CN107011697A - A kind of preparation method of mulberry red pigment powder - Google Patents
A kind of preparation method of mulberry red pigment powder Download PDFInfo
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- CN107011697A CN107011697A CN201710212260.9A CN201710212260A CN107011697A CN 107011697 A CN107011697 A CN 107011697A CN 201710212260 A CN201710212260 A CN 201710212260A CN 107011697 A CN107011697 A CN 107011697A
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- red pigment
- mulberry
- preparation
- pigment powder
- mulberry red
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B61/00—Dyes of natural origin prepared from natural sources, e.g. vegetable sources
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D311/00—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings
- C07D311/02—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings ortho- or peri-condensed with carbocyclic rings or ring systems
- C07D311/04—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring
- C07D311/58—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring other than with oxygen or sulphur atoms in position 2 or 4
- C07D311/60—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring other than with oxygen or sulphur atoms in position 2 or 4 with aryl radicals attached in position 2
- C07D311/62—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring other than with oxygen or sulphur atoms in position 2 or 4 with aryl radicals attached in position 2 with oxygen atoms directly attached in position 3, e.g. anthocyanidins
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B67/00—Influencing the physical, e.g. the dyeing or printing properties of dyestuffs without chemical reactions, e.g. by treating with solvents grinding or grinding assistants, coating of pigments or dyes; Process features in the making of dyestuff preparations; Dyestuff preparations of a special physical nature, e.g. tablets, films
- C09B67/0096—Purification; Precipitation; Filtration
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Coloring Foods And Improving Nutritive Qualities (AREA)
- Medicines Containing Plant Substances (AREA)
Abstract
The invention discloses a kind of preparation method of mulberry red pigment powder, its preparation process is first mixes mulberry fruit homogenate and extractant, under room temperature environment, by Ultrasonic Wave-Assisted Extraction, filtering, takes filtrate；Then filtrate alcohol concentration is adjusted, 4 DEG C of refrigerator overnights is placed in, the filtrate after standing is centrifuged, extract solution is made, polysaccharide concentration is adjusted；Extract solution is spray-dried, collects and is preserved at the powder in drying bottle, hermetically drying.This method is easy to operate, with low cost, is adapted to anthocyanidin content height in scale industrial production, gained mulberry red pigment powder product, and the holding time is long, is readily transported, rehydration is good.
Description
Technical field
The present invention relates to a kind of preparation method of pigment, and in particular to a kind of preparation method of mulberry red pigment powder, belongs to
Fruits and vegetables deep process technology field.
Background technology
Mulberry red pigment is the anthocyanidin that a class is present in mulberry fruit, in its natural state in the form of anthocyanin
In the presence of.Anthocyanin has the effects such as removing free radical, nourishing qi and blood.
The mulberry red pigment extracting method reported mainly has solvent extraction method, extraction, resin method of purification etc..Wu Min etc.
(" Study on extraction of haematochrome in mulberry fruit dry fruit ", Food Additives Used in China, 2008,4:64-68) report mulberry fruit dry fruit
By broken, extraction, centrifugation, mulberry pigment extract solution is obtained, determines that optimal extract process is：The mesh of raw material granularity 30, material
Liquor ratio 1: 20, Extraction solvent 0.33%HCl -60% ethanol, extraction time 30min, 50 DEG C of Extracting temperature obtains pigment medicinal extract color
Valency is up to 6.9, and the extraction method is simple to operate, but the efficiency of obtained mulberry red pigment is low and can not obtain powder-product.Wang Fang
(" mulberry pigment Study on extraction ", Master's thesis, 2013) uses aqueous two-phase extraction mulberry pigment；Chinese patent
CN201410649922.5 is disclosed " a kind of method that utilization mulberry fruit slag prepares mulberry pigment ", and the method extracts obtained product
Impurity is few, but operation is complex, is not suitable with industrialized production.Chen Meihong etc. isolates and purifies mulberry fruit with NKA type macroreticular resins
Haematochrome, obtains mulberry red pigment powder, color value is 47 times of non-purification process, but the operating time is long, and cost is high, is not suitable for
For industrial production.
It is generally the medicinal extract state obtained with solvent extraction to extract mulberry red pigment at present, and powdered mulberry pigment product is generally
Directly crushed after drying, or crush obtained after vacuum freeze drying, mulberry pigment medicinal extract is dried using being above restricted
Powder active component loses serious, and vacuum freeze drying is costly.Spray drying technology is produced pigmented powder and starched in blueberry, strawberry etc.
In fruit it has been reported that but due in mulberry fruit sugar content be significantly higher than blueberry, strawberry etc., and sugar their glass at high operating temperatures
Glass state conversion temperature (Tg) is 51 DEG C, and the instantaneous temperature (200 DEG C) in spray-drying process exceeds well over its conversion temperature, makes sugar
Viscosity increase, while lumpd because of its thermoplasticity and hygroscopicity, so the high material of sugar content is difficult dry by spraying
Dry technology realizes drying.Therefore, the fabrication process condition of mulberry pigment turns into the Pinch technology for preparing mulberry pigment.
