CN116462987B - Preparation method of acid-stable butterfly bean flower blue pigment - Google Patents

Preparation method of acid-stable butterfly bean flower blue pigment Download PDF

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Publication number
CN116462987B
CN116462987B CN202310470326.XA CN202310470326A CN116462987B CN 116462987 B CN116462987 B CN 116462987B CN 202310470326 A CN202310470326 A CN 202310470326A CN 116462987 B CN116462987 B CN 116462987B
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acid
product
water
stable
blue pigment
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CN116462987A (en
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李言威
王毅
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Shaanxi Aozhixing Biotechnology Co ltd
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Shaanxi Aozhixing Biotechnology Co ltd
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09BORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
    • C09B61/00Dyes of natural origin prepared from natural sources, e.g. vegetable sources
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L5/00Preparation or treatment of foods or foodstuffs, in general; Food or foodstuffs obtained thereby; Materials therefor
    • A23L5/40Colouring or decolouring of foods
    • A23L5/42Addition of dyes or pigments, e.g. in combination with optical brighteners
    • A23L5/43Addition of dyes or pigments, e.g. in combination with optical brighteners using naturally occurring organic dyes or pigments, their artificial duplicates or their derivatives
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09BORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
    • C09B67/00Influencing 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
    • C09B67/0096Purification; Precipitation; Filtration

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Health & Medical Sciences (AREA)
  • Nutrition Science (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Food Science & Technology (AREA)
  • Polymers & Plastics (AREA)
  • Coloring Foods And Improving Nutritive Qualities (AREA)

Abstract

The invention relates to the technical field of pigment preparation, in particular to a preparation method of acid-stable butterfly bean flower blue pigment, and dried butterfly bean flowers are picked up for standby after impurity removal. Mixing the material with water at 40-45deg.C, and stirring to extract the anthocyanidin of semen Pisi Sativi for 2 times each for 2-3 hr. Centrifuging, mixing the extractive solutions, concentrating under reduced pressure to obtain extract, and lyophilizing to obtain product A. Mixing the product A with sodium bisulphite, manganese dioxide, boric acid and water according to a certain proportion, and stirring and reacting for 3 hours at 85-90 ℃. Cooling to room temperature after the reaction is finished, regulating the PH to be neutral, standing, filtering, concentrating the filtrate under reduced pressure, and freeze-drying to obtain the product. The product is black to deep blue solid, the solubility in neutral water at room temperature is more than 10g/100ml, the product is prepared into 500ppm aqueous solution, and the color development effect under different PH conditions is as follows: the pH is below 2.5 and is purple, the pH is 2.8-10.0 and is blue, the operation is simple, safe and reliable, and the sphenoides blue pigment can be better obtained.

