CN110305496B - High-stability cassia seed pigment extraction method - Google Patents
High-stability cassia seed pigment extraction method Download PDFInfo
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- CN110305496B CN110305496B CN201910646642.1A CN201910646642A CN110305496B CN 110305496 B CN110305496 B CN 110305496B CN 201910646642 A CN201910646642 A CN 201910646642A CN 110305496 B CN110305496 B CN 110305496B
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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
- 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
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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
- 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
- C09B67/0001—Post-treatment of organic pigments or dyes
- C09B67/0017—Influencing the physical properties by treatment with an acid, H2SO4
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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
- 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)
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- Chemical Kinetics & Catalysis (AREA)
- Cosmetics (AREA)
Abstract
The invention discloses a method for extracting a high-stability cassia seed pigment, which is characterized by taking an ethanol solution with the mass concentration of 30-70% as an extraction solvent, adding an amino acid protective agent after ultrasonic-assisted extraction for a certain time, continuing ultrasonic-assisted extraction, standing, taking a supernatant to obtain a high-concentration pigment extracting solution, adjusting the pH value to 3-6 with an organic acid, adding cyclodextrin, uniformly mixing, then adding vitamin E and vitamin C, uniformly mixing, and performing spray drying to obtain pigment powder. The stability test of the obtained pigment powder proves that the light resistance, the high temperature resistance, the oxidation resistance and the reduction resistance of the pigment powder are all obviously improved.
Description
Technical Field
The invention relates to the field of natural pigment extraction, and more particularly relates to a method for extracting a high-stability cassia seed pigment.
Background
It is known that pigments play an important role in the food processing step and the like, and that pigments are classified into synthetic pigments and natural pigments, and although synthetic pigments have advantages such as low production cost and easy availability as compared with natural pigments, synthetic pigments contain many chemical substances harmful to the human body, and the addition of synthetic pigments to foods easily causes various diseases such as canceration and deformity. With the improvement of living standard of people, the food safety awareness of people is gradually enhanced, green and healthy food is favored by more and more people, and thus, a plurality of merchants and researchers begin to concentrate on the development and utilization of natural pigments.
The natural pigments are edible pigments derived from roots, stems, leaves, flowers, fruits of natural plants, animals, microorganisms, and the like, and phytochromes are frequently used. The natural pigment has various varieties and no toxic or side effect, and is widely used for coloring foods such as beverages, candies, cakes, wines and the like, medical health care products and cosmetics.
Some of the curcumin also has pharmacological effects and nutritional values, for example, tea pigment not only has good coloring effect, but also has the effects of resisting oxidation, regulating blood sugar and blood fat and the like, and curcumin has the effects of good coloring strength, resisting inflammation, resisting tumor, preventing and treating senile plaque and the like, is the mainstream of pigment industry consumption and is developed very rapidly.
Semen Cassiae is mature and dry seed of Cassia tora or Cassia tora L, which is rich in carbohydrate, amino acids and vitamins, and contains many medicinal ingredients. As early as in the medical books of compendium of materia Medica, Ben Jing, Ben Cao and Ben Cao Jing Shu, there are many records about semen Cassiae, which is sweet, bitter, salty and slightly cold in nature, and has the functions of lowering blood pressure and blood fat, relaxing bowel, clearing liver and improving eyesight. The semen Cassiae is fried to be cooked and cooled or directly decocted with water for oral administration, and has health promotion effect. Modern medical scientists have conducted a great deal of research on the effective components of cassia seed, and found that the effective components of the cassia seed, such as emodin, anthraquinone compounds, cassia seed elements, trace metal elements and the like, play an important role in treating diseases of human bodies. The cassia seed not only contains rich medicinal components, but also contains a large amount of pigment, so that the utilization of the cassia seed to extract the pigment provides a feasible path for the development of natural pigment.