The content of the invention
The technical problem of solution：For the above-mentioned deficiency of prior art, the invention provides a kind of mulberry red pigment powder
Preparation method, by ultrasonic assistant extract pigment and improve spray drying method, improve mulberry red pigment recovery rate and
Activity, and reduce cost.
Technical scheme, a kind of preparation method for mulberry red pigment powder that the present invention is provided, including following preparation process：
(1) fresh mulberry fruit is ground to form into homogenate with extractant by 1:8-10 mass ratio is mixed, and is put under room temperature environment, is passed through
Ultrasonic Wave-Assisted Extraction 60-65min, filters, takes filtrate；The extractant is 0.1%HCl and the mixture of 60% ethanol；
(2) alcohol concentration of filtrate obtained by regulating step (1) is 50-55%, and 12-14h is stood in 4 DEG C of refrigerators, to standing
Filtrate afterwards carries out centrifugation 10min, takes supernatant, and mulberry red pigment extract solution is made in repeated centrifugation process 2-3 times, and control is carried
Polysaccharide concentration is taken in liquid in the range of 90-100 μ g/ml；
(3) extract solution obtained by step (2) is added into spray dryer spray drying 20-30min and obtains mulberry red pigment powder,
Take and preserved at the powder after spray drying, hermetically drying.
The ultrasonic power is 398-405W；The volume ratio of the 0.1%HCl and 60% ethanol is 1:99；The centrifugation
Rotating speed is 8000-8500r/min.The spray dryer intake air temperature is 92-95 DEG C, and air outlet temperature is 65-68 DEG C, is entered
Sample speed is 335-340ml/min.
Beneficial effect：(1) mulberry red pigment powder output capacity of the present invention is high, and the recovery rate of mulberry pigment is 92%, through spraying
Final pigment powder yield more than 3.75% is dried, powder is fine and smooth, and no adhesion is in good condition；
(2) color value of mulberry red pigment powder of the present invention is 20-22, is much higher than the mulberry fruit medicinal extract of prior art preparation
Color value 6.9-12, property of pigment is stable, and pH is 2.5-8.5；
(3) mulberry red pigment powder finished product of the present invention is powdered, it is easy to preserved and transport.
Brief description of the drawings
Fig. 1 is influence curve figures of the different pH to pigment stability；
Influence curve figure of Fig. 2 different metal ions to pigment stability.
Embodiment
The present invention is further illustrated below by the mode of embodiment, but therefore protection scope of the present invention is not confined to
Following embodiments, but limited by description and claims of this specification.
Embodiment 1
(1) extraction of mulberry pigment：Mulberry fruit is ground to form into homogenate with extractant by 1:8-10 mass ratio is mixed, in 25 DEG C
Under room temperature environment, ultrasonic wave added extraction (ultrasonic power 398-405W, ultrasonic time 60-65min), filtering take filtrate.
(2) prepared by sample liquid：It is 50% to adjust filtrate alcohol concentration, 12-14h is stood in 4 DEG C of refrigerators, to the filtrate after standing
Centrifugation 10min is carried out, centrifugal condition is 8000r/min, takes supernatant.Repeat this process 2-3 times, sample solution is made, and make
The concentration of polysaccharide is maintained at 90-100 μ g/ml in sample solution.
(3) it is spray-dried：It is 92 DEG C of intake air temperature to keep spray dryer working condition, and 65 DEG C of air outlet temperature is entered
Sample speed 335ml/min, adds sample solution.
(4) finished product is collected：Gently wiped and preserved at the powder taken in drying bottle, hermetically drying with hairbrush.
In summary, preparation technology flow of the invention：Mulberry fruit fresh fruit homogenate-ultrasonic assistant extraction-centrifugation-control
Polyoses content-spray drying-sample collection processed.
The research of mulberry pigment extraction process is shown：Solid-liquid ratio, ultrasonic time, ultrasonic power are to mulberry pigment recovery rate
Influence is the most notable.Response surface analysis is carried out using Design-expert 8 and determines optimum process, is determined according to response surface analysis
Optimum extraction process is：Solid-liquid ratio 1:8, ultrasonic power 398W, ultrasonic time 60min.The sample liquid flower prepared in checking test
Blue or green cellulose content is 0.176mg/ml, meets the predicted value of response surface analysis, reproducible.
