provides a kind of oil tea medicinal granules with anti-oxidant activity, is made up of each component of following weight percent: the concentrated solution of the obtained each oil tea anti-oxidant activity stoste of embodiment 12,10%; Zulkovsky starch, 1%; Gum arabic, 40%; Glucose powder, 46%; Citric acid, 3%.
First Zulkovsky starch is added in the concentrated solution of oil tea anti-oxidant activity stoste, fully stir under keeping the temperature condition of 50 DEG C��60 DEG C;Add citric acid again to dissolve, then deployed mixture is slowly added with spray pattern in the gum arabic mixed and glucose powder, then all materials are dropped in mixing machine, fully mix, put into and Pendulargranulator carries out granulation. The wet granular prepared being placed in boiling drier dry, dry terminal is that pellet moisture is down to about 3%. The processing condition of described granulating and forming are: net sieve 14��20 order, drying temperature 70��80 DEG C. Gained oil tea medicinal granules is without any bitter taste, and overall organoleptic quality is good, microbiological indicator conformance with standard, and has stronger anti-oxidant activity.
The preparation of embodiment 14 oil tea medicinal granules
The present embodiment provides a kind of oil tea medicinal granules with anti-oxidant activity, is made up of each component of following weight percent: the concentrated solution of the obtained each oil tea anti-oxidant activity stoste of embodiment 12,70%; Zulkovsky starch, 4.5%; Gum arabic, 10%; Glucose powder, 15%; Citric acid, 0.5%. Preparation method is with embodiment 13. Gained oil tea medicinal granules is without any bitter taste, and overall organoleptic quality is good, microbiological indicator conformance with standard, and has stronger anti-oxidant activity.
The preparation of embodiment 15 oil tea medicinal granules
The present embodiment provides a kind of oil tea medicinal granules with anti-oxidant activity, is made up of each component of following weight percent: the concentrated solution of the obtained each oil tea anti-oxidant activity stoste of embodiment 12,40%; Zulkovsky starch, 1%; Gum arabic, 20%; Glucose powder, 37.5%; Citric acid, 1.5%. Preparation method is with embodiment 13. Gained oil tea medicinal granules is without any bitter taste, and overall organoleptic quality is good, microbiological indicator conformance with standard, and has stronger anti-oxidant activity.
The preparation of embodiment 16 oil tea medicinal granules
The present embodiment provides a kind of oil tea medicinal granules with anti-oxidant activity, is made up of each component of following weight percent: the concentrated solution of the obtained each oil tea anti-oxidant activity stoste of embodiment 12,50%; Zulkovsky starch, 2%; Gum arabic, 20%; Glucose powder, 27%; Citric acid, 1%. Preparation method is with embodiment 13. Gained oil tea medicinal granules is without any bitter taste, and overall organoleptic quality is good, microbiological indicator conformance with standard, and has stronger anti-oxidant activity.
The preparation of embodiment 17 oil tea medicinal granules
The present embodiment provides a kind of oil tea medicinal granules with anti-oxidant activity, is made up of each component of following weight percent: the concentrated solution of the obtained each oil tea anti-oxidant activity stoste of embodiment 12,40%; Zulkovsky starch, 1.5%; Gum arabic, 18%; Glucose powder, 40%; Citric acid, 0.5%. Preparation method is with embodiment 13. Gained oil tea medicinal granules is without any bitter taste, and overall organoleptic quality is good, microbiological indicator conformance with standard, and has stronger anti-oxidant activity.
The optimization of process conditions that embodiment 18 vacuum aided is extracted
For confirming the superiority of technique of the present invention further, the present embodiment is verified by experiment of single factor. Can obtaining, when adopting vacuum aided to extract, vacuum tightness, Extracting temperature and the extraction time impact extracted by the dry middle antioxidant component of oil tea of 3 factors are more remarkable. On this basis, adopting response surface CCD center combination design method, design Three factors-levels optimization Test, optimizes vacuum aided extracting factor, and experiment knot the results are shown in shown in accompanying drawing 2 to accompanying drawing 7, and optimization Test result is as shown in table 1.
