CN104140909B - A kind of rose flower wine and preparation method thereof - Google Patents
A kind of rose flower wine and preparation method thereof Download PDFInfo
- Publication number
- CN104140909B CN104140909B CN201410354426.7A CN201410354426A CN104140909B CN 104140909 B CN104140909 B CN 104140909B CN 201410354426 A CN201410354426 A CN 201410354426A CN 104140909 B CN104140909 B CN 104140909B
- Authority
- CN
- China
- Prior art keywords
- preparation
- rose flower
- wine
- rose
- elutriant
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Landscapes
- Alcoholic Beverages (AREA)
- Coloring Foods And Improving Nutritive Qualities (AREA)
Abstract
The present invention relates to a kind of rose flower wine and preparation method thereof, described preparation method comprises raw materials pretreatment, preparation compound extractant, extraction process, purification process and the large step of modulation process five, it effectively improves extraction yield by the suitable selection of pyridinium compound, auxiliary agent and binder component and the suitable optimization of technique, and by it in order among the preparation of rose flower wine, prepared rose flower wine shows bright-coloured, the long-term fragrant strong advantage of smell fast in colour in long storage periods, has marketable value very widely.
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
Containing important present-color material in Rose, it is commonly referred to anthocyanidin or cyanidin(e), it is a kind of water colo(u)r be extensively present in plant, be under the jurisdiction of flavonoid compound, exist mainly with glycoside forms, also referred to as anthocyanogen, and in Rose, the main component of anthocyanogen is Minor centaury anthocyanogen-3-glucose glucosides.Because the meta-bolites of synthesis class pigment in human body has toxic side effect, and anthocyan material is natural pigment, it has bright in colour and natural rose scent and has excellent anti-oxidant activity if removing hydroxyl radical free radical, superoxide anion etc., among the painted processing being thus widely used in the field of food such as beverage, drinks, candy.
The related process report that in prior art, existing many relevant anthocyanidin extracts and applies, such as:
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 experiments, factor temperature, time, solid-liquid ratio, alcohol concn etc. being affected to anthocyanidin extraction yield is studied, and is sorted to the size that it acts on by contribution calculation method.
Guo Yan etc. (" the microwave assisted extraction technical study of rose anthocyanidin ", Chinese food and nutrition, (12), 42-44,2009) report a kind of technique adopting microwave technology to extract anthocyanidin from Rose, and the optimal processing parameter of extraction is determined by orthogonal experiment.This technique effectively can 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 adopting acid ethanol solution to extract haematochrome in Rose, and have studied additive, soda acid, light and heat to the stability influence of pigment.
The patent application of CN102477026A also discloses a kind of technique of microwave radiation exaraction 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 have remained the target of vast researcher.
The shortcoming of the present inventor for existing extraction process and the particular feature of anthocyan material, a kind of novel anthocyanidin extraction process is developed by a large amount of literature readings and Experimental Research, and it is combined with fermented glutinous rice technique and have studied have keep healthy, health, the multi-efficiency such as beauty treatment rose flower wine, and its bright in colour, lasting lasting, possess market outlook widely.
Summary of the invention
In order to study novel rose flower wine and preparation method thereof, the present inventor, to this has been research deep in a large number, is paying sufficient creative work and after deep scientific exploration, thus is completing the present invention.
Specifically, 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 process;
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, be the wetting cleaning of aqueous formic acid or the rinsing 1-2 minute of 0.05-0.1% with mass percent concentration, 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, there is no particular limitation for the usage quantity of the aqueous formic acid in described steps A, as long as roseleaf can be carried out wetting cleaning 1-2 minute, as long as roseleaf can be carried out 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
Mixed according to a certain percentage with auxiliary agent by pyridinium compound, then add additive, described additive is the mixture of N-Methyl pyrrolidone and beta-cyclodextrin, stirs 10-15min, mix at 30-40 DEG C, obtains required compound extractant.