The preparation of step (2) sample liquid, is the committed step that mulberry pigment powder is produced in spray drying, if total starches in sample liquid
Content can not be effectively reduced, then mulberry pigment can not form good pulverulence when being spray-dried, but paste
In drying bottle and cooling tower wall, it is impossible to obtain.The key factor that influence spray drying prepares mulberry red pigment powder is sample liquid
Middle polyoses content, as a result such as table 1：
Influence of the polyoses content of table 1 to spray drying effect
| Polysaccharide concentration μ g/ml | 80 | 100 | 120 | 140 |
| Product state | Aubergine powder | Atropurpureus powder | Atropurpureus coarse granule | The deadlocked thing of atropurpureus |
| Acquisition degree | Easily | Easily | It is more difficult | It is difficult |
Mulberry red pigment powder rehydration prepared by the present invention is good, redissolves stable in property after water.
It has studied the stability of different pH, different metal ions to mulberry red pigment under the conditions of different time.As a result table
Bright, mulberry red pigment powder prepared by this method is redissolved in after water, under 4 DEG C of constant temperature, non-illuminated conditions, in 96 hours, is inhaled
Light value maintains dynamic equilibrium；Under the conditions of pH 2.5, pH 4.5, pH 8.5, pigment light absorption value stability is good (such as Fig. 1)；
Under the conditions of pH10.5, pigmentary structures destruction, light absorption value declines rapidly (such as Fig. 1).Metal ion Na+, K+, Ca2+ are with processing time
Extension it is smaller to the stability influence of pigment, three metal ion species are followed successively by mulberry pigment stability：Ca2+ ＞ Na+ ＞ K+
(such as Fig. 2).
Claims (5)
1. a kind of preparation method of mulberry red pigment powder, it is characterised in that comprise the following steps：
(1) fresh mulberry fruit is ground to form into homogenate with extractant by 1:8-10 mass ratio is mixed, and is put under room temperature environment, is passed through ultrasound
Ripple Assisted Extraction 60-65min, filters, takes filtrate；The extractant is 0.1%HCl and the mixture of 60% ethanol；
(2) alcohol concentration of filtrate obtained by regulating step (1) is 50-55%, 12-14h is stood in 4 DEG C of refrigerators, after standing
Filtrate carries out centrifugation 10-15min, takes supernatant, and mulberry red pigment extract solution is made in repeated centrifugation process 2-3 times, and control is extracted
Polysaccharide concentration is in the range of 90-100 μ g/ml in liquid；
(3) extract solution obtained by step (2) is added after spray dryer spray drying 20-30min, obtains mulberry red pigment powder,
Take and preserved at the powder after spray drying, hermetically drying.
2. a kind of preparation method of mulberry red pigment powder according to claim 1, it is characterised in that step (1) described ultrasound
Power is 398-405W.
3. the preparation method of a kind of mulberry red pigment powder according to claim 1, it is characterised in that step (1) is described to be extracted
The volume ratio of 0.1%HCl and 60% ethanol is 1 in agent:99.
4. a kind of preparation method of mulberry red pigment powder according to claim 1, it is characterised in that step (2) centrifugation
Rotating speed is 8000-8500r/min.
5. a kind of preparation method of mulberry red pigment powder according to claim 1, it is characterised in that step (3) spraying
Dryer entrance mouthful temperature is 92-95 DEG C, and air outlet temperature is 65-68 DEG C, and sample introduction speed is 335-340ml/min.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710212260.9A CN107011697A (en) | 2017-04-01 | 2017-04-01 | A kind of preparation method of mulberry red pigment powder |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710212260.9A CN107011697A (en) | 2017-04-01 | 2017-04-01 | A kind of preparation method of mulberry red pigment powder |
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| CN107011697A true CN107011697A (en) | 2017-08-04 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111084352A (en) * | 2019-12-24 | 2020-05-01 | 贵州师范大学 | Mulberry refined powder preparation method and product |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102212053A (en) * | 2011-04-16 | 2011-10-12 | 湖州柳荫生物科技有限公司 | Method for extracting mulberry cyanidin |
| CN102382485A (en) * | 2011-09-23 | 2012-03-21 | 天津市尖峰天然产物研究开发有限公司 | Method for extracting anthocyanin from mulberries |
| CN103319911A (en) * | 2013-07-17 | 2013-09-25 | 黄香利 | Technology for extracting mulberry haematochrome from mulberry residue |
-
2017
- 2017-04-01 CN CN201710212260.9A patent/CN107011697A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102212053A (en) * | 2011-04-16 | 2011-10-12 | 湖州柳荫生物科技有限公司 | Method for extracting mulberry cyanidin |
| CN102382485A (en) * | 2011-09-23 | 2012-03-21 | 天津市尖峰天然产物研究开发有限公司 | Method for extracting anthocyanin from mulberries |
| CN103319911A (en) * | 2013-07-17 | 2013-09-25 | 黄香利 | Technology for extracting mulberry haematochrome from mulberry residue |
Non-Patent Citations (1)
| Title |
|---|
| 陈运中编著: "《天然色素的生产及应用》", 31 March 2007, 中国轻工业出版社 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111084352A (en) * | 2019-12-24 | 2020-05-01 | 贵州师范大学 | Mulberry refined powder preparation method and product |
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