CN104140909A - Rose wine and preparation method thereof - Google Patents
Rose wine and preparation method thereof Download PDFInfo
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- CN104140909A CN104140909A CN201410354426.7A CN201410354426A CN104140909A CN 104140909 A CN104140909 A CN 104140909A CN 201410354426 A CN201410354426 A CN 201410354426A CN 104140909 A CN104140909 A CN 104140909A
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Abstract
The invention relates to a rose wine and a preparation method of the rose wine. The preparation method comprises the five steps of raw material preprocessing, preparation of compound extractant, extraction processing, purification and refinement processing and concoction. The extraction rate is effectively improved through proper selection of pyridinium salt compounds, auxiliaries and additives and proper optimization of the process in the preparation process of the rose wine, and the prepared rose wine has the advantages of lasting and bright in color, lasting, fragrant and rich in scent after being stored for a long time, and has wide market value.
Description
Technical field
The present invention relates to a kind of wine and preparation method thereof, relate more specifically to a kind of rose flower wine and preparation method thereof, belong to active components of plants and extract and brewing technical field.
Background technology
In Rose, contain important present-color material, it is commonly referred to anthocyanidin or cyanidin(e), it is a kind of water colo(u)r being extensively present in plant, be under the jurisdiction of flavonoid compound, exist mainly with glucosides form, also referred to as anthocyanogen, and in Rose, the main component of anthocyanogen is Minor centaury pattern glycosides-3-glucose glucosides.Because the meta-bolites of synthetic class pigment in human body has toxic side effect, and anthocyan material is natural pigment, it has bright in colour and natural rose delicate fragrance and has excellent anti-oxidant activity if remove hydroxyl radical free radical, superoxide anion etc., thereby is widely used among the painted processing of the field of food such as beverage, drinks, candy.
The related process report that in prior art, existing many relevant anthocyanidin extracts and applies, for example:
Li Shengfeng etc. (" research of Roselle Calyx anthocyanidin optimization for extracting condition ", guangdong agricultural science, (11), 83-88,2006) use four factors quadratic regression orthogonal rotational unitized design to test, the factor that temperature, time, solid-liquid ratio, alcohol concn etc. is affected to anthocyanidin extraction yield is studied, and by contribution calculation method, the size of its effect is sorted.
Guo Yan etc. (" the microwave assisted extraction technical study of rose anthocyanidin ", China's food and nutrition, (12), 42-44,2009) report a kind of technique that adopts microwave technology to extract anthocyanidin from Rose, and determined by orthogonal experiment the optimal processing parameter extracting.This technique can effectively shorten extraction time, reduces the loss of anthocyanidin in extraction.
Lian Bo etc. (" the extraction and application research of northeast man rose-bengal pigment ", Agriculture of Anhui science, 39 (28), 17540-17541,2011) report a kind of method that adopts acid ethanol solution to extract haematochrome in Rose, and studied additive, soda acid, the stability influence of light and heat to pigment.
The patent application of CN102477026A also discloses a kind of technique of microwave-assisted extraction rose anthocyanidin, and its technique is simple, product purity is high, is with a wide range of applications.
Although there is the extraction process of multiple anthocyanidin in prior art, constantly improve or improve existing extraction process farthest to realize extraction or the shortened process of anthocyanidin, these remain the target of vast researcher.
The inventor is for the shortcoming of existing extraction process and the particular feature of anthocyan material, develop a kind of novel anthocyanidin extraction process by a large amount of literature readings and Experimental Research, and it is combined with fermented glutinous rice technique and studied the rose flower wine of multi-efficiencies such as thering is health care, health, beauty treatment, and its lovely luster, lasting lasting, possess market outlook widely.
Summary of the invention
In order to study novel rose flower wine and preparation method thereof, the inventor has carried out a large amount of deep research to this, is paying sufficient creative work and after deep scientific exploration, thereby is completing the present invention.
Particularly, the present invention relates generally to a kind of rose flower wine and preparation method thereof.
