CN105533607A - Natural green kumquat flavor and preparation method thereof - Google Patents

Natural green kumquat flavor and preparation method thereof Download PDF

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Publication number
CN105533607A
CN105533607A CN201510900682.6A CN201510900682A CN105533607A CN 105533607 A CN105533607 A CN 105533607A CN 201510900682 A CN201510900682 A CN 201510900682A CN 105533607 A CN105533607 A CN 105533607A
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blue
green cumquat
green
cumquat
lemon
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CN105533607B (en
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奕志英
沈凯
杜策
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Zhejiang Lvjing Biotechnology Co., Ltd
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ZHEJIANG GREEN CRYSTAL FLAVOR CO Ltd
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Abstract

The invention discloses a natural green kumquat flavor, which comprises the following components, by weight percentage: 50-70% of a green kumquat extracted liquid, 10-20% of a sweet orange flavoring base, 10-20% of a lemon flavoring base, and 10-20% of a lemon-citrus-limetta flavoring base. The invention further discloses a preparation method of the natural green kumquat flavor. According to the method, high-quality green kumquats are taken as a raw material and are subjected to pulverization; low-temperature enzymolysis and low-temperature supersonic extraction are combined, and modern membrane separation technology is adopted to concentrate, enrich, and purify flavor substances to obtain a pure natural green kumquat flavoring base, which is a green kumquat extracted liquid and has strong fragrance, freshness, and fruit juice taste; and the green kumquat flavor is finally prepared.

Description

Blue or green cumquat natural perfume material and preparation method thereof
Technical field
The invention belongs to food ingredient technical field, particularly a kind of natural perfume material and preparation method thereof of blue or green cumquat local flavor.
Background technology
Essence and flavoring agent, as improving people's living standard, promoting one of the key factor of development of food industry, maintains in the whole world and Chinese market and steadily develops fast, and is to a certain degree that the prosperity of the world's particularly China's economic has played huge effect.But due to the continuous appearance of viewpoint of Chinese food safety event, once unlimited opportunities, mystery and the essence and flavoring agent being full of art and technological color has been coverd with negative shade, how consumer, reimage needs government in the heart, the correct direction of authoritative institution and association leads, and more needs the continuous effort of industry technology personnel.According to consumed worldwide person for green, safety, health, height that is organic and wholefood is praised highly and accreditation, and research and development and the production of natural essence spices will be the developing direction of following most potentiality.Fruit essence is as member most important in food flavor family, and the development for food industry has played huge effect.Wherein the fruits food flavor of All Pure Nature can meet people's uphold nature, returns natural life seek.
Through the development of two more than ten years, domestic and international fruit process technology constantly improves and improves, and particularly in the preservation and improvement etc. of the extraction of fruit liquid product and clarification, organoleptic quality, has larger progress: as food technologies such as counter current continuous extraction technology, enzyme engineering technology, membrane separation concentration technology, microcapsules technology, ultra-high pressure sterilization technology, hot-filling technique.The progress of comprehensive fruit drink clarification technique both at home and abroad, the enzyme membrane United Technologies that the enzyme immobilization technology based on pectase combines with Ultra filtration membrane will become the developing direction of fruit product clarification technique from now on.With the membrane separation technique of simmer down to object; By the microcapsules protected for the purpose of fragrant and flavouring and embed fruit essence technology etc. and also will become the Main way of recent fruit essence working research.
Blue or green cumquat, has another name called little blue or green tangerine, Gong Sunju, sour tangerine, green tangerine, belongs to Rutaceae, Citrus, is the fruit of the torrid zone and the evergreen dungarunga of subtropical zone Rutaceae.Blue or green cumquat is mainly planted in Chinese Hainan, and the four seasons bear fruit, and taste acid succulence, unique flavor, containing the various trace elements such as zinc, iron, have good appetizing, beauty treatment, health-care efficacy.At present, it is the same with other fruits and vegetables spices that blue or green cumquat on market extracts spices, main with spray powder, inspissated juice is main, and it is few that relevant technical literature and patent document are introduced, there is following defect in relevant blue or green cumquat aroma material preparation: 1. occurs muddy, precipitation in storage, affect product quality; 2. local flavor is not true to nature, and fragrance is impure, and natural sense is more weak, and then affects the flavor quality of blue or green cumquat goods, is not liked by consumer; 3., there is food security hidden danger in the introducing of additional food additives, essence and flavoring agent and process chemical substance.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of blue or green cumquat natural perfume material with natural aromatic sense and preparation method thereof.