At present, the research and development of the natural pigment in China mainly aims at searching more natural plants which can be used as pigment extraction raw materials and exploring an extraction and refining method matched with each natural pigment. However, the natural pigment has the defects of poor stability, weak coloring and the like, so that the application of the natural pigment in China is restricted.
The ethanol dipping method is a common method for extracting natural pigment, has the defects of needing to recover a large amount of organic solvent, having low separation efficiency, having certain influence on products by the solvent, having the advantages of strong dissolving capacity on the pigment, stable chemical property, small corrosion to equipment, solvent and water immiscible, simple separation method process principle and convenient operation, and being capable of meeting the requirements of large-scale industrial production.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provide the method for extracting the pigment of the cassia seed with high stability.
In order to achieve the purpose, the technical scheme of the invention is as follows:
the method for extracting the pigment of the cassia seeds is characterized by comprising the following steps:
step S1: pulverizing semen Cassiae to obtain semen Cassiae powder;
step S2: soaking the cassia seed powder by using an ethanol solution with the mass concentration of 30-70% as an extraction solvent, and performing ultrasonic-assisted extraction in a constant-temperature water bath at 50-70 ℃ for a certain time; the 'cavitation' action of ultrasonic waves is utilized to break organic macromolecular chains into small molecules, so that the extraction time can be shortened, the 'cavitation' action can continuously break pigment macromolecules into smaller molecules after the ultrasonic time is too long, the pigment is degraded, and the pigment extraction rate is reduced.
Step S3: adding amino acid, continuing ultrasonic-assisted extraction for a certain time, standing, and taking supernatant; the amino acid is added to protect the extracted pigment molecules, the ultrasonic stirring is carried out to fully disperse the amino acid, and the dispersed amino acid and the pigment molecules are combined into a supermolecule compound through Van der Waals acting force, so that the extracted pigment is prevented from being degraded, meanwhile, the unextracted pigment is continuously leached out, and the extraction rate of the pigment is improved. Excess amino acids and other proteins, fatty acids are removed by sedimentation. The supernatant is a uniform mixture of amino acids and pigment, and the amino acids increase the molecular weight of the pigment, improve the stability of the pigment, and improve the heat resistance and light resistance of the pigment. Preferably, the amino acid is an alpha-amino acid, and specifically, can be one or two of glutamic acid and aspartic acid.
Step S4: removing the excess ethanol extraction solvent in the supernatant by rotary evaporation; the excess ethanol may affect the stability of the pigment. The temperature of rotary evaporation is 60-80 ℃.
Step S5: adding organic acid, uniformly mixing, adjusting the pH value to 3-6, and preferably carrying out ultrasonic stirring; the organic acid contains free hydrogen ions, can protect hydroxyl in the pigment, and has the effects of improving pigment stability and acid and alkali resistance of the pigment. Preferably, the organic acid is one or more of benzoic acid, salicylic acid, tartaric acid, oxalic acid, malic acid and citric acid, and the organic acid is edible, so that the green environmental protection property of the pigment is improved.
Step S6: adding cyclodextrin, mixing, preferably, ultrasonic stirring; the cyclodextrin has hydrophobic property in the ring and hydrophilic property outside the ring, the pigment and amino acid are contained in the inner cavity, and the cyclodextrin has the embedding protection effect, so that the heat resistance, light resistance, acid resistance, alkali resistance and oxidation resistance of the pigment are further improved, and the hydrophilicity of the pigment can also be improved.
Step S7: adding vitamin C and vitamin E, mixing, preferably ultrasonic mixing, wherein the vitamin C is hydrophilic and the vitamin E is hydrophobic, and after mixing, the vitamin C is distributed outside the cyclodextrin and the vitamin E is distributed in the inner cavity of the cyclodextrin, thereby completely improving the oxidation resistance of the pigment.
Step S8: spray drying to obtain pigment powder.