More specifically, the present invention relates to two aspects, first aspect, the present invention relates to a kind of preparation method of rose flower wine, and described method comprises in accordance with the following steps:
A, raw materials pretreatment;
B, preparation compound extractant;
C, extraction process;
D, purification processing;
E, modulation process.
In the preparation method of described rose flower wine of the present invention, described steps A specifically can be:
A, raw materials pretreatment
Gather roseleaf, the aqueous formic acid that is 0.05-0.1% with mass percent concentration is wetting to be cleaned or rinsing 1-2 minute, and filtering excessive moisture, dries naturally, then is crushed to 50-100 order, can obtain rose flower.
In the preparation method of described rose flower wine of the present invention, the usage quantity of the aqueous formic acid in described steps A there is no special restriction, clean 1-2 minute as long as roseleaf can be soaked, as long as roseleaf can be carried out to rinsing appropriate time as 1-2 minute at aqueous formic acid equably in other words.
In the preparation method of described rose flower wine of the present invention, described step B specifically can be:
B, preparation compound extractant
Pyridinium salt compound is mixed according to a certain percentage with auxiliary agent, then add additive, described additive is the mixture of N-Methyl pyrrolidone and beta-cyclodextrin, at 30-40 DEG C, stirs 10-15min, mixes, and obtains required compound extractant.
In the preparation method of described rose flower wine of the present invention, the pyridinium salt compound in described step B is any one in N-hexyl pyridinium tetrafluoroborate salt, N-hexyl pyridine hexafluorophosphate, N-butyl-pyridinium a tetrafluoro borate, N-butyl-pyridinium hexafluorophosphate.
In the preparation method of described rose flower wine of the present invention, the auxiliary agent in described step B is N, N ', N "-tri-n-propyl citric amides, N, N ', N " any one in-tri-normal-butyl citric amides.
In the preparation method of described rose flower wine of the present invention, in described step B, the weight ratio of pyridinium salt compound and auxiliary agent is 1:0.2-0.6, for example, can be 1:0.2,1:0.3,1:0.4,1:0.5 or 1:0.6, is preferably 1:0.4.
In the preparation method of described rose flower wine of the present invention, in the N-Methyl pyrrolidone of described step B and the mixture of beta-cyclodextrin, the weight ratio of N-Methyl pyrrolidone and beta-cyclodextrin is 1:1, the weight of this mixture (being additive) is the 1-5% of pyridinium salt compound weight, for example can be 1%, 2%, 3%, 4% or 5%, be preferably 3%.
In the preparation method of described rose flower wine of the present invention, described step C specifically can be:
C, extraction process
Proportionally take the rose flower of steps A and the extraction agent that step B makes, then the aqueous citric acid solution that to add with the mass percent concentration of the weight such as extraction agent be 0.6-0.8%, and mix and blend extracts 20-30min at 30-40 DEG C, then filtering separation obtains filtrate I;
Filter residue is placed in to expanded solvents system, is forced into 3-4MPa and forms expanded solvents system, stirring and leaching 10-20min under room temperature, to normal pressure, again filters Pressure Drop to obtain filtrate II;
Merge twice filtrate (being merging filtrate I and filtrate II) and obtain extracting solution, after concentrating under reduced pressure, vacuum-drying, obtain crude product, lucifuge, stored refrigerated at 4 DEG C.
In the preparation method of described rose flower wine of the present invention, in described step C, the weight ratio of rose flower and compound extractant is 1:4-6, can be to indefiniteness 1:4,1:4.5,1:5,1:5.5 or 1:6, is preferably 1:5.
In the preparation method of described rose flower wine of the present invention, in described step C, the volume of expanded solvents consists of: 20% ethanol and 80%CO
2, expanded solvents is with the volume mass of rose flower than being 3-5ml/g, every 1g rose flower uses 3-5ml expanded solvents.