In order to solve the problems of the technologies described above, the invention provides a kind of blue or green cumquat natural perfume material, it is grouped into by the one-tenth of following percentage by weight: blue or green cumquat extract 50 ~ 70%, sweet orange perfume base 10 ~ 20%, lemon perfume base 10 ~ 20%, lemon-lime perfume base 10-20%.
As the improvement of blue or green cumquat natural perfume material of the present invention, it is grouped into by the one-tenth of following percentage by weight: blue or green cumquat extract 70%, sweet orange perfume base 10%, lemon perfume base 10%, lemon-lime perfume base 10%.
The present invention also provides the preparation method of above-mentioned blue or green cumquat natural perfume material simultaneously, comprises the steps:
One), prepare burden:
Blue or green cumquat natural perfume material is grouped into by the one-tenth of following percentage by weight: blue or green cumquat extract 50 ~ 70%, sweet orange perfume base 10 ~ 20%, lemon perfume base 10 ~ 20%, lemon-lime perfume base 10 ~ 20%;
Two), sweet orange perfume base, lemon perfume base and lemon-lime perfume base are mixed 10 ~ 20min while stirring in 25 ~ 35 DEG C; Obtain perfume base liquid;
Three), in perfume base liquid add blue or green cumquat extract, stir 3 ~ 10min;
Four), by step 3) the filter membrane of membrane aperture 0.45 ~ 0.55 μm essence filter of gained liquid, the filtrate of gained, through 130 ~ 140 DEG C of (being such as 135 DEG C) sterilizing 4 ~ 6s, then sterile fillings, obtains blue or green cumquat natural perfume material.
Improvement as the preparation method of blue or green cumquat natural perfume material of the present invention: the preparation method of blue or green cumquat extract is for comprising the following steps:
1), blue or green cumquat fruit cleaning entirely:
Select ripe, that nothing is rotten blue or green cumquat to be raw material, (utilizing flowing running water) cleaning, thus remove blue or green cumquat surface impurity;
2), pulverize:
By step 1) cleaning after blue or green cumquat pulverize;
3), low temperature enzymolysis:
By step 2) blue or green cumquat citrate-phosphate salt buffer (generally selects pH value to be 4.0 ~ 7.0 citrate-phosphate salt buffers after the pulverizing of gained, being preferably pH value is 5.0 ~ 7.0 citrate-phosphate salt buffers) adjust ph is 4.5 ~ 6.5, obtains mixture;
Add the mixed enzyme accounting for mixture quality 5 ~ 15 ‰, in 30 ~ 40 DEG C of low temperature enzymolysis 4 ~ 12h;
4), freezing:
By step 3) after the enzymolysis of gained blue or green cumquat in-21 ~-25 DEG C of freezing 10 ~ 20min;
5), ultrasonic extraction:
According to the amount ratio of every 1g as blue or green cumquat adapted 3 ~ 5g absolute alcohol of raw material, in step 4) add absolute alcohol, ultrasonic extraction 15 ~ 30min under room temperature in the freezing rear blue or green cumquat of gained;
6), filter:
By step 5) extraction gains carry out plate compression in 2 ~ 4 DEG C, 5 μm, filter cloth aperture, pressure 0.1 ~ 0.15MPa;
7), ultrafiltration concentration:
Step 6) filtered solution of gained adopts 10000 ~ 40000 (being preferably 15000 ~ 40000) molecular weight membrane aperture to carry out ultrafiltration, filtration temperature 2 ~ 4 DEG C, operating pressure 0.1 ~ 0.2Mpa;
8), osmotic distillation concentrates:
Step 7) filtrate of gained enters osmotic distillation membrane module, is step 7 in the side of osmotic distillation membrane module) filtrate of gained, being the aqueous solution containing removing agent at the opposite side of osmotic distillation membrane module, carrying out osmotic distillation dehydration in 20 ~ 30 DEG C; The described aqueous solution containing removing agent is inorganic salt solution (for the inorganic salt solution that infiltration activity ratio is lower), and the mass concentration of described inorganic salts is 25% ~ 43%, and described inorganic salts are at least one in magnesium chloride, magnesium sulfate, calcium chloride;
Thus obtain blue or green cumquat extract.