Description

Preparation method of acid-stable butterfly bean flower blue pigment
Technical Field
The invention relates to the technical field of pigment preparation, in particular to a preparation method of acid-stable butterfly bean flower blue pigment.
Background
Butterfly bean flower is also called blue butterfly, english name: the butterfly pea is called butterfly bean flower, blue butterfly, butterfly blue flower, butterfly bean, bean green, etc. The main distribution is thailand Chiang Mai, which is a typical tropical vine plant and is widely distributed throughout the year, and the Yunnan Xishuangbanna is also distributed in a small amount. The petals can be used for dyeing and eating. Has rich vitamins A, C and E, is rich in anthocyanin, can improve immunity, helps and promotes skin elasticity and collagen generation, and has antioxidant effect. The Tai and Xishuangbanna Dai nationality can use the tea as a blue food. The pigment extracted from the pteris crassifolia has wide application prospect in the food industry;
Therefore, the preparation method of the acid-stable sphenoid blue pigment is simple and convenient to operate, safe and reliable, and the sphenoid blue pigment can be better obtained, and the obtained sphenoid blue pigment has better blue color effect under the acidic condition of lower pH. The application range of the butterfly bean flower blue pigment is widened.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention provides a preparation method of acid-stable butterfly bean flower blue pigment.
In order to solve the technical problems, the invention provides the following technical scheme: a preparation method of acid-stable butterfly bean flower blue pigment comprises the following steps:
s1, picking and impurity-removing dried butterfly bean flowers for later use;
S2, mixing the butterfly bean flower raw material with water at 40-45 ℃ according to the butterfly bean flower: water = 1:6 (m/m), and extracting the pterocarpus vulgaris anthocyanidin by stirring for 2 times, each time for 2-3h. Centrifugally filtering, combining the two extracting solutions, concentrating under reduced pressure to obtain an extract, and freeze-drying to obtain a product A;
S3, mixing the product A with sodium bisulphite, manganese dioxide, boric acid and water according to a certain proportion, and stirring and reacting for 3 hours at 85-90 ℃. After the reaction was completed, the reaction mixture was cooled to room temperature, and the pH was adjusted to neutral. Standing, filtering, concentrating the filtrate under reduced pressure, and lyophilizing to obtain the final product.
Preferably, the extraction process of the product A is that the raw material of the butterfly bean flowers and water are mixed according to the butterfly bean flowers: water = 1: mixing and extracting the pteroceltis tatarinowii anthocyanin at the temperature of 40-45 ℃ for 2-3 h at the speed of 6 m/m;
Preferably, the reaction ratio (m/m) of the product A to sodium bisulphite, manganese dioxide, boric acid and water is the product A: sodium bisulfite: manganese dioxide: boric acid: water = 10: (3.0-6.0): (0.5-1.0): (1.0-6.0): 200, the reaction temperature is 85-90 ℃, and the reaction time is 3 hours;
Preferably, the reduced pressure concentration temperature is 45-50 ℃, the concentrated extract is obtained by concentrating, and the product is obtained by freeze drying.
Compared with the prior art, the invention has the following beneficial effects:
1. the plant blue pigment extracted from the butterfly bean flower is subjected to sulfonation treatment, so that the acid-stable blue pigment is obtained, the application range of the butterfly bean flower is expanded, and the comprehensive economic value of the butterfly bean flower is improved.
2. Through the sulfonation method, the spherulla flower blue pigment can be better in blue color under the acidic condition of a lower pH value, and an acidic blue pigment source is provided. Meanwhile, the method is simple and convenient to operate, safe and reliable, and low in use cost, and has the advantage of cost in small laboratory test preparation or large-scale factory production.
Drawings
FIG. 1 is a schematic representation of the color contrast of pigments at different pH in the present invention.
Detailed Description
In order that the manner in which the above recited features, objects and advantages of the present invention are obtained will become readily apparent, a more particular description of the invention will be rendered by reference to specific embodiments thereof which are illustrated in the appended drawings. Based on the examples in the embodiments, those skilled in the art can obtain other examples without making any inventive effort, which fall within the scope of the invention. The experimental methods in the following examples are conventional methods unless otherwise specified, and materials, reagents, etc. used in the following examples are commercially available unless otherwise specified.
