CN110283663B - Production process of rosemary extract - Google Patents
Production process of rosemary extract Download PDFInfo
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- CN110283663B CN110283663B CN201910547152.6A CN201910547152A CN110283663B CN 110283663 B CN110283663 B CN 110283663B CN 201910547152 A CN201910547152 A CN 201910547152A CN 110283663 B CN110283663 B CN 110283663B
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
- C11B9/02—Recovery or refining of essential oils from raw materials
- C11B9/025—Recovery by solvent extraction
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
- C11B9/02—Recovery or refining of essential oils from raw materials
- C11B9/027—Recovery of volatiles by distillation or stripping
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Abstract
The invention discloses a production process of rosemary extract, which comprises the following steps: (1) Smashing dry rosemary leaves, adding a mixed solvent for infiltration and stirring to obtain a mixture, wherein the mixed solvent is as follows: food grade ethanol, food grade ethyl acetate, food grade 1, 2-dichloroethane, food grade acetone; (2) Feeding the mixture into a continuous dynamic countercurrent extraction unit to obtain an extracting solution and filter residues; vacuum drying the filter residue to recover the mixed solvent; (3) Filtering the extractive solution to obtain filtrate, vacuum concentrating the filtrate, recovering mixed solvent, cooling the residual solution, and centrifuging to obtain crude herba Rosmarini officinalis extract; (4) Dissolving the crude rosemary extract in food-grade n-hexane, heating, filtering, and vacuum concentrating to obtain refined rosemary extract; (5) Adding edible salad oil and distilled water into the rosemary extract refined product, and performing membrane distillation to obtain the rosemary extract. The extraction rate of the effective components in the production process is more than or equal to 99.5 percent, and the organic solvent residue in the rosemary extract is less than or equal to 10ppm.
Description
Technical Field
The invention relates to the field of natural plant extracts, in particular to a production process of a rosemary extract.
Background
Rosemary (Rosemarinus) is a labiate herbaceous plant, is introduced and cultivated in China of south Europe, hunan, guizhou, hainan, guangxi, guangdong provinces and other provinces and markets in China, and contains various effective components such as carnosic acid, rosmanol, rosmarinic acid, carnosol, epi-rosmanol, isorosmanol, rosemary diphenol and the like, wherein the high-efficiency antioxidant substances are carnosic acid, rosmanol, carnosol and the like. The fat-soluble rosemary extract is light yellow to tawny powder or brown paste, is insoluble in water, and is soluble in ethanol and grease; the water-soluble rosemary extract is brown powder, and has peculiar smell of rosemary. The heat resistance (stable at 200 ℃) and the ultraviolet resistance are good, and the oxidation of grease can be effectively prevented.
The rosemary extract can be divided into oil-soluble (antioxidant) and water-soluble (antioxidant and antiseptic), wherein the former is mainly carnosic acid, and the latter is mainly rosmanol. The rosemary extract is natural and nontoxic, has the antioxidant effect far higher than that of the existing natural antioxidants such as vitamin C, vitamin E, tea polyphenol and the like, is 2-4 times that of the artificially synthesized antioxidants BHA and BHT, has stable structure and difficult decomposition, can resist the high temperature of 190-240 ℃, thoroughly overcomes the consistent weakness that most of the natural antioxidants such as the vitamin C, the tea polyphenol and the like are decomposed at high temperature, and has the advantages of higher efficiency and broad spectrum compared with other similar products. The investigators found that rosemary extract at 300mg/kg had antioxidant activity equivalent to 200mg/kg BHA, greater than 100mg/kg tocopherol. Generally, the antioxidant capacity of the food is increased with the increase of the addition amount, but the high concentration can cause the precipitation of grease and the discoloration of the water-containing food. The antioxidant function of rosemary mainly lies in that rosemary can quench singlet oxygen, clear free radicals, chelate metal ions, synergize organic acid and the like. The rosemary is scientifically proved to be the most safe and efficient natural antioxidant which is generally accepted in the world at present. Is 20 times of TBHQ. Widely applied to the fields of food, medicine, health products, skin care, daily chemicals and the like, and European Union (EU) regulations list rosemary extracts as organic food antioxidants and preservatives.
At present, the traditional extraction process is generally adopted in domestic rosemary extract extraction production technology and equipment, and mainly comprises a traditional organic solvent extraction method, a homogenate extraction method, an ultrasonic auxiliary extraction method, a supercritical carbon dioxide extraction method and the like.
The organic solvent extraction method comprises pulverizing dry leaves of herba Rosmarini officinalis, adding herba Rosmarini officinalis powder into extraction tank, adding 6 times, 5 times, and 4 times of organic solvent into the extraction tank, respectively, extracting under reflux for three times, concentrating the extractive solution in concentrator to obtain extract; the organic solvent extraction method has the disadvantages of relatively low extraction efficiency, small amount of organic solvent remained in rosemary extract, long extraction time, large solvent consumption, high labor intensity of operators and easy damage of heat-sensitive components.
The homogenate extraction method mixes homogenate with fresh rosemary leaf and extraction solvent in homogenate extraction device, adds inorganic acid or organic acid in the system and adjusts pH value to 3, and the material-liquid ratio is 1 12, tears the material and smashes through machinery and hydraulic shearing action, makes the material breakage and active ingredient's extraction go on in step to reach and draw the plant active ingredient fast, sends the feed liquid of extracting into the concentrator and concentrates, obtains rosemary and draws the thing extract. The homogenate extraction omits the steps of drying and crushing the materials, has simple operation, and has reference significance for extracting natural products from other fresh plant materials. However, the method still has the defects of high energy consumption, difficult post-treatment and small amount of organic solvent remained in the rosemary extract.
The ultrasonic-assisted extraction method is an enhancement means of the traditional solvent extraction, and the ultrasonic waves generate strong vibration, strong cavitation, stirring and the like to cause the damage of plant cell walls and the rapid penetration of the solvent, so that the antioxidant ingredients in the extracted rosemary leaves are rapidly dissolved in the solvent. At present, the method is only limited to a few extraction experiments and does not have industrial large-scale production.
The supercritical carbon dioxide extraction method is characterized in that compressible high-density carbon dioxide fluid in a state of above a critical temperature and a critical pressure (called critical point) is contacted with a separated substance, and due to the fact that the solubility of the substance in the supercritical fluid is greatly influenced by the pressure and the temperature, components with polarity, boiling point and relative molecular mass are selectively and sequentially extracted, and therefore the purposes of separation and purification are achieved. And (3) loading the crushed crude rosemary extract into a multi-layer simple material extraction kettle, adding a proper amount of ethanol or ethyl acetate, and extracting at a certain temperature and under a certain pressure to obtain the rosemary extract. At present, the volume of the domestic supercritical extraction equipment is small, the requirement of industrial production cannot be met, and the price of imported equipment is very high. Furthermore, supercritical CO2 extraction is suitable for the separation of non-polar compounds.