Table 1 vacuum aided optimization for extracting condition test-results
Utilize Design-Expert8.0 statistical software his-and-hers watches 1 experimental data to carry out regression fit, obtain respectively polyphenol in extracting solution, flavones, polysaccharide, anthocyanidin content to vacuum tightness, Extracting temperature and extraction time 3 factors two multinomial regression equations:
Polyphenol:
Y1=367.83+17.33X1+1.67X2+2.25X3-19.25X1X2-1.75X1X3+9.13X2X3-9.35X1 2-3.98X2 2+2.40X3 2
Flavones:
Y2=470.67+22.17X1-1.58X2+0.083X3-21.25X1X2-2.62X1X3+11.00X2X3-14.79X1 2-9.54X2 2-1.17X3 2
Polysaccharide:
Y3=774.17+19.79X1-1.13X2+0.79X3-15.69X1X2-2.06X1X3+6.31X2X3-9.99X1 2-3.74X2 2+0.010X3 2
Anthocyanidin:
Y4=48.50+3.04X1+0.54X2+0.96X3-3.94X1X2-0.56X1X3+1.19X2X3-0.36X1 2-0.36X2 2+1.64X3 2
According to Design-Expert software, regression model is analyzed, draw the optimal extract process parameter of each antioxidant component, be respectively: polyphenol: vacuum tightness 0.67Mpa, Extracting temperature 80 DEG C, extraction time 36min; Flavones: vacuum tightness 0.7Mpa, Extracting temperature 77 DEG C, extraction time 38min; Polysaccharide: vacuum tightness 0.7Mpa, Extracting temperature 80 DEG C, extraction time 35min; Anthocyanidin: vacuum tightness 0.68Mpa, Extracting temperature 75 DEG C, extraction time 38min. Consider the content of each oxidation-resistant active ingredient, in conjunction with the experiment of single factor result of other factors, show that the optimum extraction conditions that vacuum aided is extracted is: dry oil tea grinding particle size is 60��80 orders, Extraction solvent alcohol-water volume fraction is 60%��70%, solid-liquid ratio is 1g:30��40mL, extraction time is 30��40min, and Extracting temperature is 70��80 DEG C, and vacuum tightness is 0.6��0.7MPa. Single factor experiment result further demonstrates the superiority of technique of the present invention.
The optimization of process conditions of embodiment 19 ultra-high voltage two assisted extraction
For confirming the superiority of technique of the present invention further, the present embodiment is verified by experiment of single factor. When adopting ultra-high voltage two assisted extraction, pressure, Extracting temperature and the extraction time impact extracted by the dry middle antioxidant component of oil tea of 3 factors are more remarkable. On this basis, adopting Box-Behnken method of design, design Three factors-levels optimization Test, optimizes ultra-high voltage two assisted extraction processing condition, and experimental result is shown in that, shown in accompanying drawing 8 to accompanying drawing 10, concrete test-results is as shown in table 2.
Table 2 ultra-high voltage two assisted extraction condition optimizing test-results
Utilize Design-Expert8.0 statistical software his-and-hers watches 2 experimental data to carry out regression fit, obtain respectively polyphenol in extracting solution, flavones, polysaccharide, anthocyanidin content to the regression equation extracting pressure, extraction time and Extracting temperature 3 factors:
Polyphenol:
Y1=364.60+28.00X1+3.62X2-7.13X3-2.00X1X2-3.00X1X3+5.75X2X3+1.08X1 2-10.67X2 2-23.68X3 2
Flavones:
Y2=482.40+41.63X1+21.25X2+10.63X3-13.75X1X2-12.50X1X3-5.75X2X3-33.45X1 2-37.70X2 2-31.45X3 2
Polysaccharide:
Y3=799.00+27.88X1+5.13X2-5.75X3-11.50X1X2-8.25X1X3-2.25X2X3-11.50X1 2-40.50X2 2-41.75X3 2
Anthocyanidin:
Y4=59.80+3.88X1+0.88X2-1.25X3+1.75X1X2-1.50X1X3-0.50X2X3-4.78X1 2-6.28X2 2-9.52X3 2
According to Design-Expert software, regression model is analyzed, draw the optimal extract process parameter of each antioxidant component, be respectively: polyphenol: extract pressure 373Mpa, extraction time 7.2min, Extracting temperature 49 DEG C; Flavones: extract pressure 400Mpa, extraction time 6.2min, Extracting temperature 42 DEG C; Polysaccharide: extract pressure 398Mpa, extraction time 7.0min, Extracting temperature 44.3 DEG C; Anthocyanidin: extract pressure 362Mpa, extraction time 7.5min, Extracting temperature 43 DEG C. Consider the content of each oxidation-resistant active ingredient, in conjunction with the experiment of single factor result of other factors, the optimum extraction conditions drawing ultra-high voltage two assisted extraction is: dry oil tea grinding particle size is 80��100 orders, Extraction solvent alcohol-water concentration is 50%��60%, solid-liquid ratio is 1g:30��40mL, and extraction pressure is 300��400Mpa, and extraction time is 6��8min, Extracting temperature is 40��50 DEG C, and intermittent pressurized is extracted twice.Single factor experiment result further demonstrates the superiority of technique of the present invention.