Remarks illustrate: step 6) after plate compression, the mass concentration of the filtrate of gained is about 15 ~ 20%, and the mass concentration of the blue or green cumquat extract of final gained is about 40 ~ 50%.
Further improvement as the preparation method of blue or green cumquat natural perfume material of the present invention:
Described step 3) described in mixed enzyme be in pectase, cellulase, protease at least 2 kinds.
Further improvement as the preparation method of blue or green cumquat natural perfume material of the present invention:
Mixed enzyme is made up of pectase, cellulase, acid protease;
The mass ratio of pectase, cellulase, acid protease is 1.2 ~ 1:0.8 ~ 2:0.5 ~ 1.0.
Further improvement as the preparation method of blue or green cumquat natural perfume material of the present invention:
Described step 2) pulverizing be:
By step 1) cleaning after blue or green cumquat pulverize, until the granularity≤2mm (being generally 0.5 ~ 2mm) of the blue or green cumquat of 80%.Grinding time is about 10 ~ 30min.
In the preparation method of blue or green cumquat extract of the present invention, step 5) ultrasonic be extracted from the supersonic frequency of 19 ~ 21khz under carry out.Generally speaking, per kilogram is as the blue or green cumquat of raw material, and limit is slowly stirred limit probe type ultrasonic extraction apparatus and carry out ultrasonic extraction 15 ~ 30min under current strength 1.0A/25w ~ 1.2A/275w condition.
The present invention with the blue or green cumquat of high-quality (such as the blue or green cumquat in Hainan) for raw material is pulverized, combine with low temperature zymolysis technique, low temperature ultrasonic extractive technique, utilize that Modern Membrane Technology concentrates flavor substance simultaneously, enrichment, purifying, obtain fragrance sense, feeling of freshness, pure natural green grass or young crops cumquat essence base-material (blue or green cumquat extract) that fruit juice feel is stronger.
The blue or green cumquat natural perfume material full aroma adopting the inventive method to prepare is mellow and full, strong mellow; Meanwhile, the natural blue or green cumquat spices utilizing the method to prepare, eliminate the material such as macro-molecular protein, tartaric acid affecting product special flavour, stability, retain the flavour nutrient such as aromatic substance, Vc material, clarity and stability are all significantly improved, make again product have obvious flavouring and protect fragrant effect, expand the range of application of product.
In the present invention: the enzyme of pectase (food-grade) is lived as >=7 ten thousand u/ml, the enzyme of cellulase (food-grade) is lived as >=5 ten thousand u/ml, acid protease enzyme is lived as >=80 ten thousand u/ml, above-mentioned pectase, cellulase, acid protease are liquid, can purchased from Shandong Longke Enzyme Co., Ltd..
Sweet orange perfume base, lemon perfume base, lemon-lime perfume base all can purchased from Fen Meiyi spices Co., Ltds, sweet orange perfume base goods number: 583703T; Lemon perfume base goods number: 502142T; Lemon-lime perfume base goods number: 051127A;
The present invention has following advantage and disadvantage:
1, the preparation of blue or green cumquat extract of the present invention: (1) is by ferment treatment and ultrasonic process, slightly solubility component in blue or green cumquat slag can be impelled effectively to change and to turn to soluble component, along with enzyme reaction is goed deep into and ultrasonic further destruction of impelling institutional framework, increase cell membrane, membrane passage, be conducive to the release of endogenous thing, leach, the degree of depth being conducive to reacting is carried out, and makes blue or green cumquat class extract (the blue or green cumquat extract) inclusion for preparing abundanter.The effect of enzyme addition makes blue or green Fortunella Margarita structure become loose, and be conducive to realizing being separated of blue or green cumquat slag and liquid in slurries, be conducive to improving follow-up process, as shortened the operating process times such as separation, filtration, in technique, realizability is strong.(2) then raw material is carried out ultrasonic extraction through freezing processing, not only can improve the recovery rate of blue or green cumquat active ingredient, simultaneously can the activity of polyphenol oxidase in the blue or green cumquat of passivation, prevent enzymatic browning and the non-enzymatic oxidation of process, effectively prevent the oxidational losses of blue or green cumquat active ingredient.(3) omnidistance employing low temperature processing techniques, decreases the technique of high temperature water extraction, not only effectively improves the leaching rate of blue or green cumquat active ingredient, and avoid refining losses, remain the natural flavor of blue or green cumquat to greatest extent, especially the fragrant composition of head.