In the preparation method of described rose flower wine of the present invention, the pyridinium 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 "-three n-propyl citric amides, N, N ', N " any one in-three 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 compound and auxiliary agent is 1:0.2-0.6, such as, 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 (i.e. additive) is the 1-5% of pyridinium compound weight, such as 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 obtained extraction agent of step B, then adding with the mass percent concentration of the weight such as extraction agent is the aqueous citric acid solution of 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 expanded solvents system, is forced into 3-4MPa and forms expanded solvents system, in stirred at ambient temperature lixiviate 10-20min, after Pressure Drop to normal pressure, again filter and obtain filtrate II;
Merge twice filtrate (i.e. 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 1:4,1:4.5,1:5,1:5.5 or 1:6 in non-limiting manner, 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 3-5ml/g with the volume mass ratio of rose flower, and namely 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 process
D1: by step C gained crude product, add dissolve with ethanol, alumina column is adopted 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, when 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 high speed adverse current chromatogram is separated: solvent system is propyl carbinol-formic acid-deionized water, be that the above-mentioned solvent system of 10:1:10 carries out static layering by volume ratio, leave standstill 10h, getting upper strata is stationary phase, lower floor is moving phase, open sampling valve, stationary phase pump is filled chromatography column, opening speed controller, the chromatographic column of high-speed counter-current chromatograph is rotated forward, turn up 700r/min, get stationary phase and dissolve crude product to 15mg/ml, continuous sample injection, 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 the 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 alumina of chromatography, and such as 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 dissolve with ethanol, there is no particular limitation for the amount of wherein ethanol, as long as crude product can dissolve by completely, but in order to follow-up post of crossing is separated consideration, it is the most suitable completely that crude product can exactly dissolve by its consumption.
In the preparation method of described rose flower wine of the present invention, in step D1, the usage quantity of elutriant be the 6-8 of alumina column bed volume (BV) doubly, be 6-8 times that aluminum oxide volume is filled out by institute in this post;
When elutriant outflow reaches the 3rd times of bed volume, start to collect elutriant, until collect the elutriant of 2 times of bed volume, namely when the cumulative volume of flowed out elutriant reaches 3BV, start the elutriant collecting follow-up outflow, until the volume of collected elutriant be 2 times to bed volume, namely collected volume is the elutriant of 2BV.
In the preparation method of described rose flower wine of the present invention, Deng implemented step D2 process and after obtaining sterling, gained sterling being dissolved in mass percent concentration is in the HCl methanol solution of 0.01%, be mixed with the solution that mass percent concentration is 0.5%, measuring its maximum absorption wavelength between 400-600nm is about 520nm, reports consistent with literature value.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, thus 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 by step D gained anthocyanidin sterling and mass content being proportionally 0.6-0.8% citric acid is composite, adds white sugar, stirring and dissolving, obtains the former wine of Rose; Former for Rose wine is loaded fermentor tank, airtight, room temperature following lucifuge 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, such as, 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, such as, can be 3%, 3.5% or 4%.
Second aspect, the present invention relates to a kind of rose flower wine prepared by aforesaid method, 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 collecting, separating technology achieve the separation and purification of anthocyanidin component, in addition constituent species reasonable screening and achieve synergistic function unexpectedly, in a creative way institute's extract and base wine are carried out composite, the rose flower wine prepared possesses that lovely luster, fragrance are lasting, nondiscoloration, non-fading excellent effect, there are 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 any type of any restriction is formed to real protection scope of the present invention, more non-protection scope of the present invention is confined to this.
Embodiment 1: investigate pyridinium compound and auxiliary agent kind
A, raw materials pretreatment
Gather roseleaf, be the wetting cleaning of aqueous formic acid or the rinsing 1-2 minute of 0.05-0.1% with mass percent concentration, filtering excessive moisture, dries naturally, then is crushed to 80 orders, can obtain rose flower.