The traditional extraction process is to complete leaching in a closed unit, and along with the leaching process, the concentration of a leaching solution is increased, the concentration of a material is reduced (referring to the concentration of soluble substances in the material), the leaching speed is slowed down, and a certain equilibrium state is gradually reached. Therefore, to maintain a certain leaching rate, the solvent must be replaced to replace the already nearly saturated dip. These processes also have drawbacks that are difficult to avoid: the extraction rate is low, and the raw material waste is large; the extraction time is long; the effluent coefficient is large, the burden of subsequent treatment is increased, and the energy consumption is high; the difference between batches is large; the method belongs to intermittent operation, and has poor labor conditions; the solvent residue in the rosemary extract product exceeds the standard. How to solve the problems existing in the prior art has become a difficult research subject to be solved in the field of natural plant extracts.
Disclosure of Invention
The production process of the rosemary extract has the advantages of stable process, high extraction efficiency, extraction rate of effective components of more than or equal to 99.5 percent, less organic solvent residue than or equal to 10ppm in the rosemary extract, short extraction time, less solvent consumption, energy consumption reduction, labor intensity reduction, difficult damage of thermosensitive components, cost saving and unit consumption reduction.
In order to achieve the technical purpose, the technical scheme of the invention is as follows:
a production process of rosemary extract comprises the following steps:
(1) The preparation method comprises the following steps of (1) crushing dry rosemary leaves to 60-100 meshes, putting the crushed dry rosemary leaves into an infiltration tank, adding a mixed solvent, infiltrating and stirring to obtain a mixture, wherein the mixed solvent is as follows: food grade ethanol, food grade ethyl acetate, food grade 1, 2-dichloroethane and food grade acetone, wherein the volume ratio of the ethanol to the ethyl acetate is (2-5): 1 to 5:1 to 5:1 to 5;
(2) Feeding the mixture into a continuous dynamic countercurrent extraction unit, and adding a mixed solvent in a countercurrent manner for extraction to obtain an extracting solution and filter residues; vacuum drying the filter residue to recover the mixed solvent;
(3) Filtering the extractive solution with automatic cylindrical filter to obtain filtrate, vacuum concentrating the filtrate, recovering mixed solvent, cooling the residual solution, and centrifuging to obtain crude herba Rosmarini officinalis extract;
(4) Dissolving the coarse rosemary extract product in food level hexane, heating at 50-60 deg.c, filtering and vacuum concentrating to obtain fine rosemary extract product;
(5) Adding edible salad oil and distilled water into the fine rosemary extract product, and removing solvent residues and rosemary essential oil by membrane distillation to obtain the rosemary extract.
Preferably, in the step (1), the solid-to-liquid ratio of the dry rosemary leaves to the mixed solvent is 1 kg/2-4L.
Preferably, in step (2), the continuous dynamic countercurrent extraction unit: extraction processing amount: 50-200 kg/h; extraction temperature: 40 to 55 ℃; extraction time: the whole process lasts for 2-3 h; the solid-liquid ratio of the dry rosemary leaves in the mixture to the mixed solvent is 1 kg/4-6L.
The working principle of the continuous dynamic countercurrent extraction unit is as follows:
the formula of leaching and diffusing components is as follows: g = [ < D >. Times > F × (C1-C2) × (t ]/[ delta ]/]
Wherein G is a diffusion substance, t is diffusion time, F is a diffusion surface and represents the granularity and the surface state of the rosemary leaves, (C1-C2) is concentration difference, D is a diffusion coefficient, delta is the thickness of a diffusion layer of the rosemary leaves, and the minus sign represents the reduction of the concentration when the diffusion is towards equilibrium, so that the value of D is in direct proportion to the crushing degree, the surface state, the concentration difference in the diffusion process, the diffusion time and the diffusion coefficient of the rosemary leaves, if C1= C2, C1-C2=0, the concentration and difference are equal to zero, namely, the rosemary leaves are in a saturated state, all other conditions lose effects, the time is longer, the temperature is higher, and the leaching components are equal to zero. The rosemary leaves are crushed into powder of 60-100 meshes, the powder is uniformly fed into one end of a continuous dynamic countercurrent extraction unit through a quantitative feeder, the powder is slowly pushed to the other end of the unit through a conveying device with a spiral blade, the powder is automatically discharged according to a certain time required by the process, and a solvent is quantitatively controlled and added from one end of the unit through a flow meter according to the process requirement, so that the directions of the rosemary leaf powder and the solvent are completely opposite. In operation, the rosemary leaf powder is continuously stirred forward under the action of the propeller to replace and rub with the solvent, and the diffused interface is continuously updated, so that the maximum concentration difference is obtained in the whole extraction process, the extraction time is shortened, and the yield of the leaching components is improved.
The working process of the continuous dynamic countercurrent extraction unit is as follows:
the rosemary leaf powder is fed into a feeding port of a continuous dynamic countercurrent extraction unit through a quantitative feeder, the rosemary leaf powder is pushed towards a discharging device under the action of a spiral propeller in a tank body, then slag is discharged from the discharging device and enters a juice squeezer for treatment, and then waste recovery solvent treatment is carried out. And the mixed solvent is quantitatively added from a solvent inlet according to the solid-to-liquid ratio required by the rosemary leaf powder by a flowmeter. The two directions are opposite. The extracting solution (containing slag) is pumped into a drum type filter through an infusion pump for filtering, the filtered slag enters a discharging device part at the front end of the unit and is discharged by the discharging device, and the filtered extracting solution flows into a finished product storage tank and is conveyed to the lower process by a secondary infusion pump.
Preferably, in the step (3), when the recovered mixed solvent is 50% to 80% of the total amount of the mixed solvent added in the steps (1) and (2) in vacuum concentration, the ratio of the volume of the distilled water to the volume of the filtrate is 0.5 to 0.8:1 distilled water was added to continue recovering the remaining mixed solvent.
Preferably, in the step (4), the solid-to-liquid ratio of the crude rosemary extract to food-grade n-hexane is 1kg/7 to 10L.
Preferably, in the step (5), the solid-to-liquid ratio of the rosemary extract essence to the edible salad oil and the distilled water is 1 kg/2-5L/1-3L.
Preferably, in the step (5), the membrane distillation specifically comprises the following steps: distilling by using a vacuum membrane, adopting three-stage separation, wherein the treatment capacity of the first-stage distillation is 100-200L/h, the porosity of the membrane is 60-85%, the average pore diameter of the membrane is 0.1-0.5 mu m, the distillation temperature is 60-80 ℃, and the distillation vacuum degree is 20-50 Pa; the secondary distillation treatment capacity is 100-200L/h, the porosity of the membrane is 60-85%, the average pore diameter of the membrane is 0.1-0.5 mu m, the distillation temperature is 80-90 ℃, and the distillation vacuum degree is 30-50 Pa; the secondary distillation treatment capacity is 100-120L/h, the porosity of the membrane is 60-85%, the average pore diameter of the membrane is 0.1-0.5 mu m, the distillation temperature is 85-95 ℃, and the distillation vacuum degree is 35-50 Pa.