Ultrafiltration and osmotic distillation is adopted in the preparation of 2, the blue or green cumquat extract of the present invention, remove the material such as macro-molecular protein, tartaric acid affecting product special flavour, stability, retain the flavour nutrient such as aromatic substance, Vc material, thus improve the non-biostability of the natural blue or green cumquat spices of finished product, serve obvious flavouring and protect fragrant effect.
3, adopt the natural blue or green cumquat spices of the inventive method gained can retain fragrance component to the full extent, environmentally safe, there is advantage technically obvious and economically.
Detailed description of the invention
The present invention is described below by specific embodiment.Unless stated otherwise, technological means used in the present invention is method known in those skilled in the art.In addition, embodiment is interpreted as illustrative, but not limits the scope of the invention, and the spirit and scope of the invention only limited by claims.To those skilled in the art, under the prerequisite not deviating from essence of the present invention and scope, the various change carry out the material component in these embodiments and consumption or change also belong to protection scope of the present invention.
Embodiment 1, a kind of blue or green cumquat natural perfume material, be grouped into by the one-tenth of following percentage by weight:
Blue or green cumquat extract 50%, sweet orange perfume base 10%, lemon perfume base 20%, lemon-lime perfume base 20%.
One, the preparation method of blue or green cumquat extract is for carry out following steps successively:
1), blue or green cumquat fruit cleaning entirely: select the blue or green cumquat of 1Kg that maturity is high, nothing is rotted to be raw material, utilize flowing running water clean thus remove blue or green cumquat surface impurity.
2), pulverize: by step 1) cleaning after blue or green cumquat pulverize rapidly, grinding time is about 10min, and now degree of fragmentation reaches 85%, and granularity reaches 2mm.
3), low temperature enzymolysis:
By step 2) blue or green cumquat citrate-phosphate salt buffer (pH5.0 ~ 6.0 citrate-phosphate salt buffer) adjust ph is 4.5 after the pulverizing of gained, obtains mixture;
Add the mixed enzyme of mixture quality 5 ‰, in 40 DEG C of low temperature enzymolysis 4h;
Described mixed enzyme is made up of pectase, cellulase, acid protease;
The mass ratio of described pectase, cellulase, acid protease mixing is 1.2:0.8:1.0.
4), freezing:
By step 3) after the enzymolysis of gained blue or green cumquat in-21 DEG C of freezing 20min.
5), ultrasonic extraction:
By step 4) the freezing rear blue or green cumquat of gained is placed in pill tank, and add 5Kg absolute alcohol, under room temperature, limit is slowly stirred limit probe type ultrasonic extraction apparatus and carry out ultrasonic extraction 15min under the supersonic frequency, current strength 1.2A/275w condition of 20khz.
6), filter:
By step 5) extraction gains carry out plate compression in 2 DEG C, 5 μm, filter cloth aperture, pressure 0.15Mpa.
7), ultrafiltration concentration:
Step 6) filtered solution of gained adopts 40000 molecular weight membrane aperture to carry out ultrafiltration, filtration temperature 2 DEG C, operating pressure 0.1Mpa.
8), osmotic distillation concentrates:
Step 7) filtrate of gained enters osmotic distillation membrane module, step 7 in the side of osmotic distillation membrane module) filtrate of gained, at the aqueous solution that the opposite side of osmotic distillation membrane module is containing removing agent, removing agent and being obtained by mixing according to 1:1 mass ratio by magnesium chloride, magnesium sulfate; In this aqueous solution, the mass concentration sum of magnesium chloride, magnesium sulfate is 25%; Osmotic distillation dehydration is carried out in 20 DEG C; Thus obtain blue or green cumquat extract (about 2.5kg).
Remarks illustrate: step 6) after plate compression, the mass concentration of the filtrate of gained is about 20%, and the mass concentration of the blue or green cumquat extract of final gained is about 40%.That is, through osmotic distillation dehydration, after concentrated, blue or green cumquat concentration of perfume brings up to 40% from 20%.