B, preparation compound extractant
The different pyridinium compound of following table 1 is mixed according to weight ratio 1:0.4 from different auxiliary agent, then adding weight is the N-Methyl pyrrolidone of pyridinium compound weight 3% and the mixture (both weight ratios are 1:1) of beta-cyclodextrin, then at 35 DEG C, 10min is stirred, mix, obtain required compound extractant.
C, extraction process
Take the rose flower of steps A and the obtained extraction agent of step B, then adding with the mass percent concentration of the weight such as extraction agent is the aqueous citric acid solution of 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 expanded solvents system, is forced into 3MPa and forms expanded solvents system, in stirred at ambient temperature lixiviate 15min, after Pressure Drop to normal pressure, again filter and 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 process
D1: by step C gained crude product, add dissolve with ethanol, adopt alumina column chromatography (aluminum oxide grain size is 100-150 order), with 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, when 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 high speed adverse current chromatogram is separated, solvent system is propyl carbinol-formic acid-deionized water, be that the above-mentioned solvent system of 10:1:10 carries out static layering by volume ratio, leave standstill 10h, getting upper strata is stationary phase, lower floor is moving phase, open sampling valve, stationary phase pump certain flow rate is filled chromatography column, opening speed controller, the chromatographic column of high-speed counter-current chromatograph is rotated forward, turn up 700r/min, get stationary phase and dissolve crude product to 15mg/ml, continuous sample injection, 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
20 degree of base wine of to be the ratio of 1:800 according to weight ratio by step D gained sterling and mass content be 0.7% citric acid are composite, add white sugar, stirring and dissolving, obtain the former wine of Rose, former for Rose wine is loaded fermentor tank, airtight, room temperature following lucifuge 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.
When adopt in step B the rose flower that uses in different pyridinium compound and different auxiliary agent and step C for experimental result during 100g as shown in table 1 below:
Table 1
"--" representative is not added.
Embodiment 2: the impact investigating binder component a kind
A, raw materials pretreatment
Gather roseleaf, be the wetting cleaning of aqueous formic acid or the rinsing 1-2 minute of 0.08% with mass percent concentration, 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 "-three n-propyl citric amides mix according to weight ratio 1:0.4, then adding weight is the N-Methyl pyrrolidone of pyridinium compound 3% and the 1:1 mixture of beta-cyclodextrin, 10min is stirred at 35 DEG C, mix, obtain required compound extractant.
C, extraction process
Take the rose flower of steps A and the obtained extraction agent of step B, then adding with the mass percent concentration of the weight such as extraction agent is the aqueous citric acid solution of 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 expanded solvents system, is forced into 3MPa and forms expanded solvents system, in stirred at ambient temperature lixiviate 15min, after Pressure Drop to normal pressure, again filter and 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 process
D1: by step C gained crude product, add dissolve with ethanol, adopt alumina column chromatography (aluminum oxide grain size is 100-150 order), with 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, when 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 high speed adverse current chromatogram is separated, solvent system is propyl carbinol-formic acid-deionized water, be that the above-mentioned solvent system of 10:1:10 carries out static layering by volume ratio, leave standstill 10h, getting upper strata is stationary phase, lower floor is moving phase, open sampling valve, stationary phase pump certain flow rate is filled chromatography column, opening speed controller, the chromatographic column of high-speed counter-current chromatograph is rotated forward, turn up 700r/min, get stationary phase and dissolve crude product to 15mg/ml, continuous sample injection, 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
20 degree of base wine of to be the ratio of 1:800 according to weight ratio by step D gained sterling and mass content be 0.7% citric acid are composite, add white sugar, stirring and dissolving, obtain the former wine of Rose, former for Rose wine is loaded fermentor tank, airtight, room temperature following lucifuge 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.