In the preparation method of described rose flower wine of the present invention, described step D specifically can be:
D, purification processing
D1: by step C gained crude product, add dissolve with ethanol, adopt alumina column to carry out chromatographic separation, using propyl carbinol-ethyl acetate-acetone mixed solvent as elutriant, the usage quantity of this elutriant is 6-8 times of alumina column bed volume, in the time that elutriant outflow reaches the 3rd times of bed volume, starts to collect elutriant, until collect the elutriant of 2 times of bed volume, then revolve to steam and reclaim and obtain crude product;
D2: crude product is separated with high speed adverse current chromatogram: solvent system is propyl carbinol-formic acid-deionized water, the above-mentioned solvent system that is 10:1:10 by volume ratio carries out static layering, leave standstill 10h, getting upper strata is stationary phase, lower floor is moving phase, open sampling valve, stationary phase is filled to chromatography column with pump, opening speed controller, make the chromatographic column forward of high-speed counter-current chromatograph, turn up 700r/min, get stationary phase and dissolve crude product to 15mg/ml, sample injection continuously, flow rate of mobile phase is 1ml/min, detect elutant according to UV-detector and receive anthocyanidin component, vacuum concentration obtains anthocyanidin component sterling.
In the preparation method of described rose flower wine of the present invention, in propyl carbinol-ethyl acetate-acetone mixed solvent of step D1, the volume ratio of propyl carbinol, ethyl acetate and acetone is 4:2:1.
In the preparation method of described rose flower wine of the present invention, the aluminum oxide in step D1 is the conventional aluminum oxide that chromatography is used, and for example its specification can be 100-150 order.
In the preparation method of described rose flower wine of the present invention, in step D1, step C gained crude product is added to dissolve with ethanol, wherein the amount of ethanol there is no special restriction, as long as it can dissolve crude product completely, but for the follow-up post of crossing separates consideration, it is the most suitable completely that its consumption can exactly dissolve crude product.
In the preparation method of described rose flower wine of the present invention, in step D1, the usage quantity of elutriant is 6-8 times of alumina column bed volume (BV), is the 6-8 of the aluminum oxide volume of filling out in this post doubly;
In the time that elutriant outflow reaches the 3rd times of bed volume, start to collect elutriant, until collect the elutriant of 2 times of bed volume, when the cumulative volume of working as flowed out elutriant reaches 3BV, start to collect the elutriant of follow-up outflow, until the volume of collected elutriant be 2 times to bed volume, the elutriant that namely collected volume is 2BV.
In the preparation method of described rose flower wine of the present invention, obtain after sterling Deng having implemented the processing of step D2, it is in 0.01% HCl methanol solution that gained sterling is dissolved in to mass percent concentration, be mixed with mass percent concentration and be 0.5% solution, measuring its maximum absorption wavelength between 400-600nm is 520nm left and right, consistent with literature value report.Simultaneously in the interscan of 200-600nm wavelength region, the maximum absorption wavelength of visible region is between 465-550nm, the maximum absorption wavelength of ultraviolet region is near 270-280nm, consistent with bibliographical information, thereby confirms as anthocyanidin (anthocyanogen) component.
In the preparation method of described rose flower wine of the present invention, described step e specifically can be:
E, modulation process
The base wine that by step D gained anthocyanidin sterling and mass content is proportionally 0.6-0.8% citric acid is composite, adds white sugar, and stirring and dissolving, obtains the former wine of Rose; Pack former Rose wine into fermentor tank, airtight, the following lucifuge of room temperature storage fermentation 2 months; Then adopt ultrafiltration membrance filter, obtain rose flower wine of the present invention.
In the preparation method of described rose flower wine of the present invention, in described step e, the weight ratio of anthocyanidin sterling and base wine is 1:600-1000, for example, can be 1:700,1:800,1:900 or 1:1000.
In the preparation method of described rose flower wine of the present invention, in described step e, the weight of white sugar is the 3-4% of base wine weight, for example, can be 3%, 3.5% or 4%.
Second aspect, the present invention relates to a kind of rose flower wine preparing by aforesaid method, and this rose flower wine has that lovely luster, fragrance are lasting, nondiscoloration, non-fading excellent properties.