The working principle of the membrane distillation adopted by the invention is as follows:
the principle of membrane distillation is a separation process combining membrane technology with a distillation process. One side of the membrane is directly contacted with a hot solution to be treated (called a hot side), the other side of the membrane is directly or indirectly contacted with a cold solution (called a cold side), volatile components in the solution at the hot side are vaporized at the membrane surface, pass through the membrane, enter the cold side and are condensed into a liquid phase, and other components are blocked at the hot side by a hydrophobic membrane, so that the aim of separating or purifying the mixture is fulfilled. The membrane distillation process must have the following characteristics to distinguish it from other membrane processes: (1) the film used is a microporous film; (2) the membrane is not wettable by the liquid being treated; (3) no capillary condensation occurs in the membrane pores; (4) only steam can transfer mass through the membrane pores; (5) the used membrane can not change the gas-liquid balance of all components in the treated liquid; (6) at least one side of the membrane is in contact with the liquid to be treated; (7) the driving force for the membrane process for any component is the partial pressure difference of that component in the gas phase.
The rosemary extract and the sunflower seed oil are nonvolatile substances, the distillate is water, a small amount of solvent residue and rosemary essential oil components, and the three-stage vacuum membrane distillation is adopted to complete the process.
The rosemary extract is dissolved in the salad oil and contains 1 to 2 percent of solvent and rosemary essential oil, and after membrane distillation, the residual amount of the solvent in the product is less than or equal to 10ppm, thereby meeting the quality requirement.
Preferably, the extraction rate of the active ingredients of the rosemary extract obtained after the treatment of the dry leaves of the rosemary is more than or equal to 99.50 percent, and the solvent residue is less than or equal to 10ppm.
Compared with the prior art, the invention has the beneficial effects that:
(1) Compared with the traditional extraction process, the extraction rate of the effective components of the rosemary leaves is improved by about 10-20%, the extraction process is uniform in heating and can be leached at low temperature, and the thermosensitive components are kept from being damaged; the product quality is stable, the equipment continuously works, and the defect of difference among batches is overcome; the extraction rate of the effective components of the rosemary extract obtained after the treatment of the dry leaves of the rosemary is more than or equal to 99.50 percent, and the solvent residue is less than or equal to 10ppm.
(2) The liquid outlet coefficient of the extraction process is small (generally controlled between 5 and 8 times), while the liquid outlet coefficient of the traditional extraction process is large (generally controlled between 18 and 30 times), so that the steam consumption and the solvent recovery loss required by heating the solvent in excess times are saved; meanwhile, the concentration time and the steam consumption of the subsequent process (evaporation equipment) can be greatly reduced, and the utilization rate of the evaporation equipment is improved.
Drawings
Fig. 1 is a flow chart of the production process of rosemary extract.
FIG. 2 is a schematic diagram of the operation of the present invention using membrane distillation.
Detailed Description
Example 1
(1) 100kg of dry rosemary leaves are crushed into 60 to 100 meshes, the dry rosemary leaves contain 3.65 percent of carnosic acid, the mixture is put into an infiltration tank, 200L of mixed solvent (80L of food grade ethanol, 40L of food grade ethyl acetate, 40L of food grade 1, 2-dichloroethane and 40L of food grade acetone) is added, and the mixture is stirred for 30 minutes;
(2) Feeding into a feeding port of a continuous dynamic countercurrent extraction unit by a quantitative feeder, pushing a discharging device under the action of a screw propeller in a tank body, and quantitatively adding 400L of mixed solvent (160L of food grade ethanol, 80L of food grade ethyl acetate, 80L of food grade 1, 2-dichloroethane, and 80L of food grade acetone) into a solvent liquid inlet through a flow meter. Extracting at 40 deg.C for 2 hr;
(3) Then discharging the slag materials from a discharging device, treating the slag materials in a juice squeezing machine, and then performing waste recovery solvent treatment to obtain 60kg of waste slag and 15L of mixed solvent;
(4) The extract passes through a drum type automatic filter (a filter screen with 500-600 meshes) to obtain 620L of filtrate;
(5) Concentrating 620L filtrate in a reaction cylinder under vacuum (-0.05 to-0.095 Mpa), recovering mixed solvent, adding 300L distilled water when the recovered mixed solvent reaches 445L, and recovering the residual 150L mixed solvent and 60L water;
(6) Transferring the materials in the reaction cylinder into a crystallization cylinder after recovery, cooling the materials to 20-30 ℃, and performing centrifugal separation to obtain 21.5kg of crude rosemary extract; the centrifuged filtrate is used to produce rosmarinic acid.
(7) Dissolving 21.5kg of crude rosemary extract in 150L of food grade n-hexane, heating and filtering to obtain filter residue; concentrating the filtrate under vacuum (-0.05-0.095 Mpa) to obtain refined rosemary extract 12.5kg;
(8) Adding 17.5kg sunflower seed oil and 12.5kg distilled water into 12.5kg fine rosemary extract, distilling under reduced pressure membrane, and removing water, solvent residue 12.85kg and rosemary essential oil 0.32kg by three-stage separation; to obtain 29.33kg of rosemary extract, the carnosic acid content is 12.39%.
(9) 29.33kg of rosemary extract treated by the membrane distillation process is prepared into 36.34kg of carnosic acid with the content of 10 percent. The extraction rate of the effective components is 99.56%.
Example 2
(1) Crushing 100kg of dry rosemary leaves containing 3.65 percent of carnosic acid into 60-100 meshes, putting the crushed dry rosemary leaves into an infiltration tank, adding 300L of mixed solvent (food grade ethanol 135L, food grade ethyl acetate 75L, food grade 1, 2-dichloroethane 45L and food grade acetone 45L), and stirring for 30 minutes;
(2) Feeding into a feeding port of a continuous dynamic countercurrent extraction unit by a quantitative feeder, pushing the discharging device under the action of a screw propeller in the tank body, and quantitatively adding 500L of mixed solvent (food grade ethanol 225L, food grade ethyl acetate 125L, food grade 1, 2-dichloroethane 75L and food grade acetone 75L) into the mixed solvent from a solvent inlet by a flow meter. Extracting at 50 deg.C for 2.5 hr;
(3) Then discharging the slag from a discharging device, treating the slag in a juice extractor, and performing waste recovery solvent treatment to obtain 58kg of waste slag and 14L of mixed solvent;
(4) The extract passes through a cylinder type automatic filter (a filter screen with 500-600 meshes) to obtain 846L of filtrate;
(5) 846L of filtrate is concentrated under vacuum (-0.05 to-0.095 Mpa) in a reaction cylinder, mixed solvent is recovered, when the recovered mixed solvent reaches 615L, 450L of distilled water is added, and 180L of mixed solvent and 135L of water are remained after recovery;
(6) Transferring the materials in the reaction cylinder into a crystallization cylinder after recovery, cooling the materials to 20-30 ℃, and performing centrifugal separation to obtain 21.0kg of crude rosemary extract; the centrifuged filtrate is used to produce rosmarinic acid.