When beta-cyclodextrin in step B is replaced with the rose flower that uses in other component as shown in the table and step C for experimental result during 100g as shown in table 2 below:
Table 2
"--" representative is not added
Embodiment 3: the impact investigating binder component 2 kind
A, raw materials pretreatment
Gather roseleaf, be the wetting cleaning of aqueous formic acid or the rinsing 1-2 minute of 0.08% with mass percent concentration, 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 "-three n-propyl citric amides mix according to weight ratio 1:0.4, then adding weight is the N-Methyl pyrrolidone of pyridinium compound weight 3% and the mixture (both weight ratios are 1:1) of beta-cyclodextrin, 10min is stirred at 35 DEG C, mix, obtain required compound extractant.
C, extraction process
Take the rose flower of steps A and the obtained extraction agent of step B, then adding with the mass percent concentration of the weight such as extraction agent is the aqueous citric acid solution of 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 expanded solvents system, is forced into 3MPa and forms expanded solvents system, in stirred at ambient temperature lixiviate 15min, after Pressure Drop to normal pressure, again filter and 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 process
D1: by step C gained crude product, add dissolve with ethanol, adopt alumina column chromatography (aluminum oxide grain size is 100-150 order), with 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, when 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 high speed adverse current chromatogram is separated, solvent system is propyl carbinol-formic acid-deionized water, be that the above-mentioned solvent system of 10:1:10 carries out static layering by volume ratio, leave standstill 10h, getting upper strata is stationary phase, lower floor is moving phase, open sampling valve, stationary phase pump certain flow rate is filled chromatography column, opening speed controller, the chromatographic column of high-speed counter-current chromatograph is rotated forward, turn up 700r/min, get stationary phase and dissolve crude product to 15mg/ml, continuous sample injection, 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
According to weight ratio be 1:800 ratio by step D gained sterling be that 20 degree of base wine of 0.7% citric acid are composite with mass content, add white sugar, stirring and dissolving, obtain the former wine of Rose, former for Rose wine is loaded fermentor tank, airtight, room temperature following lucifuge 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.
When N-Methyl pyrrolidone in step B replace with the rose flower used in other component as shown in the table and step C for experimental result during 100g as shown in table 3 below:
Table 3
"--" representative is not added.
The extraction sterling obtained in all for the present invention embodiments being dissolved in mass percent concentration is in the HCl methanol solution of 0.01%, be mixed with the solution that mass percent concentration is 0.5%, measuring its maximum absorption wavelength between 400-600nm is 515-525nm, consistent with literature value coverage; And the maximum absorption wavelength of ultraviolet region is near 270-280nm, is also consistent with bibliographical information, thus confirm as anthocyanidin (anthocyanogen) component.
performance test
Rose flower wine prepared by the present invention is tested
Experimental technique: get the preparation-obtained different numbering rose flower wine of the embodiment of the present invention respectively, be placed in container, refrigerated storage 6-12 month, specialty mirror wine teacher is engaged to contrast the change storing front and back rose flower wine color and fragrance, wherein rose flower wine color can adopt that specialty mirror wine teacher is visual to test and assess, and colorimetric instrument also can be adopted to determine.Wherein, when 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 collecting preparation of pyridinium compound, auxiliary agent and additive, furthermore auxiliary with expanded solvents extraction, thus significantly improves 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 kind and the combination of material, and the replacement of kind or omission all can significantly impact the effect of extraction, and visible extraction process of the present invention achieves unforeseeable technique effect.
3, the present invention by the effective constituent extracted be in harmonious proportion mutually with base wine, and additional with white sugar seasoning, form through fermentation, its can standing storage and keep bright in colour, fragrant is strong, makes this drinking utensils have the charm of rose uniqueness.
Should be appreciated that the purposes of these embodiments is only not intended to for illustration of the present invention limit the scope of the invention.In addition; also should understand; after having read technology contents of the present invention, those skilled in the art can make various change, amendment and/or modification to the present invention, and these all equivalent form of values fall within the protection domain that the application's appended claims limits equally.