According to the technical scheme, on the basis of ethanol immersion extraction, ultrasonic extraction is assisted, edible amino acid is added as a protective agent and a stabilizing agent in the extraction process to improve the stability of the pigment and the extraction rate of the pigment, an acid-base regulator of organic acid is added to enable the pH value of the pigment of the cassia seed to be in the most stable range of the pigment, an embedding agent of cyclodextrin is added to improve the stability of the pigment and the hydrophilicity of the pigment and widen the application range of the pigment, and the antioxidant of hydrophilic VC and hydrophobic VE is added to a solution after the cyclodextrin is added to enable the cyclodextrin to be uniformly distributed in vitro and in cavity, so that the antioxidant performance of the pigment is improved. On the whole, the method has the advantages of simple process, no violent reactions such as high temperature and high pressure, no introduction of toxic reagents, improvement of the pigment extraction rate of the cassia seeds, great improvement of the light resistance, heat resistance, acid and alkali resistance, reduction resistance and oxidation resistance of the cassia seeds, and hydrophilic property, and has a large-scale industrial application prospect.
Drawings
FIG. 1 is a graph of the relationship between ethanol concentration and absorbance with other factors unchanged;
FIG. 2 is a graph of the relationship between the mass of cassia seed and the volume ratio of 50% ethanol (i.e. feed-liquid ratio) and the absorbance when other factors are unchanged;
FIG. 3 is a graph of temperature versus absorbance for other factors;
FIG. 4 is a graph of extraction time versus absorbance for other factors;
FIG. 5 is a graph showing the relationship between the extraction time and the absorbance when other factors are not changed, and amino acids are added when the extraction time is 20 min;
FIG. 6 is a graph of time versus absorbance for a light experiment;
FIG. 7 is a graph showing the relationship between temperature and absorbance in a high temperature test;
FIG. 8 is a graph showing the relationship between time and absorbance in a light irradiation experiment of a pigment extract solution having improved stability;
FIG. 9 is a graph showing the relationship between temperature and absorbance in a high-temperature test of a pigment extract solution having improved stability.
Detailed Description
The following describes embodiments of the present invention in further detail with reference to the accompanying drawings.
The invention discloses a method for extracting pigment of cassia seed, which comprises the following steps:
1. pretreatment of cassia seed sample
Pulverizing purchased semen Cassiae with high-speed universal pulverizer, collecting pulverized semen Cassiae powder, and placing in dark dry place for use.
2. Extraction of pigments
Taking an ethanol solution as an extracting agent, carrying out ultrasonic-assisted extraction for a certain time, setting an extraction temperature, standing, taking supernatant of an upper layer, and carrying out centrifugal treatment to obtain a high-concentration pigment extracting solution.
Ultrasonic-assisted extraction is a new extraction technology in recent years, and the strong cavitation effect, mechanical vibration, high acceleration, emulsification, diffusion, crushing and stirring effects generated by ultrasonic waves are utilized to increase the molecular motion frequency and speed of a substance and increase the penetrating power of a solvent.
In order to optimize the ultrasound-assisted extraction time, the extraction temperature, and the amount and concentration of the ethanol extract, the present invention separately performed the following experiments,
1) optimization of ethanol concentration parameters
Accurately weighing 5 parts of 1.0g of cassia seed powder into a conical flask, respectively adding 30mL of 30%, 40%, 50%, 60% and 70% ethanol solution, and numbering for later use. And placing the five conical flasks into an ultrasonic cleaning machine, performing ultrasonic extraction at 60 ℃ for 30min, putting the supernatant of 10mL of the pigment extracting solution into a low-speed centrifuge, setting the rotating speed to be 4000r/min, centrifuging for ten minutes, taking the supernatant, diluting, and respectively measuring the maximum absorbance of each pigment extracting solution. Triplicate determinations were averaged.
The relation curve of ethanol concentration and absorbance is shown in fig. 1, and it can be seen that when the ethanol concentration is 50%, the absorbance value of the cassia seed pigment is the maximum, i.e. the pigment extraction rate is the highest. The extraction rate of the pigment tends to decrease with the increase of the ethanol concentration, and may be caused by the deterioration of the stability of the pigment due to the excessive ethanol concentration. The mass concentration of the ethanol is preferably in the range of 40-60%.