Blue or green cumquat concentration of perfume can adopt hand-hold refractometer to measure, and this is routine techniques.
Two, the preparation method of above-mentioned blue or green cumquat natural perfume material, comprises the steps:
Accurately take sweet orange perfume base, lemon perfume base and lemon-lime perfume base according to above-mentioned formula rate, mix 20min while stirring in 25 DEG C; Then add the blue or green cumquat extract of above-mentioned formula rate, slowly stir 3min; Finally in the filter membrane essence filter of membrane aperture 0.45 μm, filtered solution through 135 DEG C of sterilizing 4s, then sterile fillings, both blue or green cumquat natural perfume material.
Embodiment 2, a kind of blue or green cumquat natural perfume material are grouped into by the one-tenth of following percentage by weight:
Blue or green cumquat extract 70%, sweet orange perfume base 10%, lemon perfume base 10%, lemon-lime perfume base 10%;
One, the preparation method of blue or green cumquat extract is for carry out following steps successively:
1), blue or green cumquat fruit cleaning entirely: select the blue or green cumquat of 1Kg that maturity is high, nothing is rotted to be raw material, utilize flowing running water clean thus remove blue or green cumquat surface impurity.
2), pulverize: by step 1) cleaning after blue or green cumquat pulverize rapidly, grinding time is about 30min, and now degree of fragmentation reaches 95%, and granularity reaches 1mm.
3), low temperature enzymolysis:
By step 2) blue or green cumquat citrate-phosphate salt buffer (pH6.0 ~ 7.0 citrate-phosphate salt buffer) adjust ph is 5.5 after the pulverizing of gained, obtains mixture;
Add the mixed enzyme of mixture quality 10 ‰, in 30 DEG C of low temperature enzymolysis 12h;
Described mixed enzyme is made up of pectase, cellulase, acid protease;
The mass ratio of described pectase, cellulase, acid protease mixing is 1:1:0.5.
4), freezing:
By step 3) after the enzymolysis of gained blue or green cumquat in-25 DEG C of freezing 10min.
5), ultrasonic extraction:
By step 4) the freezing rear blue or green cumquat of gained is placed in pill tank, and add 3Kg absolute alcohol, under room temperature, limit is slowly stirred limit probe type ultrasonic extraction apparatus and carry out ultrasonic extraction 30min under the supersonic frequency, current strength 1.0A/25w condition of 20khz.
6), filter:
By step 5) extraction gains carry out plate compression in 4 DEG C, 5 μm, filter cloth aperture, pressure 0.1Mpa.
7), ultrafiltration concentration:
Step 6) filtered solution of gained adopts 15000 molecular weight membrane aperture to carry out ultrafiltration, filtration temperature 4 DEG C, operating pressure 0.2Mpa.
8), osmotic distillation concentrates:
Step 7) filtrate of gained enters osmotic distillation membrane module, step 7 in the side of osmotic distillation membrane module) filtrate of gained, at the aqueous solution that the opposite side of osmotic distillation membrane module is containing removing agent, removing agent is magnesium chloride, and its mass concentration is 30%; Osmotic distillation dehydration is carried out in 30 DEG C.Thus obtain blue or green cumquat extract (about 1.8kg).
Remarks illustrate: through osmotic distillation dehydration, after concentrated, blue or green cumquat concentration of perfume brings up to 45% from 25%.
Two, the preparation method of above-mentioned blue or green cumquat natural perfume material, comprises the steps:
Accurately take sweet orange perfume base, lemon perfume base and lemon-lime perfume base according to above-mentioned formula rate, mix 10min while stirring in 30 DEG C; Then add the blue or green cumquat extract of above-mentioned formula rate, slowly stir 5min; Finally in the filter membrane essence filter of membrane aperture 0.55 μm, filtered solution through 135 DEG C of sterilizing 6s, then sterile fillings, both blue or green cumquat natural perfume material.
Embodiment 3, a kind of blue or green cumquat natural perfume material, be grouped into by the one-tenth of following percentage by weight:
Blue or green cumquat extract 55%, sweet orange perfume base 15%, lemon perfume base 15%, lemon-lime perfume base 15%.
One, the preparation method of blue or green cumquat extract is for carry out following steps successively:
1), blue or green cumquat fruit cleaning entirely: select the blue or green cumquat of 1Kg that maturity is high, nothing is rotted to be raw material, utilize flowing running water clean thus remove blue or green cumquat surface impurity.