(7) Dissolving 21.0kg of crude rosemary extract in 175L of food grade n-hexane, heating and filtering to obtain filter residue; concentrating the filtrate under vacuum (-0.05-0.095 Mpa) to obtain refined rosemary extract 12.0kg;
(8) 12.0kg of rosemary extract essence is added with 18.0kg of sunflower seed oil and 24.0kg of distilled water, and then the mixture is distilled by a vacuum membrane, and water, solvent residue 24.3kg and rosemary essential oil 0.30kg are removed by three-stage separation; 29.4kg of rosemary extract is obtained, and the carnosic acid content is 12.38%.
(9) 29.4kg of rosemary extract treated by the membrane distillation process is prepared into 36.40kg of carnosic acid with the content of 10 percent. The extraction rate of the effective components is 99.73 percent.
Example 3
(1) Crushing 100kg of dry rosemary leaves containing 3.65% carnosic acid into 60-100 meshes, putting the crushed dry rosemary leaves into an infiltration tank, adding 400L of a mixed solvent (200L of food grade ethanol, 120L of food grade ethyl acetate, 40L of food grade 1, 2-dichloroethane and 40L of food grade acetone) into the tank, and stirring the mixture for 30 minutes;
(2) Feeding into a feeding port of a continuous dynamic countercurrent extraction unit by a quantitative feeder, pushing a discharging device in the tank body under the action of a screw propeller, and quantitatively adding 600L of mixed solvent (food grade ethanol 300L, food grade ethyl acetate 180L, food grade 1, 2-dichloroethane 60L and food grade acetone 60L) into a solvent liquid inlet by a flow meter. Extracting at 55 deg.C for 3 hr;
(3) Then discharging the slag materials from a discharging device, treating the slag materials in a juice squeezing machine, and then performing waste recovery solvent treatment to obtain 56kg of waste residues and 13L of mixed solvent;
(4) The extract passes through a cylinder type automatic filter (a filter screen with 500-600 meshes) to obtain 1020L of filtrate;
(5) Concentrating 1020L filtrate in reaction cylinder under vacuum (-0.05-0.095 Mpa), recovering mixed solvent, adding 650L distilled water when the recovered mixed solvent reaches 650L, and recovering 300L mixed solvent and 250L water;
(6) Transferring the materials in the reaction cylinder into a crystallizing cylinder after recovery, cooling the materials to 20-30 ℃, and performing centrifugal separation to obtain 20.50kg of crude rosemary extract; the centrifuged filtrate is used to produce rosmarinic acid.
(7) Dissolving 20.5kg of crude herba Rosmarini officinalis extract in 200L of food grade n-hexane, heating, and filtering to obtain filter residue; concentrating the filtrate under vacuum (-0.05-0.095 Mpa) to obtain refined rosemary extract 11.50kg;
(8) Adding 18.5kg sunflower seed oil and 34.5kg distilled water into 11.5kg fine rosemary extract, distilling under reduced pressure membrane, and removing water, solvent residue 34.9kg and rosemary essential oil 0.45kg by three-stage separation; 29.15kg of rosemary extract is obtained, and the content of carnosic acid is 12.46 percent.
(9) 29.15kg of rosemary extract treated by the membrane distillation process is prepared into 36.32kg of carnosic acid with the content of 10 percent. The extraction rate of the effective components is 99.51 percent.
Comparative example 1
(1) Crushing 100kg of dry rosemary leaves to 60-100 meshes, wherein the dry rosemary leaves contain 3.65 percent of carnosic acid, putting the dry rosemary leaves into an extraction tank, adding 1000L of mixed solvent (500L of food grade ethanol, 300L of food grade ethyl acetate, 100L of food grade 1, 2-dichloroethane and 100L of food grade acetone) into the extraction tank, and stirring the mixture for 30 minutes;
(2) Extracting at 55 deg.C for 3 hr;
(3) Discharging slag from the bottom of the extraction tank, and performing waste recovery solvent treatment to obtain 76kg of waste slag and 33L of mixed solvent;
(4) Extracting solution discharged from the bottom of the extracting tank passes through a cylinder type automatic filter (a filter screen with 500-600 meshes) to obtain 950L of filtrate;
(5) 950L of filtrate is concentrated in a concentration cylinder under vacuum (-0.05 to-0.095 Mpa), mixed solvent is recovered, 650L of distilled water is added when the recovered mixed solvent reaches 600L, and 300L of mixed solvent and 250L of water are remained after recovery;
(6) After the recovery, transferring the materials in the reaction cylinder into a crystallization cylinder, cooling the materials to 20-30 ℃, and performing centrifugal separation to obtain 15.50kg of crude rosemary extract; the centrifuged filtrate is used to produce rosmarinic acid.
(7) Dissolving 15.5kg Rosemary extract crude product in 200L food grade n-hexane, heating and filtering to obtain filter residue; vacuum concentrating the filtrate under vacuum (-0.05-0.095 Mpa) to obtain refined rosemary extract 8.50kg;
(8) Adding 17.3kg sunflower seed oil and 12.5kg distilled water into 8.5kg fine rosemary extract, distilling under reduced pressure membrane, and removing water, solvent residue 12.9kg and rosemary essential oil 0.40kg by three-stage separation; 25.0kg of rosemary extract is obtained, and the carnosic acid content is 12.00 percent.
(9) 25.0kg of rosemary extract treated by the membrane distillation process is prepared into 30.00kg of carnosic acid with the content of 10 percent. The extraction rate of the effective components is 82.19 percent.
The comparative example does not adopt a continuous dynamic countercurrent extraction unit, adopts an extraction tank for extraction, adopts the same mixed solvent and the same amount for incomplete extraction, and reduces the extraction rate to 82.19 percent.
Comparative example 2
(1) Crushing 100kg of dry rosemary leaves containing 3.65% carnosic acid into 60-100 meshes, putting the crushed dry rosemary leaves into an infiltration tank, adding 400L of a mixed solvent (200L of food grade ethanol, 120L of food grade ethyl acetate, 40L of food grade 1, 2-dichloroethane and 40L of food grade acetone) into the tank, and stirring the mixture for 30 minutes;
(2) Feeding into a feeding port of a continuous dynamic countercurrent extraction unit by a quantitative feeder, pushing a discharging device in the tank body under the action of a screw propeller, and quantitatively adding 600L of mixed solvent (food grade ethanol 300L, food grade ethyl acetate 180L, food grade 1, 2-dichloroethane 60L and food grade acetone 60L) into a solvent liquid inlet by a flow meter. Extracting at 55 deg.C for 3 hr;
(3) Then discharging the slag materials from a discharging device, treating the slag materials in a juice squeezing machine, and then performing waste recovery solvent treatment to obtain 56kg of waste residues and 13L of mixed solvent;
(4) The extract passes through a cylinder type automatic filter (a filter screen with 500-600 meshes) to obtain 1020L of filtrate;
(5) Concentrating 1020L filtrate in reaction cylinder under vacuum (-0.05-0.095 Mpa), recovering mixed solvent, adding 650L distilled water when the recovered mixed solvent reaches 650L, and recovering 300L mixed solvent and 250L water;
(6) Transferring the materials in the reaction cylinder into a crystallizing cylinder after recovery, cooling the materials to 20-30 ℃, and performing centrifugal separation to obtain 20.50kg of crude rosemary extract; centrifuging the filtrate to produce rosmarinic acid.