As mentioned above, the invention provides a kind of rose flower wine and preparation method thereof, compared with prior art, the extraction preparation that employing of the present invention is special and compound extraction, separating technology have been realized the separation and purification of anthocyanidin component, in addition the reasonable screening of component kind and obtained unexpectedly synergistic function, in a creative way institute's extract and base wine are carried out composite, the rose flower wine preparing possesses that lovely luster, fragrance are lasting, nondiscoloration, non-fading excellent effect, has good market outlook and industrialization promotion potentiality.
Embodiment
Below by specific embodiment, the present invention is described in detail; but the purposes of these exemplary embodiments and object are only used for exemplifying the present invention; not real protection scope of the present invention is formed to any type of any restriction, more non-protection scope of the present invention is confined to this.
Embodiment 1: investigate pyridinium salt compound and auxiliary agent kind
A, raw materials pretreatment
Gather roseleaf, the aqueous formic acid that is 0.05-0.1% with mass percent concentration is wetting to be cleaned or rinsing 1-2 minute, and filtering excessive moisture, dries naturally, then is crushed to 80 orders, can obtain rose flower.
B, preparation compound extractant
The different pyridinium salt compounds of following table 1 are mixed according to weight ratio 1:0.4 from different auxiliary agents, then adding weight is the N-Methyl pyrrolidone of pyridinium salt compound weight 3% and the mixture of beta-cyclodextrin (both weight ratios are 1:1), then at 35 DEG C, stir 10min, mix, obtain required compound extractant.
C, extraction process
Take the rose flower of steps A and the extraction agent that step B makes, the aqueous citric acid solution that then to add with the mass percent concentration of the weight such as extraction agent be 0.7%, and in container at 40 DEG C mix and blend extract 25min, then filtering separation obtains filtrate I;
Filter residue is placed in to expanded solvents system, is forced into 3MPa and forms expanded solvents system, stirring and leaching 15min under room temperature, to normal pressure, again filters Pressure Drop to obtain filtrate II;
Merge twice filtrate and obtain extracting solution, after concentrated, vacuum-drying, obtain crude product, lucifuge, 4 DEG C of stored refrigerated.
Wherein the weight ratio of rose flower and compound extractant is 1:5, and expanded solvents volume consists of: 20% ethanol and 80%CO
2, the usage ratio of expanded solvents and rose flower is 5ml/g.
D, purification processing
D1: by step C gained crude product, add dissolve with ethanol, adopt alumina column chromatography (aluminum oxide grain size is 100-150 order), by propyl carbinol-ethyl acetate-acetone mixed solvent (three's volume ratio is 4:2:1) as elutriant, the usage quantity of this elutriant is 6 times of alumina column bed volume, in the time that elutriant outflow reaches the 3rd times of bed volume, starts to collect elutriant, until collect the elutriant of 2 times of bed volume, then revolve to steam and reclaim and obtain crude product;
D2: crude product is separated with high speed adverse current chromatogram, solvent system is propyl carbinol-formic acid-deionized water, the above-mentioned solvent system that is 10:1:10 by volume ratio carries out static layering, leave standstill 10h, getting upper strata is stationary phase, lower floor is moving phase, open sampling valve, stationary phase is filled to chromatography column by pump certain flow rate, opening speed controller, make the chromatographic column forward of high-speed counter-current chromatograph, turn up 700r/min, get stationary phase and dissolve crude product to 15mg/ml, sample injection continuously, flow rate of mobile phase is 1ml/min, detect elutant according to UV-detector and receive anthocyanidin component, vacuum concentration obtains anthocyanidin component sterling.
E, modulation process
The ratio that is 1:800 according to weight ratio is that 20 degree base wine of 0.7% citric acid are composite by step D gained sterling and mass content, add white sugar, stirring and dissolving, obtain the former wine of Rose, pack former Rose wine into fermentor tank, airtight, the following lucifuge of room temperature storage fermentation 2 months, adopt ultrafiltration membrance filter, obtain rose flower wine of the present invention.
Wherein, white sugar weight is 3.5% of base wine weight.
Experimental result in the time adopting the rose flower using in different pyridinium salt compounds and different auxiliary agent and step C for 100g in step B is as shown in table 1 below:
Table 1
"--" representative is not added.