Embodiment 20 oil tea medicinal granules formula optimization test
For confirming the superiority of technique of the present invention further, the present embodiment is verified by formula optimization experiment. In conjunction with preparing the conventional auxiliary material of medicinal granules and consider the activeconstituents in the oil tea extraction concentrated solution extracted and itself local flavor, emphasis considers the limits reservation of nutritive ingredient and the preferred of local flavor, the present invention is by a large amount of early-stage Study, determine to add Zulkovsky starch embedding bitter substance, add gum arabic, glucose powder as vehicle, add citric acid and regulate local flavor, obtaining the optimum formula of oil tea medicinal granules with anti-oxidant activity, the organoleptic qualities such as the fragrance of auxiliary material and oil tea extraction concentrated solution, taste bring out the best in each other.
In the formula of described oil tea medicinal granules, each composition weight percent is: concentrated solution 10%��70%, Zulkovsky starch 1%��5%, gum arabic 10%��40%, glucose powder 10%��70%, citric acid 0.5%��3%, described concentrated solution obtains by oil tea anti-oxidant activity stoste is concentrated. Screening formulation is: concentrated solution 30%��50%, Zulkovsky starch 1%��2%, gum arabic 10%��20%, glucose powder 30%��50%, citric acid 0.5%��1.5%. The present embodiment, taking the interpolation weight percent of oil tea extraction concentrated solution, Zulkovsky starch, gum arabic, glucose powder and citric acid as factor, selects L18(35) orthogonal design table carry out formula optimization test checking. The anti-oxidant medicinal granules of oil tea is prepared according to processing sequence after allotment, each formula gets 15g particle, add 100mL warm water dissolved, 10 are allowed to have the insider of trial test experience to taste, taking the sense organ state of medicinal granules, dissolved property, dissolved after color and luster, flavour and smell etc. carry out evaluating as evaluation index and give a mark, finally obtaining comprehensive grading, experimental result is shown in Table 3.
Table 3 is filled a prescription preferred orthogonal design table
Can optimize, by range analysis, the optimum proportioning obtaining oil tea medicinal granules formula by the data of table 3 is: oil tea extracts concentrated solution 40%, Zulkovsky starch 1.5%, gum arabic 18%, glucose powder 40% and citric acid 0.5%.
Embodiment 21 oil tea medicinal granules product quality analysis
Oil tea medicinal granules the present invention obtained randomly draws the analysis that product carries out Oranoleptic indicator, microbiological indicator and antioxidant property.
(1) Oranoleptic indicator: the color and luster of the anti-oxidant medicinal granules of oil tea, tissue morphology, granularity, flavour and brew are evaluated. Color and luster: particle is brown, and color and luster is consistent; After reconstituting, decoction is light brown; Tissue morphology: outward appearance is dry, uniform particles; Inclusion-free, phenomenon of making moist without caking; Granularity: 14��30 object particle accountings more than 95%; Flavour: after reconstituting, decoction flavour is good to eat, and has the peculiar fragrance of oil tea, without other strange taste; Brew: brew is good, it is possible to comparatively fast dissolve, the impurity such as considers to be worth doing without Jiao at the bottom of soup.
(2) microbiological indicator: after testing, result is total plate count (cfu/g)��100/g, and intestinal bacteria (MPN/100g)��30, without pathogenic bacterium detection.
(3) antioxidant property: get the anti-oxidant medicinal granules of oil tea of the present invention, reconstitutes as a series of different concns taking warm water, measure sample liquid reducing power and to the Scavenging activity of free radical.