2) Optimization of material-liquid ratio parameters
Accurately weighing 5 parts of 1.0g of cassia seed powder into a conical flask, respectively adding 10mL, 20mL, 30mL, 40mL and 50mL of 50% ethanol solution, and numbering for later use. And placing the five conical flasks into an ultrasonic cleaning machine, performing ultrasonic extraction at 60 ℃ for 30min, putting the supernatant of 10mL of the pigment extracting solution into a low-speed centrifuge, setting the rotating speed to be 4000r/min, centrifuging for ten minutes, taking the supernatant, diluting, and respectively measuring the maximum absorbance of each pigment extracting solution. Triplicate determinations were averaged.
The relationship between the mass of semen Cassiae and the volume ratio of 50% ethanol (i.e. the ratio of material to liquid) and the absorbance is shown in FIG. 2. it can be seen that the absorbance value gradually decreases with the increase of the ratio of material to liquid, and the decrease of the absorbance value may be caused by the concentration of pigment in the extract.
3) Influence of temperature on extraction rate of pigment from semen Cassiae
Accurately weighing 5 parts of 1.0g of cassia seed powder into a conical flask, and respectively adding 30mL of 50% ethanol solution for numbering for later use. And performing ultrasonic extraction on the five conical flasks at 40 ℃, 50 ℃, 60 ℃, 70 ℃ and 80 ℃ for 30min, respectively, putting the supernatant of 10mL of the pigment extracting solution into a low-speed centrifuge, setting the rotating speed to 4000r/min, centrifuging for ten minutes, taking the supernatant, diluting, and respectively measuring the maximum absorbance of each pigment extracting solution. Triplicate determinations were averaged.
The relationship curve between temperature and absorbance is shown in fig. 3, and it can be seen that the absorbance value of the pigment of cassia seed is the maximum when the extraction temperature is 60 ℃, i.e. the extraction rate of the pigment is the highest. When the temperature exceeds 60 ℃, the extraction rate of the pigment gradually decreases with the increase of the extraction temperature, probably because the pigment is easily decomposed by high temperature. The preferred range of extraction temperature is 50 ℃ to 70 ℃.
4) Influence of extraction time on extraction rate of pigment from semen Cassiae
Accurately weighing 5 parts of 1.0g of cassia seed powder into a conical flask, and respectively adding 30mL of 50% ethanol solution for numbering for later use. Placing five conical flasks in an ultrasonic cleaning machine, setting the extraction temperature at 60 ℃, extracting for 10min, 20min, 30min, 40min and 50min respectively, placing the supernatant of 10mL of pigment extracting solution in a centrifuge at the set rotation speed of 4000r/min, centrifuging for ten minutes, taking each pigment extracting supernatant, diluting, and measuring the maximum absorbance of the extracting solution respectively. Triplicate determinations were averaged.
FIG. 4 shows the relationship between the extraction time and the absorbance, and it can be seen that the absorbance value of the pigment of semen Cassiae is 0.609Abs at the maximum when the extraction time is 20min, and the extraction rate of the pigment is the highest. Within 20min, the extraction time is increased, the pigment extraction rate is gradually increased, and after 20min, the pigment extraction rate is in a remarkable reduction trend. The longer the extraction time is, the better the pigment extraction effect is, and the longer the extraction time is, other impurities are easily generated, which affects the pigment extraction effect. The preferable extraction time is 10-30 min.
The invention designs a response surface experiment by Design-Expert software and by using a Box-Behnken center combination Design principle. On the basis of the single-factor experiment result, 4 factors of extraction time, extraction temperature, feed-liquid ratio and extraction concentration are selected as variables, and the experiment is designed by taking the absorbance of the pigment of the cassia seed as a response value. The experimental factors and level codes are shown in table 1. The analysis of the experimental results shows that: the influence on the extraction of the cassia seed pigment is sequentially as follows: extraction time > extraction temperature > extraction concentration > material-to-liquid ratio.