Embodiment 2: investigate the impact of binder component a kind
A, raw materials pretreatment
Gather roseleaf, the aqueous formic acid that is 0.08% with mass percent concentration is wetting to be cleaned or rinsing 1-2 minute, and filtering excessive moisture, dries naturally, then is crushed to 80 orders, can obtain rose flower.
B, preparation compound extractant
By N-hexyl pyridinium tetrafluoroborate salt and N, N '; N "-tri-n-propyl citric amides mix according to weight ratio 1:0.4, then add N-Methyl pyrrolidone that weight is pyridinium salt compound 3% and the 1:1 mixture of beta-cyclodextrin, at 35 DEG C, stir 10min, mix, obtain required compound extractant.
C, extraction process
Take the rose flower of steps A and the extraction agent that step B makes, the aqueous citric acid solution that then to add with the mass percent concentration of the weight such as extraction agent be 0.7%, and in container at 40 DEG C mix and blend extract 25min, then filtering separation obtains filtrate I;
Filter residue is placed in to expanded solvents system, is forced into 3MPa and forms expanded solvents system, stirring and leaching 15min under room temperature, to normal pressure, again filters Pressure Drop to obtain filtrate II;
Merge twice filtrate and obtain extracting solution, after concentrated, vacuum-drying, obtain crude product, lucifuge, 4 DEG C of stored refrigerated.
Wherein the weight ratio of rose flower and compound extractant is 1:5, and expanded solvents volume consists of: 20% ethanol and 80%CO
2, the usage ratio of expanded solvents and rose flower is 5ml/g.
D, purification processing
D1: by step C gained crude product, add dissolve with ethanol, adopt alumina column chromatography (aluminum oxide grain size is 100-150 order), by propyl carbinol-ethyl acetate-acetone mixed solvent (three's volume ratio is 4:2:1) as elutriant, the usage quantity of this elutriant is 7 times of alumina column bed volume, in the time that elutriant outflow reaches the 3rd times of bed volume, starts to collect elutriant, until collect the elutriant of 2 times of bed volume, then revolve to steam and reclaim and obtain crude product;
D2: crude product is separated with high speed adverse current chromatogram, solvent system is propyl carbinol-formic acid-deionized water, the above-mentioned solvent system that is 10:1:10 by volume ratio carries out static layering, leave standstill 10h, getting upper strata is stationary phase, lower floor is moving phase, open sampling valve, stationary phase is filled to chromatography column by pump certain flow rate, opening speed controller, make the chromatographic column forward of high-speed counter-current chromatograph, turn up 700r/min, get stationary phase and dissolve crude product to 15mg/ml, sample injection continuously, flow rate of mobile phase is 1ml/min, detect elutant according to UV-detector and receive anthocyanidin component, vacuum concentration obtains anthocyanidin component sterling.
E, modulation process
The ratio that is 1:800 according to weight ratio is that 20 degree base wine of 0.7% citric acid are composite by step D gained sterling and mass content, add white sugar, stirring and dissolving, obtain the former wine of Rose, pack former Rose wine into fermentor tank, airtight, the following lucifuge of room temperature storage fermentation 2 months, adopt ultrafiltration membrance filter, obtain rose flower wine of the present invention.
Wherein, white sugar accounts for 3.5% of base wine weight.
Experimental result in the time that beta-cyclodextrin in step B is replaced with to the rose flower using in other component as shown in the table and step C for 100g is as shown in table 2 below:
Table 2
"--" representative is not added
Embodiment 3: investigate the impact of binder component 2 kinds
A, raw materials pretreatment
Gather roseleaf, the aqueous formic acid that is 0.08% with mass percent concentration is wetting to be cleaned or rinsing 1-2 minute, and filtering excessive moisture, dries naturally, then is crushed to 80 orders, can obtain rose flower.