(7) Dissolving 20.5kg of crude herba Rosmarini officinalis extract in 200L of food grade n-hexane, heating, and filtering to obtain filter residue; concentrating the filtrate under vacuum (-0.05-0.095 Mpa) to obtain refined rosemary extract 11.50kg;
(8) 11.5kg of refined rosemary extract, 18.4kg of sunflower seed oil and 12.5kg of distilled water are added, and distilled by a distillation still to remove water and leave 12.0kg of solvent; to obtain 29.60kg of rosemary extract, the carnosic acid content is 12.27%.
(9) 29.60kg of rosemary extract treated by the distillation process of a distillation still is prepared into 36.32kg of carnosic acid with the content of 10 percent. The extraction rate of the effective components is 99.51 percent.
The comparative example adopts a continuous dynamic countercurrent extraction unit, does not adopt membrane distillation, but changes a distillation kettle distillation process, the extraction rate is not changed, rosemary essential oil can not be distilled and recovered, and rosemary extract residual solvents (150 ppm of normal hexane, 200ppm of methanol, 300ppm of ethanol, 60ppm of ethyl acetate, 120ppm of 1, 2-dichloroethane and 100ppm of acetone) are unqualified.
Comparative example 3
(1) 100kg of dry rosemary leaves are crushed into 60 to 100 meshes, the dry rosemary leaves contain 3.65 percent of carnosic acid, the mixture is put into an infiltration tank, 400L of food grade ethanol is added, and the mixture is stirred for 30 minutes;
(2) The mixture is fed into a feeding port of a continuous dynamic countercurrent extraction unit through a quantitative feeder, a discharging device is pushed to the inside of the tank body under the action of a spiral propeller, and the mixed solvent is quantitatively added into 600L of food grade ethanol from a solvent liquid inlet through a flow meter. Extracting at 55 deg.C for 3 hr;
(3) Then discharging the slag from a discharging device, treating the slag in a juice extractor, and performing waste recovery solvent treatment to obtain 56kg of waste slag and 13L of mixed solvent;
(4) The extract passes through a cylinder type automatic filter (a filter screen with 500-600 meshes) to obtain 1020L of filtrate;
(5) Concentrating 1020L filtrate in reaction cylinder under vacuum (-0.05-0.095 Mpa), recovering solvent, adding 650L distilled water when the recovered solvent reaches 550L, and recovering 300L mixed solvent and 250L water;
(6) Transferring the material in the reaction tank into a crystallization tank after recovery, cooling the material to 20-30 ℃, and performing centrifugal separation to obtain 20.50kg of crude rosemary extract; the centrifuged filtrate is used to produce rosmarinic acid.
(7) Dissolving 20.5kg of crude rosemary extract in 200L of food grade n-hexane, heating and filtering to obtain filter residue; concentrating the filtrate under vacuum (-0.05-0.095 Mpa) to obtain refined rosemary extract product 9.50kg;
(8) Adding 17.8kg sunflower seed oil and 12.5kg distilled water into 9.5kg fine rosemary extract, distilling under reduced pressure membrane, and removing water, solvent residue 12.9kg and rosemary essential oil 0.40kg by three-stage separation; 26.5kg of rosemary extract is obtained, and the content of carnosic acid is 12.50 percent.
(9) 26.5kg of rosemary extract treated by the membrane distillation process is prepared into 33.125kg of carnosic acid with the content of 10 percent. The extraction rate of the effective components is 90.75 percent.
The comparative example adopts a continuous dynamic countercurrent extraction unit and membrane distillation, does not use a mixed solvent, only uses a single solvent food grade ethanol, and reduces the extraction rate to 90.75 percent.
Comparative example 4
(1) Crushing 100kg of dry rosemary leaves to 60-100 meshes, putting the dry rosemary leaves containing 3.65% of carnosic acid into an infiltration tank, adding 400L of food-grade ethyl acetate, and stirring for 30 minutes;
(2) The mixture is fed into a feeding port of a continuous dynamic countercurrent extraction unit through a quantitative feeder, a discharging device is pushed to the inside of a tank body under the action of a spiral propeller, and 600L of food grade ethyl acetate is quantitatively added into the mixed solvent from a solvent liquid inlet through a flow meter. Extracting at 55 deg.C for 3 hr;
(3) Then discharging the slag materials from a discharging device, treating the slag materials in a juice squeezing machine, and then performing waste recovery solvent treatment to obtain 55kg of waste residues and 15L of mixed solvent;
(4) The extract passes through a cylinder type automatic filter (a filter screen with 500-600 meshes) to obtain 1010L of filtrate;
(5) Concentrating 1010L of filtrate in a reaction cylinder under vacuum (-0.05 to-0.095 Mpa), recovering mixed solvent, adding 650L of distilled water when the recovered solvent reaches 650L, and recovering 320L of solvent and 250L of water;
(6) Transferring the materials in the reaction cylinder into a crystallizing cylinder after recovery, cooling the materials to 20-30 ℃, and performing centrifugal separation to obtain 20.50kg of crude rosemary extract; the centrifuged filtrate is used to produce rosmarinic acid.
(7) Dissolving 20.5kg of crude herba Rosmarini officinalis extract in 200L of food grade n-hexane, heating, and filtering to obtain filter residue; concentrating the filtrate under vacuum (-0.05-0.095 Mpa) to obtain refined rosemary extract product 9.80kg;
(8) Adding 17.8kg sunflower seed oil and 12.5kg distilled water into 9.8kg fine rosemary extract, distilling under reduced pressure, and removing water, solvent residue 12.9kg and rosemary essential oil 0.40kg by three-stage separation; 26.8kg of rosemary extract is obtained, and the content of carnosic acid is 12.25 percent.
(9) 26.8kg of rosemary extract treated by the membrane distillation process is prepared into 32.83kg of carnosic acid with the content of 10 percent. The extraction rate of the effective components is 89.95 percent.
The comparative example adopts a continuous dynamic countercurrent extraction unit and membrane distillation, does not use a mixed solvent, only uses a single solvent food grade ethyl acetate, and reduces the extraction rate to 89.95 percent.