2), pulverize: by step 1) cleaning after blue or green cumquat pulverize rapidly, grinding time is about 20min, and now degree of fragmentation reaches 90%, and granularity reaches 0.5mm.
3), low temperature enzymolysis:
By step 2) blue or green cumquat citrate-phosphate salt buffer (pH7.0 citrate-phosphate salt buffer) adjust ph is 6.5 after the pulverizing of gained, obtains mixture;
Add the mixed enzyme of mixture quality 15 ‰, in 35 DEG C of low temperature enzymolysis 8h;
Described mixed enzyme is made up of pectase, cellulase, acid protease;
The mass ratio of described pectase, cellulase, acid protease mixing is 1:2:1.
4), freezing:
By step 3) after the enzymolysis of gained blue or green cumquat in-23 DEG C of freezing 15min.
5), ultrasonic extraction:
By step 4) the freezing rear blue or green cumquat of gained is placed in pill tank, and add 4Kg absolute alcohol, under room temperature, limit is slowly stirred limit probe type ultrasonic extraction apparatus and carry out ultrasonic extraction 20min under the supersonic frequency, current strength 1.1A/100w condition of 20khz.
6), filter:
By step 5) extraction gains carry out plate compression in 3 DEG C, 5 μm, filter cloth aperture, pressure 0.12Mpa.
7), ultrafiltration concentration:
Step 6) filtered solution of gained adopts 30000 molecular weight membrane aperture to carry out ultrafiltration, filtration temperature 3 DEG C, operating pressure 0.15Mpa.
8), osmotic distillation concentrates:
Step 7) filtrate of gained enters osmotic distillation membrane module, step 7 in the side of osmotic distillation membrane module) filtrate of gained, at the aqueous solution that the opposite side of osmotic distillation membrane module is containing removing agent, removing agent and being obtained by mixing according to 1:1:1 mass ratio by magnesium chloride, magnesium sulfate, calcium chloride; The mass concentration sum of magnesium chloride, magnesium sulfate, calcium chloride is 43%; Osmotic distillation dehydration is carried out at 30 DEG C; Thus obtain blue or green cumquat extract (2.5kg).
Through osmotic distillation dehydration, after concentrated, blue or green cumquat concentration of perfume brings up to 45% from 25%.
Two, the preparation method of above-mentioned blue or green cumquat natural perfume material, comprises the steps:
Accurately take sweet orange perfume base, lemon perfume base and lemon-lime perfume base according to above-mentioned formula rate, mix 15min while stirring in 25 DEG C; Then the blue or green cumquat extract of above-mentioned formula rate is added, slow stirring and dissolving 4min; Finally in the filter membrane essence filter of membrane aperture 0.5 μm, filtered solution through 135 DEG C of sterilizing 5s, then sterile fillings, both blue or green cumquat natural perfume material.
Comparative example 1-1, blue or green cumquat natural perfume material is made into by the raw material of following percentage by weight formulated: blue or green cumquat extract 70%, sweet orange perfume base 10%, lemon perfume base 20%; All the other contents are equal to embodiment 2.
Comparative example 1-2, blue or green cumquat natural perfume material is made into by the raw material of following percentage by weight formulated: blue or green cumquat extract 70%, sweet orange perfume base 10%, lemon-lime perfume base 20%; All the other contents are equal to embodiment 2.
Comparative example 1-3, blue or green cumquat natural perfume material is made into by the raw material of following percentage by weight formulated: blue or green cumquat extract 70%, lemon perfume base 15%, lemon-lime perfume base 15%; All the other contents are equal to embodiment 2.
Comparative example 1-4, blue or green cumquat natural perfume material is made into by the raw material of following percentage by weight formulated: blue or green cumquat extract 70%, sweet orange perfume base 20%, lemon perfume base 5%, lemon-lime perfume base 5%; All the other contents are equal to embodiment 2.
Comparative example 1-5, blue or green cumquat natural perfume material is made into by the raw material of following percentage by weight formulated: blue or green cumquat extract 70%, sweet orange perfume base 15%, lemon perfume base 5%, lemon-lime perfume base 10%; All the other contents are equal to embodiment 2.