Claims (6)
1. a preparation method for rose flower wine, described method comprises the steps:
A, raw materials pretreatment
Gather roseleaf, be the wetting cleaning of aqueous formic acid or the rinsing 1-2 minute of 0.05-0.1% with mass percent concentration, filtering excessive moisture, dries naturally, then is crushed to 50-100 order, can obtain rose flower;
B, preparation compound extractant
Mixed according to a certain percentage with auxiliary agent by pyridinium compound, then add additive, described additive is the mixture of N-Methyl pyrrolidone and beta-cyclodextrin, stirs 10-15min, mix at 30-40 DEG C, obtains required compound extractant;
C, extraction process
Proportionally take the rose flower of steps A and the obtained extraction agent of step B, then adding with the mass percent concentration of the weight such as extraction agent is the aqueous citric acid solution of 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 expanded solvents system, is forced into 3-4MPa and forms expanded solvents system, in stirred at ambient temperature lixiviate 10-20min, after Pressure Drop to normal pressure, again filter and 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 process
D1: by step C gained crude product, add dissolve with ethanol, alumina column is adopted 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, when 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 high speed adverse current chromatogram is separated: solvent system is propyl carbinol-formic acid-deionized water, be that the above-mentioned solvent system of 10:1:10 carries out static layering by volume ratio, leave standstill 10h, getting upper strata is stationary phase, lower floor is moving phase, open sampling valve, stationary phase pump is filled chromatography column, opening speed controller, the chromatographic column of high-speed counter-current chromatograph is rotated forward, turn up 700r/min, get stationary phase and dissolve crude product to 15mg/ml, continuous sample injection, 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 by step D gained anthocyanidin sterling and mass content being proportionally 0.6-0.8% citric acid is composite, adds white sugar, stirring and dissolving, obtains the former wine of Rose; Former for Rose wine is loaded fermentor tank, airtight, room temperature following lucifuge storage fermentation 2 months; Then adopt ultrafiltration membrance filter, obtain rose flower wine of the present invention;
Pyridinium 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;
Auxiliary agent in described step B is N, N ', N "-three n-propyl citric amides, N, N ', N " any one in-three normal-butyl citric amides.
2. preparation method as claimed in claim 1, is characterized in that: in described step B, the part by weight of pyridinium compound and auxiliary agent is 1:0.2-0.6.
3. preparation method as claimed in claim 1, is characterized in that: in described step B, the weight of additive is the 1-5% of pyridinium compound weight.
4. preparation method as claimed in claim 1, is characterized in that: in described step C, the weight ratio of rose flower and compound extractant is 1:4-6.
5. preparation method as claimed in claim 1, 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.
6. the preparation method as described in any one of claim 1-5, is characterized in that: in described step e, the weight ratio of anthocyanidin sterling and base wine is 1:600-1000.
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 |
Applications Claiming Priority (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 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104140909A CN104140909A (en) | 2014-11-12 |
| CN104140909B true CN104140909B (en) | 2015-08-19 |
Family
ID=51850251
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410354426.7A Active CN104140909B (en) | 2014-07-24 | 2014-07-24 | A kind of rose flower wine and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104140909B (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| 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 |
| 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 |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101343603A (en) * | 2008-08-15 | 2009-01-14 | 邢海明 | Rose liquor wine and preparation thereof |
| CN102994325A (en) * | 2011-09-15 | 2013-03-27 | 朱勤舟 | Rose wine and its preparation method |