Comparative example 5
(1) 100kg of dry rosemary leaves are crushed into 60 to 100 meshes, the dry rosemary leaves contain 3.65 percent of carnosic acid and are put into an infiltration tank, 400L of food-grade 1, 2-dichloroethane is added and stirred for 30 minutes;
(2) The mixture is fed into a feeding port of a continuous dynamic countercurrent extraction unit through a quantitative feeder, a discharging device is pushed to the inside of a tank body under the action of a spiral propeller, and 600L of food grade 1, 2-dichloroethane is quantitatively added into the mixed solvent from a solvent liquid inlet through a flow meter. Extracting at 55 deg.C for 3 hr;
(3) Then discharging the slag materials from a discharging device, treating the slag materials in a juice squeezing machine, and then performing waste recovery solvent treatment to obtain 55kg of waste residues and 15L of mixed solvent;
(4) The extract passes through a cylinder type automatic filter (a filter screen with 500-600 meshes) to obtain 1010L of filtrate;
(5) Concentrating 1010L of filtrate in a reaction cylinder under vacuum (-0.05 to-0.095 Mpa), recovering the mixed solvent, adding 650L of distilled water when the recovered solvent reaches 650L, and recovering the residual 320L of solvent and 250L of water;
(6) Transferring the material in the reaction tank into a crystallization tank after recovery, cooling the material to 20-30 ℃, and performing centrifugal separation to obtain 20.50kg of crude rosemary extract; the centrifuged filtrate is used to produce rosmarinic acid.
(7) Dissolving 20.5kg of crude herba Rosmarini officinalis extract in 200L of food grade n-hexane, heating, and filtering to obtain filter residue; concentrating the filtrate under vacuum (-0.05-0.095 Mpa) to obtain refined rosemary extract product 10.5kg;
(8) 10.5kg of rosemary extract essence is added with 18.8kg of sunflower seed oil and 12.5kg of distilled water, and the mixture is distilled by a vacuum membrane, and water, solvent residue 12.9kg and rosemary essential oil 0.40kg are removed by three-stage separation; 28.5kg of rosemary extract is obtained, and the carnosic acid content is 11.80%.
(9) 28.5kg of rosemary extract treated by the membrane distillation process is prepared into 33.63kg of carnosic acid with the content of 10 percent. The extraction rate of the effective components is 92.14 percent.
The comparative example adopts a continuous dynamic countercurrent extraction unit and membrane distillation, does not use a mixed solvent, only uses a single solvent and food grade 1, 2-dichloroethane, and reduces the extraction rate to 92.14 percent.
Comparative example 6
(1) Crushing 100kg of dry rosemary leaves to 60-100 meshes, putting the dry rosemary leaves containing 3.65% of carnosic acid into an infiltration tank, adding 400L of food-grade acetone, and stirring for 30 minutes;
(2) The mixed solvent is quantitatively added into a feeding port of the continuous dynamic countercurrent extraction unit through a quantitative feeder, a discharging device is pushed down by the action of a spiral propeller in the tank body, and the mixed solvent is quantitatively added into 600L of food grade acetone from a solvent liquid inlet through a flow meter. Extracting at 55 deg.C for 3 hr;
(3) Then discharging the slag materials from a discharging device, treating the slag materials in a juice squeezing machine, and then recovering a solvent from the waste materials to obtain 55kg of waste residues and 15L of the solvent;
(4) The extract passes through a cylinder type automatic filter (filter screen with 500-600 meshes) to obtain 950L of filtrate;
(5) 950L of filtrate is concentrated in a reaction cylinder under vacuum (-0.05 to-0.095 Mpa), the mixed solvent is recovered, 650L of distilled water is added when the recovered mixed solvent reaches 600L, and 300L of solvent and 250L of water are remained after recovery;
(6) Transferring the materials in the reaction cylinder into a crystallizing cylinder after recovery, cooling the materials to 20-30 ℃, and performing centrifugal separation to obtain 20.50kg of crude rosemary extract; centrifuging the filtrate to produce rosmarinic acid.
(7) Dissolving 21.5kg of crude herba Rosmarini officinalis extract in 200L of food grade n-hexane, heating, and filtering to obtain filter residue; concentrating the filtrate under vacuum (-0.05-0.095 Mpa) to obtain refined rosemary extract product 10.8kg;
(8) Adding 10.8kg of fine rosemary extract into 19.00kg of sunflower seed oil and 12.5kg of distilled water, distilling by a vacuum membrane, and removing water by three-stage separation, wherein the solvent residue is 12.9kg and the rosemary essential oil is 0.40kg; 29.0kg of rosemary extract is obtained, and the carnosic acid content is 11.70%.
(9) 29.0kg of rosemary extract treated by the membrane distillation process is prepared into 33.93kg of carnosic acid with the content of 10 percent. The extraction rate of the effective components is 92.96 percent.
The comparative example adopts a continuous dynamic countercurrent extraction unit and membrane distillation, does not use mixed solvent, only uses single solvent food grade acetone, and reduces the extraction rate to 92.96 percent.
Comparative example 7
(1) Crushing 100kg of dry rosemary leaves to 60-100 meshes, wherein the dry rosemary leaves contain 3.65% of carnosic acid, putting the dry rosemary leaves into an infiltration tank, adding 400L of mixed solvent (200L of food grade isopropanol, 120L of food grade petroleum ether, 40L of food grade No. 6 light gasoline and 40L of food grade acetone) into the tank, and stirring the mixture for 30 minutes;
(2) The mixed solvent is quantitatively added from a solvent inlet through a flowmeter, wherein 600L of the mixed solvent (300L of food grade isopropanol, 180L of food grade petroleum ether, 60L of food grade No. 6 light gasoline and 60L of food grade acetone) is fed into a feeding port of a continuous dynamic countercurrent extraction unit through a quantitative feeder and is pushed to a discharging device under the action of a spiral propeller in a tank body. Extracting at 55 deg.C for 3 hr;
(3) Then discharging the slag materials from a discharging device, treating the slag materials in a juice extractor, and then performing waste recovery solvent treatment to obtain 58kg of waste residues and 15L of mixed solvent;
(4) The extract passes through a cylinder type automatic filter (a filter screen with 500-600 meshes) to obtain 950L of filtrate;
(5) Concentrating 950L filtrate in reaction cylinder under vacuum (-0.05 to-0.095 Mpa), recovering mixed solvent, adding 650L distilled water when the recovered mixed solvent reaches 600L, and recovering 300L mixed solvent and 250L water;
(6) Transferring the materials in the reaction cylinder into a crystallizing cylinder after recovery, cooling the materials to 20-30 ℃, and performing centrifugal separation to obtain 19.50kg of crude rosemary extract; the centrifuged filtrate is used to produce rosmarinic acid.
(7) Dissolving 19.5kg of crude rosemary extract in 200L of food-grade n-hexane, heating and filtering to obtain filter residue; concentrating the filtrate under vacuum (-0.05-0.095 Mpa) to obtain refined rosemary extract 11.00kg;
(8) Adding 18.0kg sunflower seed oil and 12.5kg distilled water into 11.0kg fine rosemary extract, distilling under reduced pressure membrane, and removing water, solvent residue 12.9kg and rosemary essential oil 0.45kg by three-stage separation; 28.15kg of rosemary extract is obtained, and the carnosic acid content is 12.00 percent.
(9) 28.15kg of rosemary extract treated by the membrane distillation process is prepared into 33.78kg of carnosic acid with the content of 10 percent. The extraction rate of the effective components is 92.55 percent.
The comparative example adopts a continuous dynamic countercurrent extraction unit and membrane distillation, and the extraction rate of other mixed solvent combinations (food grade petroleum ether, food grade isopropanol, food grade No. 6 light gasoline and food grade acetone) is reduced to 92.55 percent.