1. the reducing power of oil tea medicinal granules measures
2.5mLpH=6.6 phosphoric acid buffer adds 1ml sample liquid (diluting certain sample liquid gradient) and 1mL1% potassium ferricyanide solution, after mixture being heated 20min under 50 DEG C of constant temperatures after mixing, cool rapidly, add 2.5mL10% trichoroacetic acid(TCA), centrifugation 10min.Get supernatant liquid 5ml, add 5ml water and 1ml0.1% ferric chloride Solution successively, mix, after leaving standstill 10min, under wavelength 710nm, measure light absorption value (A). A value is more big, then the reducing power of sample is more strong. Test taking the xitix of lower concentration 0.05mg/mL as comparison. Experimental result is as shown in Figure 12.
Can obtaining by accompanying drawing 12, the reducing power of oil tea medicinal granules of the present invention is very strong, and the reducing power reconstituting the decoction of rear 4g/100mL is equivalent to the ascorbic acid solution of 0.005g/100mL.
2. oil tea medicinal granules removes the effect of DPPH free radical
It is 1 �� 10 by concentration-4The DPPH ethanol solution 3.0mL of M mixes with the sample liquid of 0.1mL different concns, shakes even, and room temperature, darkroom reaction 30min, measure its 517nm place light absorption value (A) with dehydrated alcohol zeroing. Light absorption value (the A of the light absorption value (B) of Simultaneously test 0.1mL sample liquid and 3.0mL dehydrated alcohol mixed solution and 0.1mL dehydrated alcohol and 3.0mLDPPH alcoholic solution mixed solution0). Sample is to clearance rate (%)=[1-(the A-B)/A of DPPH free radical0] �� 100 (%). Experimental result is as shown in Figure 13. Can obtaining by accompanying drawing 13, the clearance rate of DPPH free radical is improved by oil tea medicinal granules of the present invention with the increase of concentration, and the clearance rate of DPPH just can be reached more than 95% by the decoction of 10g/100mL concentration.
3. oil tea medicinal granules removes the effect of OH free radical
Get the test tube of some 25mL, it is sequentially added into 9mmol/LFeSO4Solution 0.5mL, 9mmol/L Whitfield's ointment-ethanolic soln 0.5mL, the sample liquid 0.5mL of different mass concentration, 8.8mmol/LH2O2Solution 5mL, then supplement 3.5mL distilled water. Add H2O2Start reaction, under 37 DEG C of water-baths, react 0.5h. Take distilled water as blank, measure the absorbance A of sample at 510nm place1. Replacing sample liquid with distilled water, absorbancy is designated as A0. Consider the light absorption value of sample liquid itself, with 0.5mL9mmol/LFeSO4, 0.5mL9mmol/L Whitfield's ointment-ethanol, the sample liquid of 0.5mL different concns and 8.5mL distilled water is as the background absorption value A of sample liquid2. It is calculated as follows its clearance rate (%)=[A0-(A1-A2)]/A0�� 100 (%). Experimental result is as shown in figure 14. Can obtaining by accompanying drawing 14, the clearance rate of OH free radical is improved by oil tea medicinal granules of the present invention with the increase of concentration, and the clearance rate of OH can be reached more than 95% by the decoction of 10g/100mL concentration.
4. oil tea medicinal granules removes O2 -The effect of free radical
By 4.5mL0.05mol/LTris-HCL (pH8.2) in 25 DEG C of water-baths after preheating 20min, respectively to wherein adding 0.5mL sample liquid and 0.5mL25mmol/L pyrogallol solution, mixed even and in 25 DEG C of water-baths accurate response 5min, immediately by the HCL termination reaction of 2 8.0mol/L, by the zero point of deionized water conditioning instrumentation, at wavelength 325nm place, the absorbance A i of assaying reaction system; Separately in the Tris-HCL (pH8.2) of preheating 20min, add 0.5mL test liquid, after mixed even, in 25 DEG C of water-baths, after accurate response 5min, survey its absorbance A j in 325nm; The Tris-HCL (pH8.2) of preheating 20min adds 0.5mL distilled water and 0.5mL25mmol/L pyrogallol mix even after in 25 DEG C of water-baths accurate response 5min, in contrast, survey its absorbance A c in 325nm. According to following formulae discovery absorbancy: clearance rate %=[1-(Ai-Aj)/Ac] �� 100 (%). Experimental result is as shown in figure 14.