TABLE 1 response surface experiment factors and horizontal coding tables
Therefore, the extraction rate of the pigment is seriously affected by the excessively long ultrasonic extraction time, and it is inferred that the structure of the pigment is destroyed by the ultrasonic action. For the purpose of protecting the pigment, the protective agent is added after the ultrasonic treatment is carried out for a certain time, and then the ultrasonic extraction is continued, so that the extracted pigment is protected, and the extraction rate is further improved.
The stability of the extracted simple pigment extract of cassia seed without being protected by the protective agent and the stabilizing agent is respectively studied as follows:
1) illumination experiment
Placing the pigment extractive solution into three conical flasks, respectively placing in a show window under sunlight, indoors and in a dark place, and measuring absorbance of the pigment extractive solution of semen Cassiae at wavelength of 278nm every 2 hr with 50% ethanol as reference solution. Each group was measured three times. Referring to fig. 6, it can be seen that the pigment extraction rate is significantly reduced under the illumination condition, and the illumination resistance is poor.
2) High temperature test
Placing the four pigment extractive solution conical bottles into a constant temperature water bath kettle at 60 deg.C, 70 deg.C, 80 deg.C and 90 deg.C, respectively. Taking 50% ethanol as reference solution, keeping the temperature for 3h, and measuring the absorbance of the pigment extract of semen Cassiae at wavelength of 278nm, three times for each group. Referring to fig. 7, it can be seen that the cassia pigment has poor high temperature resistance.
3) Determination of Oxidation resistance
Preparing 0.1mol/L hydrogen peroxide and potassium permanganate solution, taking 2 parts of 15mL diluted cassia seed pigment extracting solution, putting the cassia seed pigment extracting solution into a 50mL conical flask, respectively adding the hydrogen peroxide solution and the potassium permanganate solution with the same volume, shaking up, standing for 20min, and measuring the absorbance value of the cassia seed pigment extracting solution at 278 nm. Each group was measured three times. The results are shown in Table 2. As shown in Table 2, the oxidants such as hydrogen peroxide and potassium permanganate can significantly reduce the absorbance of the pigment extract of semen Cassiae, significantly reduce the extraction rate of the pigment, and thus the oxidation resistance of the pigment of semen Cassiae is poor.
Table 2: experiment on Oxidation resistance
4) And (4) measuring the reduction resistance.
Preparing 0.1mol/L ascorbic acid solution and sodium sulfite solution, taking 2 parts of 15mL diluted cassia seed pigment extracting solution, putting the cassia seed pigment extracting solution into a 50mL conical flask, respectively adding the ascorbic acid solution and the sodium sulfite solution with the same volume, shaking up, standing for 20min, and measuring the absorbance value at 278 nm. Each group was measured three times. The measurement results are shown in table 3, and it can be seen that antioxidants such as ascorbic acid and sodium sulfite can significantly reduce the absorbance of the pigment extract of cassia seed, significantly reduce the extraction rate of the pigment, and show that the pigment of cassia seed has poor anti-reduction property.
TABLE 3 reduction resistance test
The invention improves the extraction process of the cassia seed pigment from the aspect of improving the stability of the cassia seed pigment.
Because the main components of the cassia seed pigment are emodin and anthraquinone compounds, the stability, high temperature resistance, light resistance and the like of the pigment can be improved by introducing a strong electron-donating group into the anthraquinone pigment or increasing the molecular weight of the pigment. The amino acid is preferably used as a protective agent, the amino acid contains strong electron-donating group amino, the amino acid also contains weak carboxyl electron-donating group, and the anthraquinone compound also contains strong electron-donating group-OH and weak electron-donating group on a biphenyl ring, so that the amino and carboxyl at the head and the tail of the amino acid are respectively connected with the weak electron-donating group and the strong electron-donating group on the anthraquinone compound by utilizing the intermolecular van der Waals force, the amino acid becomes a bridge for connecting pigments, the active group is passivated, the molecular weight of the pigments is increased, and the purposes of protecting the pigments and improving the stability of the pigments are achieved. Preferably, the amino acid is an alpha-amino acid, and preferably is highly polar, such as one or a combination of two of glutamic acid, aspartic acid.