B, preparation compound extractant
By N-hexyl pyridinium tetrafluoroborate salt and N, N '; N "-tri-n-propyl citric amides mix according to weight ratio 1:0.4, then adding weight is the N-Methyl pyrrolidone of pyridinium salt compound weight 3% and the mixture of beta-cyclodextrin (both weight ratios are 1:1), at 35 DEG C, stir 10min, mix, obtain required compound extractant.
C, extraction process
Take the rose flower of steps A and the extraction agent that step B makes, the aqueous citric acid solution that then to add with the mass percent concentration of the weight such as extraction agent be 0.7%, and in container at 40 DEG C mix and blend extract 25min, then filtering separation obtains filtrate I;
Filter residue is placed in to expanded solvents system, is forced into 3MPa and forms expanded solvents system, stirring and leaching 15min under room temperature, to normal pressure, again filters Pressure Drop to obtain filtrate II;
Merge twice filtrate and obtain extracting solution, after concentrated, vacuum-drying, obtain crude product, lucifuge, 4 DEG C of stored refrigerated.
Wherein the weight ratio of rose flower and compound extractant is 1:5, and expanded solvents volume consists of: 20% ethanol and 80%CO
2, the usage ratio of expanded solvents and rose flower is 5ml/g.
D, purification processing
D1: by step C gained crude product, add dissolve with ethanol, adopt alumina column chromatography (aluminum oxide grain size is 100-150 order), by propyl carbinol-ethyl acetate-acetone mixed solvent (three's volume ratio is 4:2:1) as elutriant, the usage quantity of this elutriant is 7 times of alumina column bed volume, in the time that elutriant outflow reaches the 3rd times of bed volume, starts to collect elutriant, until collect the elutriant of 2 times of bed volume, then revolve to steam and reclaim and obtain crude product;
D2: crude product is separated with high speed adverse current chromatogram, solvent system is propyl carbinol-formic acid-deionized water, the above-mentioned solvent system that is 10:1:10 by volume ratio carries out static layering, leave standstill 10h, getting upper strata is stationary phase, lower floor is moving phase, open sampling valve, stationary phase is filled to chromatography column by pump certain flow rate, opening speed controller, make the chromatographic column forward of high-speed counter-current chromatograph, turn up 700r/min, get stationary phase and dissolve crude product to 15mg/ml, sample injection continuously, flow rate of mobile phase is 1ml/min, detect elutant according to UV-detector and receive anthocyanidin component, vacuum concentration obtains anthocyanidin component sterling.
E, modulation process
The ratio that is 1:800 according to weight ratio by step D gained sterling with mass content be that 20 degree base wine of 0.7% citric acid are composite, add white sugar, stirring and dissolving, obtain the former wine of Rose, pack former Rose wine into fermentor tank, airtight, the following lucifuge of room temperature storage fermentation 2 months, adopt ultrafiltration membrance filter, obtain rose flower wine of the present invention.
Wherein, white sugar accounts for 3.5% of base wine weight.
Experimental result in the time that N-Methyl pyrrolidone in step B replaces with the rose flower using in other component as shown in the table and step C for 100g is as shown in table 3 below:
Table 3
"--" representative is not added.
It is in 0.01% HCl methanol solution that the extraction sterling obtaining in all the present invention embodiment is dissolved in to mass percent concentration, be mixed with mass percent concentration and be 0.5% solution, measuring its maximum absorption wavelength between 400-600nm is 515-525nm, consistent with literature value coverage; And the maximum absorption wavelength of ultraviolet region, near 270-280nm, is also consistent with bibliographical information, thereby confirm as anthocyanidin (anthocyanogen) component.
performance test
Rose flower wine prepared by the present invention is tested
Experimental technique: get respectively the preparation-obtained different numbering rose flower wines of the embodiment of the present invention, be placed in container, refrigeration storage 6-12 month, engage specialty mirror wine teacher to contrast the variation that stores front and back rose flower wine color and fragrance, wherein rose flower wine color can adopt visual test and appraisal of specialty mirror wine teacher, also can adopt colorimetric instrument to determine.Wherein, in the time just preparing, the color of the rose flower wine of numbering 1-20 is bright-coloured, pleasing redness, aromatic flavour.