Can obtaining by accompanying drawing 14, oil tea medicinal granules of the present invention is to O2 -The clearance rate of free radical improves with the increase of concentration, and the decoction of 10g/100mL is to O2 -Clearance rate can reach more than 95%.
The preparation of embodiment 22 oil tea medicinal granules
The present embodiment provides the manufacture embodiment of oil tea medicinal granules entirety, and process flow diagram is as shown in Figure 1. Specifically, comprise the following steps:
S1. oil tea is plucked and selects removal of impurities: pluck just open Thistle oil camellia; Select the oil tea that each organ sites is complete; Remove the impurity such as the blade being wherein mingled with, careless bits;
S2. complete drying treatment: adopts microwave hot air combined drying process, and drying conditions is: microwave power 350W, microwave time 30S, temperature 50 DEG C, dry 12h, and dried oil tea water content is 6.2%; Then adopt medicinal herb grinder to pulverize, cross 60 order sieves, obtain dry oil tea pollen;
S3. oil tea anti-oxidant activity stoste preparation: taking above-mentioned dry oil tea pollen as raw material, alcohol-water using 60% is as Extraction solvent, vacuum aided is adopted to extract the antioxidant component in oil tea, obtain oil tea anti-oxidant activity stoste, extraction conditions is solid-liquid ratio 1g:35mL, vacuum tightness 0.7Mpa, Extracting temperature 75 DEG C, extraction time 30min;
S4. extracting solution concentrates: S3 extracting the oil tea anti-oxidant activity stoste obtained and carries out cryogenic vacuum concentration, condition is 50 DEG C, 10Kpa, and recording soluble solid content in final concentrated solution is 38%;
S5. allocate: get the concentrated solution that S4 obtains, add Zulkovsky starch embedding bitter substance, heating in water bath, stirring under 50 DEG C of conditions so that it is fully dissolve; Add citric acid again to dissolve; Finally the concentrated solution mixed is joined with the form of spraying in the vehicle (gum arabic and glucose powder) pulverizing 120 order sieves in advance, fully mix in mixing machine; Formula rate is that oil tea extracts concentrated solution 40%, Zulkovsky starch 1.5%, gum arabic 18%, glucose powder 40% and citric acid 0.5%;
S6. granulation, drying: get the material that S5 mixes and fully rub evenly; softwood is put into granulation in Pendulargranulator; then 20 order net sieve crushing and pelletizings are crossed; wet granular after pulverizing is placed in boiling drier drying; drying temperature 70 DEG C; obtaining oil tea medicinal granules, finally recording dried pellet moisture content is 2.8%.
S7. detect the granularity of products obtained therefrom, consider impurity etc. to be worth doing with or without Jiao, and microbiological indicator whether conformance with standard. Get 10g particle, reconstitute with 100mL warm water, the antioxidant component polyphenol content measured after cooling in decoction to be 310mg/100mL, flavones content be 385mg/100mL, polysaccharide content are 767mg/100mL, anthocyanidin content is 38mg/100mL, to DPPH, OH, O2 -The clearance rate of free radical improves with the increase of concentration, and the decoction of 10g/100mL is to O2 -Clearance rate can reach more than 95%.
Claims (10)
1. an oil tea anti-oxidant activity stoste, it is characterised in that, be prepare by the following method:
S1. taking green oil camellia as raw material, dry after selected removal of impurities, pulverize, obtain oil tea pollen;
S2. by step S1 gained oil tea pollen using alcohol-water as Extraction solvent, oil tea anti-oxidant activity stoste is obtained through vacuum aided extraction or ultra-high voltage two assisted extraction;
Wherein, the condition that vacuum aided described in step S2 is extracted is: the granularity of oil tea pollen is 20��120 orders, ethanol-water solution taking volume fraction as 20%��90% is for Extraction solvent, according to 1g oil tea pollen: the mixing of the ratio of the solid-liquid ratio of 10��50mL Extraction solvent, Extracting temperature be 30��90 DEG C, vacuum tightness be 0.1��0.9MPa when extract 10��50min;
Or, described in step S2, the condition of ultra-high voltage two assisted extraction is: the granularity of oil tea pollen is 20��120 orders, ethanol-water solution taking volume fraction as 20%��90% is for Extraction solvent, according to 1g oil tea pollen: the ratio mixing of the solid-liquid ratio of 10��50mL Extraction solvent, extracting, pressure is 100��700MPa, intermittent pressurized extracts 2 times under Extracting temperature is 20��80 DEG C of conditions, extracts 2��10min altogether.