Comparative example 1-6, blue or green cumquat natural perfume material is made into by the raw material of following percentage by weight formulated: blue or green cumquat extract 70%, sweet orange perfume base 5%, lemon perfume base 15%, lemon-lime perfume base 10%; All the other contents are equal to embodiment 2.
Comparative example 1-7, blue or green cumquat natural perfume material is made into by the raw material of following percentage by weight formulated: blue or green cumquat extract 70%, sweet orange perfume base 15%, lemon perfume base 10%, lemon-lime perfume base 5%; All the other contents are equal to embodiment 2.
Comparative example 1-8, blue or green cumquat natural perfume material is made into by the raw material of following percentage by weight formulated: blue or green cumquat extract 70%, sweet orange perfume base 5%, lemon perfume base 10%, lemon-lime perfume base 15%; All the other contents are equal to embodiment 2.
Comparative example 2-1, the preparation method of the blue or green cumquat extract of embodiment 2 to be made the following changes: cancellation step 4) freezing, that is, by step 3) enzymolysis after blue or green cumquat directly carry out follow-up step 5) ultrasonic extraction; All the other contents are equal to embodiment 2.
Comparative example 2-2, by the step 4 in the preparation method of the blue or green cumquat extract of embodiment 2) make the following changes: " in-25 DEG C of freezing 10min " are made into " in-50 DEG C of freezing 5min ".All the other contents are equal to embodiment 2.
Comparative example 2-3, by the step 4 in the preparation method of the blue or green cumquat extract of embodiment 2) make the following changes: " in-25 DEG C of freezing 10min " are made into " in-5 DEG C of freezing 20min ".All the other contents are equal to embodiment 2.
Comparative example 3-1, by the step 3 in the preparation method of the blue or green cumquat extract of embodiment 2) make the following changes: make pectase, cellulase, acid protease into 1:0.5:1 by 1:1:0.5; All the other contents are equal to embodiment 2.
Comparative example 3-2, by the step 3 in the preparation method of the blue or green cumquat extract of embodiment 2) make the following changes: make pectase, cellulase, acid protease into 0.5:1:1 by 1:1:0.5; All the other contents are equal to embodiment 2.
Comparative example 3-3, by the step 3 in the preparation method of the blue or green cumquat extract of embodiment 2) make the following changes: " 30 DEG C of low temperature enzymolysis 12h " is made into " in 50 DEG C of enzymolysis 12h ", and all the other contents are equal to embodiment 2.
Experiment:
By above-mentioned all embodiments and comparative example according to GBT14454.2-2008 " spices fragrance assessment method ", ask 10 experts to carry out sensory evaluation, provide scoring.
The method of sensory evaluation is: select 10 to blue or green cumquat fragrance than more sensitive evaluation personnel, and early stage carries out Simulation evaluation, shows the difference that these sensory evaluation persons all can distinguish blue or green cumquat fragrance sample room in various degree.Simultaneously, all sensory evaluation personnel are provided and directly to be squeezed the juice gained juice sample in contrast by fresh blue or green cumquat, sensory evaluation personnel are allowed to carry out giving a mark 1 ~ 9 point of scope according to the fragrance degree of closeness of the fragrance of example and control sample, more higher close to mark with control sample, have peculiar smell or the light then mark of fragrance low.The identical embodiment finally provided 10 valuation officers or comparative example evaluation score are added up, and adopt Q method of inspection to carry out analysiss rejecting, then average to evaluation score, report the result as shown in table 1 exceptional value.Result shows, comparative example and embodiment 2 all exist significant difference.
Table 1
Finally, it is also to be noted that what enumerate above is only several specific embodiments of the present invention.Obviously, the invention is not restricted to above embodiment, many distortion can also be had.All distortion that those of ordinary skill in the art can directly derive from content disclosed by the invention or associate, all should think protection scope of the present invention.

Claims (7)

1. blue or green cumquat natural perfume material, is characterized in that being grouped into by the one-tenth of following percentage by weight: blue or green cumquat extract 50 ~ 70%, sweet orange perfume base 10 ~ 20%, lemon perfume base 10 ~ 20%, lemon-lime perfume base 10-20%.
2. blue or green cumquat natural perfume material according to claim 1, is characterized in that being grouped into by the one-tenth of following percentage by weight: blue or green cumquat extract 70%, sweet orange perfume base 10%, lemon perfume base 10%, lemon-lime perfume base 10%.