The method improves the steps of ultrasonic extraction, namely, the extraction is carried out in ethanol solution, amino acid is added after ultrasonic-assisted extraction is carried out for a certain time at a certain temperature, and then the ultrasonic-assisted extraction is carried out for a certain time.
Specifically, 5 parts of 1.0g of cassia seed powder are accurately weighed into a conical flask, and 30mL of 50% ethanol solution is respectively added, and the materials are numbered for standby. Placing five conical flasks in an ultrasonic cleaning machine, setting the extraction temperature to be 60 ℃, extracting for 10min, 20min, 30min, 40min and 50min respectively, adding 0.3g of glutamic acid when the extraction time of No. 3, 4 and 5 reagents reaches 20min, placing 10mL of supernatant of pigment extracting solution in a centrifugal machine respectively, setting the rotation speed to be 4000r/min, centrifuging for ten minutes, diluting each pigment extracting supernatant, and measuring the maximum absorbance of the extracting solution respectively. Triplicate determinations were averaged.
The curve of the relationship between the extraction time and the absorbance is shown in FIG. 5, and compared with the result in FIG. 4, the stability of the pigment is obviously improved by adding the amino acid when the extraction time is 20 min.
3. Purification, protection and solidification
The invention then continues to purify, protect and solidify the extracted pigment, extends shelf life, and is used directly as a pigment additive.
And removing the redundant ethanol extraction solvent in the supernatant by rotary evaporation to obtain a high-concentration pigment extracting solution, so that the influence of the ethanol solvent on the pigment is avoided. Specifically, the supernatant after ultrasonic extraction was placed in a rotary evaporator at a temperature of 60 ℃.
And (3) carrying out pH adjustment on the high-concentration pigment extracting solution by using edible organic acid to ensure that the pH value is in a weak acid range of 3-6, and because the pigment is protected in the previous step, ultrasonic-assisted stirring can be used in the step and the later steps to ensure that the mixture is more sufficient, so that a supermolecular structure with amino acid uniformly distributed in the pigment is more easily formed. Specifically, the pH was adjusted to 5 with citric acid.
After the pH value is adjusted, the cyclodextrin aqueous solution is continuously added, preferably, ultrasonic mixing is carried out, the cyclodextrin has hydrophobicity in the ring and hydrophilicity outside the ring, the pigment and the amino acid are contained in the inner cavity, and the cyclodextrin has the embedding protection effect. Specifically, 10mL of an aqueous cyclodextrin solution having a concentration of 0.1g/mL was added.
Adding vitamin C and vitamin E into pigment embedded and protected by cyclodextrin, and preferably ultrasonic mixing to make pigment have antioxidant effect. Specifically, 0.05g of vitamin C and 0.05g of vitamin E were added, respectively.
Spray drying to obtain pigment powder.
4. Stability test of the protected pigment extract
1) Illumination experiment
Numbering three ground conical flasks with plugs, and adding 15mL of 0.1mg/mL cassia seed pigment extract diluted with 50% ethanol solvent. Three conical bottles are respectively placed in a show window which is in the sun, indoors and out of the sun. And (3) taking 50% ethanol as a reference solution, and measuring the maximum absorbance of the pigment extracting solution of the cassia seeds every 2 hours. Three measurements were taken for each group and averaged. Referring to fig. 8, it can be seen that the light fastness of the cassia pigment with improved stability is improved as compared with fig. 6.