Comparative example 8
(1) Crushing 100kg of dry rosemary leaves containing 3.65% carnosic acid to 60-100 meshes, putting the crushed dry rosemary leaves into an infiltration tank, adding 400L of a mixed solvent (200L of food-grade 1-butanol, 120L of food-grade ether, 40L of food-grade butane and 40L of food-grade ethyl acetate), and stirring for 30 minutes;
(2) Feeding into a feeding port of a continuous dynamic countercurrent extraction unit through a quantitative feeder, pushing a discharging device under the action of a screw propeller in a tank body, and quantitatively adding 600L of mixed solvent (food grade 1-butanol 300L, food grade diethyl ether 180L, food grade butane 60L and food grade ethyl acetate 60L) into a solvent liquid inlet through a flow meter. Extracting at 55 deg.C for 3 hr;
(3) Then discharging the slag materials from a discharging device, treating the slag materials in a juice squeezing machine, and then performing waste recovery solvent treatment to obtain 60kg of waste slag and 15L of mixed solvent;
(4) The extract passes through a cylinder type automatic filter (a filter screen with 500-600 meshes) to obtain 960L of filtrate;
(5) 960L filtrate is concentrated under vacuum (-0.05 to-0.095 Mpa) in a reaction cylinder, mixed solvent is recovered, 650L distilled water is added when the recovered mixed solvent is 600L, and 300L mixed solvent and 250L water are remained after recovery;
(6) Transferring the materials in the reaction cylinder into a crystallizing cylinder after recovery, cooling the materials to 20-30 ℃, and performing centrifugal separation to obtain 18.50kg of crude rosemary extract; the centrifuged filtrate is used to produce rosmarinic acid.
(7) Dissolving 18.5kg crude herba Rosmarini officinalis extract in 200L food grade n-hexane, heating, and filtering to obtain filter residue; concentrating the filtrate under vacuum (-0.05-0.095 Mpa) to obtain fine rosemary extract 10.50kg;
(8) 10.50kg of fine rosemary extract product is added with 18.0kg of sunflower seed oil and 12.5kg of distilled water, and the mixture is distilled by a vacuum membrane, and water, 12.9kg of solvent residue and 0.40kg of rosemary essential oil are removed by three-stage separation; 27.70kg of rosemary extract is obtained, and the content of carnosic acid is 12.25 percent.
(9) 27.70kg of rosemary extract after being processed by the membrane distillation process is prepared into 33.93kg of carnosic acid with the content of 10 percent. The extraction rate of the effective components is 92.97 percent.
The comparative example uses a continuous dynamic countercurrent extractor set and membrane distillation with other mixed solvent combinations (food grade diethyl ether, food grade 1-butanol, butane and food grade ethyl acetate) and the extraction rate decreased to 92.97%.
Comparative example 9
(1) Crushing 100kg of dry rosemary leaves to 60-100 meshes, wherein the dry rosemary leaves contain 3.65 percent of carnosic acid, putting the dry rosemary leaves into an infiltration tank, adding 400L of mixed solvent (200L of food grade ethanol, 120L of food grade ethyl acetate, 40L of food grade 1, 2-dichloroethane and 40L of food grade acetone) into the tank, and stirring the mixture for 30 minutes;
(2) Feeding into a feeding port of a continuous dynamic countercurrent extraction unit by a quantitative feeder, pushing a discharging device in the tank body under the action of a screw propeller, and quantitatively adding 600L of mixed solvent (food grade ethanol 300L, food grade ethyl acetate 180L, food grade 1, 2-dichloroethane 60L and food grade acetone 60L) into a solvent liquid inlet by a flow meter. Extracting at 55 deg.C for 3 hr;
(3) Then discharging the slag from a discharging device, treating the slag in a juice extractor, and performing waste recovery solvent treatment to obtain 56kg of waste slag and 13L of mixed solvent;
(4) The extract passes through a cylinder type automatic filter (a filter screen with 500-600 meshes) to obtain 1020L of filtrate;
(5) Concentrating 1020L filtrate in reaction cylinder under vacuum (-0.05-0.095 Mpa), recovering mixed solvent, adding 650L distilled water when the recovered mixed solvent reaches 650L, and recovering 300L mixed solvent and 250L water;
(6) Transferring the materials in the reaction cylinder into a crystallizing cylinder after recovery, cooling the materials to 20-30 ℃, and performing centrifugal separation to obtain 20.50kg of crude rosemary extract; the centrifuged filtrate is used to produce rosmarinic acid.
(7) Dissolving 20.5kg of crude herba Rosmarini officinalis extract in 200L of food grade ethanol, heating, filtering, and filtering to obtain filter residue (only 0.1kg of ursolic acid in crude herba Rosmarini officinalis extract is dissolved in food grade ethanol); concentrating the filtrate under vacuum (-0.05-0.095 Mpa) to obtain refined rosemary extract 20.40kg; the product tests the content of the ursolic acid to be 20.55 percent, the rosemary extract can not contain the ursolic acid, and the product is unqualified.
In the comparative example, a continuous dynamic countercurrent extraction unit is adopted, food grade normal hexane in the step 4 is replaced by food grade ethanol, and as a result, ursolic acid in the rosemary extract crude product is dissolved in the food grade ethanol, and can not be separated, so that the rosemary extract product is unqualified.
Comparative example 10
(1) Crushing 100kg of dry rosemary leaves to 60-100 meshes, wherein the dry rosemary leaves contain 3.65 percent of carnosic acid, putting the dry rosemary leaves into an infiltration tank, adding 400L of mixed solvent (200L of food grade ethanol, 120L of food grade ethyl acetate, 40L of food grade 1, 2-dichloroethane and 40L of food grade acetone) into the tank, and stirring the mixture for 30 minutes;
(2) Feeding into a feeding port of a continuous dynamic countercurrent extraction unit by a quantitative feeder, pushing a discharging device in the tank body under the action of a screw propeller, and quantitatively adding 600L of mixed solvent (food grade ethanol 300L, food grade ethyl acetate 180L, food grade 1, 2-dichloroethane 60L and food grade acetone 60L) into a solvent liquid inlet by a flow meter. Extracting at 55 deg.C for 3 hr;
(3) Then discharging the slag materials from a discharging device, treating the slag materials in a juice squeezing machine, and then performing waste recovery solvent treatment to obtain 56kg of waste residues and 13L of mixed solvent;
(4) The extract passes through a cylinder type automatic filter (a filter screen with 500-600 meshes) to obtain 1020L of filtrate;
(5) Concentrating 1020L filtrate in reaction cylinder under vacuum (-0.05-0.095 Mpa), recovering mixed solvent, adding 650L distilled water when the recovered mixed solvent reaches 650L, and recovering 300L mixed solvent and 250L water;
(6) Transferring the materials in the reaction cylinder into a crystallizing cylinder after recovery, cooling the materials to 20-30 ℃, and performing centrifugal separation to obtain 20.50kg of crude rosemary extract; the centrifuged filtrate is used to produce rosmarinic acid.