Example 1:
in this example, the extraction of the blue pigment from the butterfly bean flower is directly carried out on the butterfly bean flower raw material.
And (5) selecting the dried butterfly bean flower raw materials, removing impurities and then reserving. Weighing 200g of the butterfly bean flower raw material, adding the butterfly bean flower raw material into 1200ml of water, stirring and extracting for 2 hours, centrifuging and filtering, and reserving the liquid; the solid was added to 1200ml of water and extracted for 2h with stirring, and the liquid was left for use. Mixing the 2 times of extracting solutions, concentrating under reduced pressure to obtain extract, and freeze-drying to obtain the product A of the sphenoids blue pigment.
Example 2:
The example is a butterfly bean flower blue pigment product A and sodium bisulphite, manganese dioxide, boric acid and water according to a weight ratio of 10:5:1:1:200, and preparing an acid-stable spherulitic blue pigment.
10.0G of the pteridopsis variabilis blue pigment product A, 5.0g of sodium bisulphite, 1.0g of manganese dioxide and 1.0g of boric acid are weighed and added into 200ml of water, and stirred until the mixture is completely dissolved. Heating to 85-90 ℃, and reacting for 3h with heat preservation. After the reaction was completed, the temperature was lowered to room temperature, the pH of the reaction solution was adjusted to neutrality with 3.5% sodium hydroxide solution, and the reaction solution was allowed to stand for 30min and was centrifugally filtered. Concentrating the filtrate under reduced pressure at 45-50deg.C, and lyophilizing to obtain the final product.
Example 3:
The example is a butterfly bean flower blue pigment product A and sodium bisulphite, manganese dioxide, boric acid and water according to a weight ratio of 10:3:0.5:3:200, and preparing an acid-stable spherulitic blue pigment.
10.0G of the pteridopsis variabilis blue pigment product A, 3.0g of sodium bisulphite, 0.5g of manganese dioxide and 3.0g of boric acid are weighed and added into 200ml of water, and stirred until the mixture is completely dissolved. Heating to 85-90 ℃, and reacting for 3h with heat preservation. After the reaction was completed, the temperature was lowered to room temperature, the pH of the reaction solution was adjusted to neutrality with 3.5% sodium hydroxide solution, and the reaction solution was allowed to stand for 30min and was centrifugally filtered. Concentrating the filtrate under reduced pressure at 45-50deg.C, and lyophilizing to obtain the final product.
Example 4:
the example is a butterfly bean flower blue pigment product A and sodium bisulphite, manganese dioxide, boric acid and water according to a weight ratio of 10:3:0.5:6:200, and preparing an acid-stable spherulitic blue pigment.
10.0G of the pteridopsis variabilis blue pigment product A, 3.0g of sodium bisulphite, 0.5g of manganese dioxide and 6.0g of boric acid are weighed and added into 200ml of water, and stirred until the mixture is completely dissolved. Heating to 85-90 ℃, and reacting for 3h with heat preservation. After the reaction was completed, the temperature was lowered to room temperature, the pH of the reaction solution was adjusted to neutrality with 3.5% sodium hydroxide solution, and the reaction solution was allowed to stand for 30min and was centrifugally filtered. Concentrating the filtrate under reduced pressure at 45-50deg.C, and lyophilizing to obtain the final product.
The color contrast (0.05% diluted hydrochloric acid adjustment) of the spherulitic blue pigment obtained in example 1-example 4 at different pH is shown in figure 1 of the specification.
Comparative examples 1 to 4, the use of the bluish-pea pigments obtained by the methods described in examples 2 to 4 were all blue (series) at pH2.8 to 10.0, whereas the direct extraction of the obtained bluish-pea pigments was green at pH9.0 to 10.0, blue at pH8.0 to 5.5, blue-violet at pH5.0 to 4.5, violet below pH4.0
The present invention may be better implemented as described above, and the above examples are merely illustrative of preferred embodiments of the present invention and not intended to limit the scope of the present invention, and various changes and modifications made by those skilled in the art to the technical solution of the present invention should fall within the scope of protection defined by the present invention without departing from the spirit of the design of the present invention.