| CN103524314A (en) * | 2013-10-28 | 2014-01-22 | 杨雪飞 | Preparation method for L-gossypol through high-speed countercurrent chromatography |
| CN103709136A (en) * | 2014-01-09 | 2014-04-09 | 闵令杰 | Combined type method for extracting schisandrin b from fructus schisandrae |
-
2014
- 2014-07-24 CN CN201410354426.7A patent/CN104140909B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101343603A (en) * | 2008-08-15 | 2009-01-14 | 邢海明 | Rose liquor wine and preparation thereof |
| CN102994325A (en) * | 2011-09-15 | 2013-03-27 | 朱勤舟 | Rose wine and its preparation method |
| CN103524314A (en) * | 2013-10-28 | 2014-01-22 | 杨雪飞 | Preparation method for L-gossypol through high-speed countercurrent chromatography |
| CN103709136A (en) * | 2014-01-09 | 2014-04-09 | 闵令杰 | Combined type method for extracting schisandrin b from fructus schisandrae |
Non-Patent Citations (2)
| Title |
|---|
| 玫瑰花露酒的研制;张海云;《农产品加工》;20130415;第30页的"操作要点" * |
| 花青素的提取、分离以及纯化方法研究进展;孙建霞 等;《食品与发酵工业》;20080830;第34卷(第8期);第111-117页 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN104140909A (en) | 2014-11-12 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Deineka et al. | Anthocyans from fruit of some plants of the Caprifoliaceae family | |
| D’Alessandro et al. | Integrated process extraction–adsorption for selective recovery of antioxidant phenolics from Aronia melanocarpa berries | |
| Yang et al. | Purification of anthocyanins from extracts of red raspberry using macroporous resin | |
| Ferrara et al. | Extraction of bioactive compounds of saffron (Crocus sativus L.) by ultrasound assisted extraction (UAE) and by rapid solid-liquid dynamic extraction (RSLDE) | |
| CN104140909B (en) | A kind of rose flower wine and preparation method thereof | |
| Dong et al. | Efficient removal of ginkgolic acids from Ginkgo biloba leaves crude extract by using hydrophobic deep eutectic solvents | |
| Zhang et al. | Efficient extraction of flavonoids from Polygonatum sibiricum using a deep eutectic solvent as a green extraction solvent | |
| Vayupharp et al. | Antioxidant properties and color stability of anthocyanin purified extracts from Thai waxy purple corn cob | |
| CN103265519A (en) | Method for separating and preparing proanthocyanidins in bayberry leaves | |
| Maimulyanti et al. | Development of natural deep eutectic solvent (NADES) based on choline chloride as a green solvent to extract phenolic compound from coffee husk waste | |
| Spórna-Kucab et al. | High-speed counter-current chromatography in separation of betacyanins from flowers of red Gomphrena globosa L. cultivars | |
| CN103387755B (en) | Natural complex brown pigment preparation and application thereof | |
| Bakhshayeshi et al. | The effects of light, storage temperature, pH and variety on stability of anthocyanin pigments in four Malus varieties | |
| US7261769B2 (en) | Stabilized anthocyanin extract from Garcinia indica | |
| CN110305736A (en) | A kind of preparation method of lasting fragrance flavoring apple essence material | |
| CN105315706B (en) | A kind of natural pigment color stabilizer, preparation method and application | |
| CN104483429B (en) | In Folium Camelliae sinensis, external source adds the fast and convenient detection method of 12 kinds of water solublity synthetic dyestuffs | |
| CN101845236B (en) | Method for extracting melanin from black waxy corn | |
| CN106866455A (en) | A kind of preparation method of high-purity numb-taste components | |
| RU2639291C2 (en) | Method and composition of producing dry forms of blue anthocyanins | |
| CN103725035A (en) | Method for extracting natural haematochrome and marennin from folium photiniae | |
| Sidorov et al. | Solanum retroflexum Fruits: A Rich Source of Anthocyanins | |
| KR101505311B1 (en) | Method to separate and purify vegetable ascorbic acid-2-glucoside from lycium chinense mill extract by utilizing the characteristics of sugar-binding protein | |
| CN105038298A (en) | Wheat bran purple pigment extracting method | |
| CN105175463A (en) | Extraction process for blueberry anthocyanin |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20171226 Address after: Eight Street in Anning City Yunnan province 650000 Kunming City Subdistrict Office small business area Patentee after: Yunnan legend Foods Co., Ltd. Address before: Anning City, Yunnan province 650300 Kunming City eight Street Town small area Patentee before: ANNING TANGCHUANYUAN LIQUOR INDUSTRY ECONOMIC AND TRADE CO., LTD. |