(7) Adding 20.5kg rosemary extract crude product into 200L food grade No. 6 light gasoline, heating and filtering, and filtering to obtain filter residue of 5.5kg (some ursolic acid in rosemary extract crude product is dissolved in No. 6 light gasoline); concentrating the filtrate under vacuum (-0.05-0.095 Mpa) to obtain refined rosemary extract 15.40kg; the product tests the ursolic acid content to be 9.5 percent, the rosemary extract can not contain the ursolic acid, and the product is unqualified.
In the above examples 1 to 3, rosemary leaves contained 3.65% carnosic acid; detecting carnosic acid and carnosol by HPLC with total antioxidant components (calculated as carnosic acid and carnosol) of herba Rosmarini officinalis extract; the residual solvent (n-hexane, methanol, ethanol, ethyl acetate, 1, 2-dichloroethane, acetone) of rosemary extract was detected by gas chromatograph, and other physical and chemical analysis data are shown in table 1 below. As can be seen from Table 1: the product meets the GB 1886.172-2016 standard, and the extraction rate of effective components is greatly raised to 99.50% or higher.
TABLE 1 HPLC analysis of the total antioxidant components of rosemary extract and other physicochemical data
Claims (5)
1. The production process of the rosemary extract is characterized by comprising the following steps:
(1) The preparation method comprises the following steps of (1) crushing dry rosemary leaves to 60-100 meshes, putting the crushed dry rosemary leaves into an infiltration tank, adding a mixed solvent, infiltrating and stirring to obtain a mixture, wherein the mixed solvent is as follows: food grade ethanol, food grade ethyl acetate, food grade 1, 2-dichloroethane and food grade acetone, wherein the volume ratio of the ethanol to the ethyl acetate is 2-5: 1 to 5:1 to 5:1 to 5;
(2) Feeding the mixture into a continuous dynamic countercurrent extraction unit, and adding a mixed solvent in a countercurrent manner for extraction to obtain an extracting solution and filter residues; vacuum drying the filter residue to recover the mixed solvent;
(3) Filtering the extractive solution with automatic cylindrical filter to obtain filtrate, vacuum concentrating the filtrate, recovering mixed solvent, cooling the residual solution, and centrifuging to obtain crude herba Rosmarini officinalis extract;
(4) Dissolving the coarse rosemary extract product in food level hexane, heating at 50-60 deg.c, filtering and vacuum concentrating to obtain fine rosemary extract product;
(5) Adding edible salad oil and distilled water into the fine rosemary extract product, and removing solvent residue and rosemary essential oil by membrane distillation to obtain rosemary extract;
in the step (2), the continuous dynamic countercurrent extraction unit comprises: extraction processing amount: 50-200 kg/h; extraction temperature: 40 to 55 ℃; extraction time: the whole process lasts for 2-3 h; the solid-to-liquid ratio of the dry rosemary leaves in the mixture to the mixed solvent is 1 kg/4-6L;
in the step (5), the edible salad oil is sunflower seed oil;
in the step (5), the specific process of membrane distillation is as follows: distilling by using a vacuum membrane, adopting three-stage separation, wherein the treatment capacity of the first-stage distillation is 100-200L/h, the porosity of the membrane is 60-85%, the average pore diameter of the membrane is 0.1-0.5 mu m, the distillation temperature is 60-80 ℃, and the distillation vacuum degree is 20-50 Pa; the secondary distillation treatment capacity is 100-200L/h, the porosity of the membrane is 60-85%, the average pore diameter of the membrane is 0.1-0.5 mu m, the distillation temperature is 80-90 ℃, and the distillation vacuum degree is 30-50 Pa; the three-stage distillation treatment capacity is 100-120L/h, the porosity of the membrane is 60-85%, the average pore diameter of the membrane is 0.1-0.5 mu m, the distillation temperature is 85-95 ℃, and the distillation vacuum degree is 35-50 Pa;
the extraction rate of the effective components of the rosemary extract obtained after the treatment of the dry leaves of the rosemary is more than or equal to 99.50 percent, and the residual solvent is less than or equal to 10ppm.
2. A process for the production of a rosemary extract according to claim 1, wherein: in the step (1), the solid-to-liquid ratio of the dry rosemary leaves to the mixed solvent is 1 kg/2-4L.
3. A process for the production of a rosemary extract according to claim 1, wherein: in the step (3), when the recovered mixed solvent is 50-80% of the total amount of the mixed solvent added in the step (1) and the step (2) during vacuum concentration, the volume ratio of distilled water to filtrate is 0.5-0.8: 1 distilled water was added to continue recovering the remaining mixed solvent.
4. A process for the production of rosemary extract according to claim 1, wherein: in the step (4), the solid-to-liquid ratio of the rosemary extract crude product to the food-grade n-hexane is 1 kg/7-10L.
5. A process for the production of a rosemary extract according to claim 1, wherein: in the step (5), the solid-to-liquid ratio of the fine rosemary extract product to the edible salad oil and the distilled water is 1 kg/2-5L/1-3L.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102031116A (en) * | 2010-11-17 | 2011-04-27 | 合肥工业大学科教开发部 | New method for preparing rosemary natural antioxidant |
| CN102432469A (en) * | 2011-12-08 | 2012-05-02 | 刘正芳 | Method for extracting and separating rosmarinic acid and ursolic acid from rosemary |
| CN108070453A (en) * | 2016-11-11 | 2018-05-25 | 长沙卫生物科技有限公司 | A kind of method that extraction separates Rosemary Oil, Rosmarinic acid, ursolic acid and carnosic acid from rosemary |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102031116A (en) * | 2010-11-17 | 2011-04-27 | 合肥工业大学科教开发部 | New method for preparing rosemary natural antioxidant |
| CN102432469A (en) * | 2011-12-08 | 2012-05-02 | 刘正芳 | Method for extracting and separating rosmarinic acid and ursolic acid from rosemary |
| CN108070453A (en) * | 2016-11-11 | 2018-05-25 | 长沙卫生物科技有限公司 | A kind of method that extraction separates Rosemary Oil, Rosmarinic acid, ursolic acid and carnosic acid from rosemary |
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| "迷迭香叶中鼠尾草酸的分离纯化及其生物活性研究";夏田娟;《中国优秀硕士学位论文全文数据库》;20160615(第06期);"1.2.1.1 传统的溶剂提取" * |
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Effective date of registration: 20230804 Address after: 416100 Area C, Phase III, Standard Plant, Innovation and Entrepreneurship Park, High tech Zone, Wuxi Town, Luxi County, Xiangxi Tujia and Miao Autonomous Prefecture, Hunan Province Patentee after: Hunan zhizhiyuan agriculture and animal husbandry Co.,Ltd. Address before: 416117 interchange of Changji expressway, Wuxi Town, Luxi County, Xiangxi Tujia and Miao Autonomous Prefecture, Hunan Province (in Wuling Sunshine Biotechnology Co., Ltd.) Patentee before: Hunan Xianwei sunshine Biotechnology Co.,Ltd. |