Experimental result is as shown in table 4 below:
Table 4
From upper table 1-4:
1, the present invention adopts novel extraction process, creatively uses the special compound extraction preparation of pyridinium salt compound, auxiliary agent and additive, furthermore auxiliary with expanded solvents extraction, thereby has significantly improved the extraction yield of anthocyanin class material, takes full advantage of material.
2, in extracting method of the present invention, a large amount of experiment screenings is all passed through in the kind of material and combination, and the replacement of kind or omission all can significantly impact the effect of extraction, and visible extraction process of the present invention has obtained unforeseeable technique effect.
3, the present invention is in harmonious proportion the effective constituent of being extracted and base wine mutually, and additional with white sugar seasoning, form through fermentation, its can standing storage and keep bright in colour, smell is fragrant strong, makes this drinking utensils have the charm of rose uniqueness.
The purposes that should be appreciated that these embodiment only limits the scope of the invention for the present invention being described but not being intended to.In addition; also should understand; after having read technology contents of the present invention, those skilled in the art can make various changes, amendment and/or modification to the present invention, within these all equivalent form of values fall within the protection domain that the application's appended claims limits equally.
Claims (10)
1. a preparation method for rose flower wine, described method comprises the steps:
A, raw materials pretreatment;
B, preparation compound extractant;
C, extraction process;
D, purification processing;
E, modulation process.
2. preparation method as claimed in claim 1, is characterized in that described method comprises the steps:
A, raw materials pretreatment
Gather roseleaf, the aqueous formic acid that is 0.05-0.1% with mass percent concentration is wetting to be cleaned or rinsing 1-2 minute, filtering excessive moisture, dries naturally, then is crushed to 50-100 order, can obtain rose flower and gather roseleaf, the aqueous formic acid that is 0.05-0.1% with mass percent concentration is wetting to be cleaned or rinsing 1-2 minute, and filtering excessive moisture, dries naturally, be crushed to again 50-100 order, obtain rose flower;
B, preparation compound extractant
Pyridinium salt compound is mixed according to a certain percentage with auxiliary agent, then add additive, described additive is the mixture of N-Methyl pyrrolidone and beta-cyclodextrin, at 30-40 DEG C, stirs 10-15min, mixes, and obtains required compound extractant;
C, extraction process
Proportionally take the rose flower of steps A and the extraction agent that step B makes, then the aqueous citric acid solution that to add with the mass percent concentration of the weight such as extraction agent be 0.6-0.8%, and mix and blend extracts 20-30min at 30-40 DEG C, then filtering separation obtains filtrate I;
Filter residue is placed in to expanded solvents system, is forced into 3-4MPa and forms expanded solvents system, stirring and leaching 10-20min under room temperature, to normal pressure, again filters Pressure Drop to obtain filtrate II;
Merge twice filtrate and obtain extracting solution, after concentrating under reduced pressure, vacuum-drying, obtain crude product, lucifuge, stored refrigerated at 4 DEG C;
D, purification processing
D1: by step C gained crude product, add dissolve with ethanol, adopt alumina column to carry out chromatographic separation, using propyl carbinol-ethyl acetate-acetone mixed solvent as elutriant, the usage quantity of this elutriant is 6-8 times of alumina column bed volume, in the time that elutriant outflow reaches the 3rd times of bed volume, starts to collect elutriant, until collect the elutriant of 2 times of bed volume, then revolve to steam and reclaim and obtain crude product;
D2: crude product is separated with high speed adverse current chromatogram: solvent system is propyl carbinol-formic acid-deionized water, the above-mentioned solvent system that is 10:1:10 by volume ratio carries out static layering, leave standstill 10h, getting upper strata is stationary phase, lower floor is moving phase, open sampling valve, stationary phase is filled to chromatography column with pump, opening speed controller, make the chromatographic column forward of high-speed counter-current chromatograph, turn up 700r/min, get stationary phase and dissolve crude product to 15mg/ml, sample injection continuously, flow rate of mobile phase is 1ml/min, detect elutant according to UV-detector and receive anthocyanidin component, vacuum concentration obtains anthocyanidin component sterling,
E, modulation process
The base wine that by step D gained anthocyanidin sterling and mass content is proportionally 0.6-0.8% citric acid is composite, adds white sugar, and stirring and dissolving, obtains the former wine of Rose; Pack former Rose wine into fermentor tank, airtight, the following lucifuge of room temperature storage fermentation 2 months; Then adopt ultrafiltration membrance filter, obtain rose flower wine of the present invention.