2. oil tea anti-oxidant activity stoste according to claim 1, it is characterised in that, pluck fresh oil tea described in step S1 and for Thistle oil camellia or common spend oil tea in vain; Selecting removal of impurities described in step S1 is select wherein without the complete oil tea of disease and pest, nothing breakage, and removes the blade being mingled with or grass bits.
3. oil tea anti-oxidant activity stoste according to claim 1, it is characterised in that, drying described in step S1 adopts microwave hot air combined drying process, drying conditions is: microwave power 350W, microwave time 30S, temperature 50 DEG C, dry 12h, dried oil tea water content is less than 8%.
4. oil tea anti-oxidant activity stoste according to claim 1, it is characterised in that, in step S2, when adopting vacuum aided to extract, the ethanol-water solution taking volume fraction as 60%��70% is for Extraction solvent; Solid-liquid ratio is 1g oil tea pollen: 30��40mL Extraction solvent; Extraction time is 30��40min; Extracting temperature is 70��80 DEG C; Vacuum tightness is 0.6��0.7MPa.
5. oil tea anti-oxidant activity stoste according to claim 1, it is characterized in that, in step S2, when adopting ultra-high voltage two assisted extraction, adopting grinding particle size to be 80��100 dry oil tea pollen of objects is raw material, and the ethanol-water solution taking volume fraction as 50%��60% is for Extraction solvent; Solid-liquid ratio is 1g oil tea pollen: 30��40mL Extraction solvent; Extraction pressure is 300��400Mpa; Extraction time is 6��8min; Extracting temperature is 40��50 DEG C.
6. one kind has the oil tea medicinal granules of anti-oxidant activity, it is characterised in that, it is made up of each component of following weight percent:
The concentrated solution 10%��70% of the described oil tea anti-oxidant activity stoste of the arbitrary item of claim 1 to 5;
Wherein, the concentrated solution of described oil tea anti-oxidant activity stoste is concentrated to wherein soluble solid mass percent by oil tea anti-oxidant activity stoste and reaches 35��40% and get final product.
7. there is the oil tea medicinal granules of anti-oxidant activity according to claim 6, it is characterised in that, described oil tea medicinal granules is made up of each component of following weight percent:
8. there is the oil tea medicinal granules of anti-oxidant activity according to claim 6, it is characterised in that, described oil tea medicinal granules is made up of each component of following weight percent:
Preferably, described Icing Sugar can adopt glucose powder.
9. the preparation method of the described oil tea medicinal granules of the arbitrary item of claim 6 to 8, it is characterized in that, Zulkovsky starch is added in the concentrated solution of oil tea anti-oxidant activity stoste, fully stir under keeping the temperature condition of 50 DEG C��60 DEG C, add citric acid and dissolve, deployed mixture is added with spray pattern in the gum arabic mixed and Icing Sugar, then all materials are dropped in mixing machine, fully mix, granulating and forming, it is drying to obtain.
10. the application of the described oil tea medicinal granules of the arbitrary item of claim 6 to 8, it is characterised in that, obtained beverage after described oil tea medicinal granules is reconstituted according to 1g:20mL boiling water.
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| CN111184097A (en) * | 2020-03-11 | 2020-05-22 | 广东仙塘红茶业有限公司 | Technology for extracting and purifying tea polyphenol of ancient mountain tree and preparation process of antioxidant granules |
| CN114271486A (en) * | 2020-09-27 | 2022-04-05 | 中方县瑶山青钱柳农业开发有限公司 | Instant cyclocarya paliurus powder |
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| CN116650579A (en) * | 2023-05-31 | 2023-08-29 | 常山富而康山茶油有限公司 | Application of oil tea flower extract in aspects of freckle removal, whitening and anti-saccharification |
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