3. the preparation method of blue or green cumquat natural perfume material, is characterized in that comprising the steps:
One), prepare burden:
Blue or green cumquat natural perfume material is grouped into by the one-tenth of following percentage by weight: blue or green cumquat extract 50 ~ 70%, sweet orange perfume base 10 ~ 20%, lemon perfume base 10 ~ 20%, lemon-lime perfume base 10 ~ 20%;
Two), sweet orange perfume base, lemon perfume base and lemon-lime perfume base are mixed 10 ~ 20min while stirring in 25 ~ 35 DEG C; Obtain perfume base liquid;
Three), in perfume base liquid add blue or green cumquat extract, stir 3 ~ 10min;
Four), by step 3) the filter membrane of membrane aperture 0.45 ~ 0.55 μm essence filter of gained liquid, the filtrate of gained, through 130 ~ 140 DEG C of sterilizing 4 ~ 6s, then sterile fillings, obtains blue or green cumquat natural perfume material.
4. the preparation method of blue or green cumquat natural perfume material according to claim 3, is characterized in that the preparation method of blue or green cumquat extract is for comprising the following steps:
1), blue or green cumquat fruit cleaning entirely:
Select ripe, that nothing is rotten blue or green cumquat to be raw material, cleaning, thus remove blue or green cumquat surface impurity;
2), pulverize:
By step 1) cleaning after blue or green cumquat pulverize;
3), low temperature enzymolysis:
By step 2) blue or green cumquat citrate-phosphate salt buffer adjust ph is 4.5 ~ 6.5 after the pulverizing of gained, obtains mixture;
Add the mixed enzyme accounting for mixture quality 5 ~ 15 ‰, in 30 ~ 40 DEG C of low temperature enzymolysis 4 ~ 12h;
4), freezing:
By step 3) after the enzymolysis of gained blue or green cumquat in-21 ~-25 DEG C of freezing 10 ~ 20min;
5), ultrasonic extraction:
According to the amount ratio of every 1g as blue or green cumquat adapted 3 ~ 5g absolute alcohol of raw material, in step 4) add absolute alcohol, ultrasonic extraction 15 ~ 30min under room temperature in the freezing rear blue or green cumquat of gained;
6), filter:
By step 5) extraction gains carry out plate compression in 2 ~ 4 DEG C, 5 μm, filter cloth aperture, pressure 0.1 ~ 0.15MPa;
7), ultrafiltration concentration:
Step 6) gained filtered solution adopt 10000 ~ 40000 molecular weight membrane aperture carry out ultrafiltration, filtration temperature 2 ~ 4 DEG C, operating pressure 0.1 ~ 0.2Mpa;
8), osmotic distillation concentrates:
Step 7) filtrate of gained enters osmotic distillation membrane module, is step 7 in the side of osmotic distillation membrane module) filtrate of gained, being the aqueous solution containing removing agent at the opposite side of osmotic distillation membrane module, carrying out osmotic distillation dehydration in 20 ~ 30 DEG C; The described aqueous solution containing removing agent is inorganic salt solution, and the mass concentration of described inorganic salts is 25% ~ 43%, and described inorganic salts are at least one in magnesium chloride, magnesium sulfate, calcium chloride;
Thus obtain blue or green cumquat extract.
5. the preparation method of blue or green cumquat natural perfume material according to claim 4, is characterized in that:
Described step 3) described in mixed enzyme be in pectase, cellulase, acid protease at least 2 kinds.
6. the preparation method of blue or green cumquat natural perfume material according to claim 5, is characterized in that:
Mixed enzyme is made up of pectase, cellulase, acid protease;
The mass ratio of pectase, cellulase, acid protease is 1.2 ~ 1:0.8 ~ 2:0.5 ~ 1.0.
7. the preparation method of the blue or green cumquat natural perfume material according to claim 5 or 6, is characterized in that:
Described step 2) pulverizing be:
By step 1) cleaning after blue or green cumquat pulverize, until the granularity≤2mm of the blue or green cumquat of 80%.
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CN114886147A (en) * 2022-06-10 2022-08-12 云南中烟新材料科技有限公司 Extraction method of old medicine orange spice and application of old medicine orange spice in cigarettes

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