2) High temperature test
Numbering four ground conical flasks with plugs, and adding 15mL of 0.1mg/mL cassia seed pigment extract diluted with 50% ethanol solvent. The four conical flasks are respectively placed in a constant-temperature water bath kettle at 60 ℃, 70 ℃, 80 ℃ and 90 ℃. Taking 50% ethanol as reference solution, keeping the temperature for 3h, measuring the maximum absorbance of the pigment extract of semen Cassiae, and taking the average value for three times per group. As shown in fig. 9, it can be seen that the high temperature resistance of the cassia pigment with improved stability is improved as compared with fig. 7.
3) Determination of Oxidation resistance
Preparing 0.1mol/L hydrogen peroxide and potassium permanganate solution, taking 2 parts of 0.1mg/mL cassia seed pigment extracting solution diluted by 15mL of 50% ethanol solvent, putting the 0.1mg/mL cassia seed pigment extracting solution into a 50mL conical flask, respectively adding the hydrogen peroxide solution and the potassium permanganate solution with the same volume, shaking up, standing for 20min, and measuring the absorbance value of the solution at 278 nm. Each group was measured three times. The results are shown in Table 4. The antioxidant properties of the pigment from cassia seed are improved compared to table 2.
Table 4: experiment on Oxidation resistance
4) And (4) measuring the reduction resistance.
Preparing 0.1mol/L ascorbic acid solution and sodium sulfite solution, taking 2 parts of 0.1mg/mL cassia seed pigment extracting solution diluted by 15mL of 50% ethanol solvent, putting the 0.1mg/mL cassia seed pigment extracting solution into a 50mL conical flask, respectively adding the same volume of ascorbic acid solution and sodium sulfite solution, shaking up, standing for 20min, and measuring the absorbance value at 278 nm. Each group was measured three times. The results are shown in Table 5, and it can be seen that the reduction resistance of the pigment of cassia seed is improved as compared with Table 3.
TABLE 5 reduction resistance test
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (6)
1. The method for extracting the pigment of the cassia seeds with high stability is characterized by comprising the following steps:
step S1: pulverizing semen Cassiae to obtain semen Cassiae powder;
step S2: soaking the cassia seed powder by using an ethanol solution with the mass concentration of 30-70% as an extraction solvent, and performing ultrasonic-assisted extraction in a constant-temperature water bath at 50-70 ℃ for a certain time;
step S3: adding one or two of glutamic acid and aspartic acid, continuing ultrasonic-assisted extraction for a certain time, standing, and taking supernatant;
step S4: removing excessive ethanol extraction solvent in the supernatant by rotary evaporation to obtain high-concentration pigment extract;
step S5: adding organic acid, mixing uniformly, and adjusting the pH value to 3-6;
step S6: adding cyclodextrin and mixing;
step S7: adding vitamin E and vitamin C, and mixing;
step S8: spray drying to obtain pigment powder.
2. The method according to claim 1, wherein in step S4, the temperature of rotary evaporation is 60-80 ℃.
3. The method according to claim 1, wherein in step S5, the organic acid is one or more of benzoic acid, salicylic acid, tartaric acid, oxalic acid, malic acid, and citric acid.
4. The method according to claim 1, wherein in the step S2, the volume ratio of the mass of the cassia seed powder to the ethanol solution with the mass concentration of 50% is 1: 30-50 g/mL.
5. The method according to claim 1, wherein in the step S3, the glutamic acid and the aspartic acid are added in a total amount of 10-30% by mass based on the mass of the powder of the cassia seed in the step S2.
6. The method according to claim 1, wherein the temperature of the thermostatic water bath is 60 ℃ and the mass concentration of the ethanol solution is 50%.
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Denomination of invention: A High Stability Extraction Method for Cassia Seed Pigment Granted publication date: 20210212 Pledgee: Xingshan County Sub branch of Agricultural Bank of China Co.,Ltd. Pledgor: Hubei kaloer New Material Technology Co.,Ltd. Registration number: Y2024980004544 |