Claims (10)

1. The preparation method of the acid-stable butterfly bean flower blue pigment is characterized by comprising the following steps of:
s1: picking and removing impurities from the dried butterfly bean flowers for later use;
s2: mixing the butterfly bean flower raw material with water, filtering, concentrating to obtain an extract, and freeze-drying to obtain a product A;
S3: mixing the product A with sodium bisulphite, manganese dioxide, boric acid and water according to a certain proportion, stirring, standing, filtering, concentrating the filtrate under reduced pressure, and freeze-drying to obtain the product.
2. The method for preparing acid-stable sphenoid blue pigment according to claim 1, wherein the mixing of the sphenoid raw material in S2 with water is performed at 40-45 ℃.
3. The method for preparing the acid-stable pteridophyte blue pigment according to claim 2, wherein the pteridophyte raw material and water in S2 are prepared according to the following pteridophyte: water = 1:6 m/m.
4. The method for preparing acid-stable pteroceltis peas flower blue pigment according to claim 3, wherein the pteroceltis peas flower raw material in step S2 is mixed with water and stirred to extract the pteroceltis peas flower pigment 2 times, each time for 2-3 hours.
5. The method for preparing acid-stable pteroceltin according to claim 4, wherein the stirring and extracting of the pteroceltin in step S2 is followed by centrifugal filtration, combining the two extracts, and concentrating under reduced pressure to obtain an extract.
6. The method for preparing acid-stable pteroceltis falcatum pigment according to claim 5, wherein in the step S3, the product A is mixed with sodium bisulphite, manganese dioxide, boric acid and water according to a certain proportion, and then stirred and reacted for 3 hours at 85-90 ℃.
7. The method for preparing acid-stable pteridophyte blue pigment according to claim 6, wherein the product A in S3 is mixed with sodium bisulphite, manganese dioxide, boric acid and water according to a certain proportion, and then stirred at 85-90 ℃ for reaction for 3 hours, and then cooled to room temperature.
8. The method for preparing acid-stable pteroceltin according to claim 7, wherein the mixture of product A and sodium bisulphite, manganese dioxide, boric acid and water in S3 is cooled to room temperature and then the pH is adjusted to neutral.
9. The method for preparing the acid-stable pteroceltis faerie flower blue pigment according to claim 8, wherein the mixing ratio of the product A to sodium bisulphite, manganese dioxide, boric acid and water in the step S3 is the product A: sodium bisulfite: manganese dioxide: boric acid: water = 10: (3.0-6.0): (0.5-1.0): (1.0-6.0): 200m/m, and the reaction temperature is 85-90 ℃.
10. The method for preparing the acid-stable pteroceltis falcata flower blue pigment according to claim 9, wherein the color development effect of the pteroceltis falcata flower pigment under different pH conditions is as follows: the pH is below 2.5 and the pH is 2.8-10.0 and the pH is blue, the centrifugation condition is 5000r/min, the time is 20min, and the pH adjusting step is 3.5% m/m sodium hydroxide.
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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102432580A (en) * 2011-12-23 2012-05-02 晨光生物科技集团股份有限公司 Method for degrading high polymer proanthocyanidin
CN109400569A (en) * 2018-10-18 2019-03-01 赣州华汉生物科技有限公司 A kind of method of extraction purification anthocyanidin in butterfly Tofu pudding

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Publication number Priority date Publication date Assignee Title
JPH03223298A (en) * 1990-01-26 1991-10-02 Ajinomoto Co Inc Delphinidin 3,3',5'-triglucoside compound
JP2003292810A (en) * 2002-03-29 2003-10-15 Toyo Ink Mfg Co Ltd Coloring matter composition
WO2010115073A2 (en) * 2009-04-03 2010-10-07 Richard Rice Natural blue flavorants and colorants
AU2013301615B2 (en) * 2012-08-09 2017-02-02 Nestec S.A. Anthocyanin colouring composition
CN111533723B (en) * 2020-05-29 2024-04-30 河南龙亭药业有限公司 Method for extracting anthocyanin from mature fresh fruit of black fungus
CN112521770A (en) * 2020-12-15 2021-03-19 上海应用技术大学 Preparation method and application of oroxylum indicum pigment extract
CN114208998A (en) * 2021-12-23 2022-03-22 江西丹霞生物科技股份有限公司 Process for extracting anthocyanin from clitocybe maxima
CN115414404A (en) * 2022-09-21 2022-12-02 广西壮族自治区亚热带作物研究所(广西亚热带农产品加工研究所) Extraction method of Clitoria ternatea flower

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102432580A (en) * 2011-12-23 2012-05-02 晨光生物科技集团股份有限公司 Method for degrading high polymer proanthocyanidin
CN109400569A (en) * 2018-10-18 2019-03-01 赣州华汉生物科技有限公司 A kind of method of extraction purification anthocyanidin in butterfly Tofu pudding

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