3. preparation method as claimed in claim 2, is characterized in that: the pyridinium salt compound in described step B is any one in N-hexyl pyridinium tetrafluoroborate salt, N-hexyl pyridine hexafluorophosphate, N-butyl-pyridinium a tetrafluoro borate, N-butyl-pyridinium hexafluorophosphate.
4. the preparation method as described in claim 2-3 any one, is characterized in that: the auxiliary agent in described step B is N, N ', N "-tri-n-propyl citric amides, N, N ', N " any one in-tri-normal-butyl citric amides.
5. the preparation method as described in claim 2-4 any one, is characterized in that: in described step B, the part by weight of pyridinium salt compound and auxiliary agent is 1:0.2-0.6.
6. the preparation method as described in claim 2-5 any one, is characterized in that: in described step B, the weight of additive is the 1-5% of pyridinium salt compound weight.
7. the preparation method as described in claim 2-6 any one, is characterized in that: in described step C, the weight ratio of rose flower and compound extractant is 1:4-6.
8. the preparation method as described in claim 2-7 any one, is characterized in that: in described step C, the volume of expanded solvents consists of: 20% ethanol and 80%CO
2, expanded solvents is 3-5ml/g with the volume mass ratio of rose flower.
9. the preparation method as described in claim 2-8 any one, is characterized in that:, in described step e, the weight ratio of anthocyanidin sterling and base wine is 1:600-1000.
10. right to use requires preparation method described in 1-9 any one and the rose flower wine for preparing.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410354426.7A CN104140909B (en) | 2014-07-24 | 2014-07-24 | A kind of rose flower wine and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410354426.7A CN104140909B (en) | 2014-07-24 | 2014-07-24 | A kind of rose flower wine and preparation method thereof |
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| Publication Number | Publication Date |
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| CN104140909A true CN104140909A (en) | 2014-11-12 |
| CN104140909B CN104140909B (en) | 2015-08-19 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104610682A (en) * | 2015-01-08 | 2015-05-13 | 江苏黄金龙风筒科技有限公司 | Composite PVC water hose and preparation method thereof |
| CN105331493A (en) * | 2015-12-23 | 2016-02-17 | 秦皇岛大惠生物技术有限公司 | Rose sparking wine and production method thereof |
| CN105713787A (en) * | 2016-04-25 | 2016-06-29 | 浙江农林大学 | Preparation method of liver protection type saffron crocus-kudzuvine root yellow wine |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104610682A (en) * | 2015-01-08 | 2015-05-13 | 江苏黄金龙风筒科技有限公司 | Composite PVC water hose and preparation method thereof |
| CN104610682B (en) * | 2015-01-08 | 2016-10-26 | 江苏黄金龙风筒科技有限公司 | A kind of composite PVC water band and preparation method thereof |
| CN105331493A (en) * | 2015-12-23 | 2016-02-17 | 秦皇岛大惠生物技术有限公司 | Rose sparking wine and production method thereof |
| CN105331493B (en) * | 2015-12-23 | 2017-12-26 | 秦皇岛大惠生物技术有限公司 | A kind of rose fizz and its production method |
| CN105713787A (en) * | 2016-04-25 | 2016-06-29 | 浙江农林大学 | Preparation method of liver protection type saffron crocus-kudzuvine root yellow wine |
| CN105713787B (en) * | 2016-04-25 | 2018-09-21 | 浙江农林大学 | A kind of preparation method of liver-protecting type safflower pueraria lobata yellow rice wine |
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| CN104140909B (en) | 2015-08-19 |
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