CN118542893B - Preparation process of hypoallergenic lotus flower powder extract - Google Patents
Preparation process of hypoallergenic lotus flower powder extractInfo
- Publication number
- CN118542893B CN118542893B CN202411021855.2A CN202411021855A CN118542893B CN 118542893 B CN118542893 B CN 118542893B CN 202411021855 A CN202411021855 A CN 202411021855A CN 118542893 B CN118542893 B CN 118542893B
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- lotus powder
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Abstract
The invention belongs to the field of pollen extract preparation processes, and particularly relates to a preparation process of a hypoallergenic lotus powder extract. Soaking fresh lotus pollen in sodium sulfite solution, breaking cell wall under ultrahigh pressure, adding pollen protein modifier, and covalently binding citral with pollen protein under oxidation of methemoglobin; the polymer formed by the reaction of the organic acid, polylactic acid and the hydroformylation protein in the lotus pollen has good biocompatibility, and the sensitization structure of the protein and the organic acid surface in the pollen is modified; cellulose in lotus powder is crosslinked with p-oxybenzaldehyde under the action of mandelic acid, and a compact film structure is formed by cooperating with lac resin to cover the surface of aldehyde group polymer, so that the recognition between antigen and antibody is effectively blocked, and the prepared hypoallergenic lotus powder extract has stable quality, is not influenced by extraction conditions, has hypoallergenicity and can not grow microorganisms after long-term storage.
Description
Technical Field
The invention belongs to the field of pollen extract preparation processes, and particularly relates to a preparation process of a hypoallergenic lotus flower powder extract.
Background
Lotus pollen is an important component in the lotus propagation process, and the lotus pollen is rich in various components including proteins, amino acids, vitamins, minerals, enzymes and the like. The lotus pollen has the advantages that the protein is one of main components of the lotus pollen, the lotus pollen is high in content, and contains rich vitamin B groups, so that the lotus pollen has wide application value in the fields of foods, health products, cosmetics, medicines and the like, can be used for preparing foods and health products with rich nutrition, has the effects of nourishing, building body and improving immunity by taking pollen capsules, pollen particles and the like as nutritional supplements, can also be used for preparing cosmetics such as masks, shampoos and the like, has the effects of nourishing skin and improving skin, and has medicinal value in the medicine field, and is used for treating insomnia and dyspepsia.
Lotus pollen contains allergen substances which have a specific structure for generating an immune response with the immune system of the organism, when the allergen substances are contacted with the immune system of a sensitive individual, the immune system generates specific types of antibodies, called IgE antibodies, which bind to eosinophils and mast cells, and when the lotus pollen is contacted again, the allergic response occurs.
At present, the existing lotus powder extract preparation technology has the following problems: firstly, the chemical components of lotus powder are complex and are easily influenced by the extraction environment, and the extraction efficiency can be influenced by the change of the extraction conditions in the extraction process, so that the quality of the extract is inconsistent; secondly, the extract contains three high sensitization components of protein, cellulose and organic acid, so that the health of organisms is damaged by contact, and the application range of the lotus powder extract is greatly limited; thirdly, the pollen extract needs special preservation conditions in the long-term storage process, so that microorganisms are easy to breed, and the microorganisms can continuously absorb and destroy nutrient substances in the pollen extract.
Disclosure of Invention
Aiming at the situation, the invention provides a preparation process of the hypoallergenic lotus powder extract to overcome the defects of the prior art, and in order to solve the problems that the quality of the existing lotus powder extract is inconsistent due to the extraction condition, the lotus powder extract has high allergenicity and can be stored for a long time and can be easily bred with microorganisms, the invention uses the lotus powder mixture subjected to sodium sulfite treatment to break the wall and then reacts with pollen protein modifier, polylactic acid and film forming agent, the prepared hypoallergenic lotus powder extract has stable quality, the quality of the extract is not influenced by the extraction condition, the lotus powder extract has low allergenicity and can not be bred with microorganisms after being stored for a long time, and the nutrient substances contained in the lotus powder extract can not be damaged.
In order to achieve the above purpose, the invention adopts the following technical scheme that the invention provides a preparation process of a hypoallergenic lotus powder extract, which comprises the following steps:
Weighing 400-500 parts by weight of fresh lotus powder, 30-40 parts by weight of sodium sulfite and 320-360 parts by weight of ultrapure water, putting into a stirring pot with the power of 1.6-1.8 kW for stirring, wherein the stirring temperature is 30-35 ℃, the stirring time is 10-15 min, the stirring rotating speed is 60-80 r/min, and soaking for 2-3 h after uniformly mixing to obtain a lotus powder mixture;
step two, placing the lotus powder mixture prepared in the step one into an ultrahigh pressure wall breaking machine with the power of 11.5-13.5 kW, the pressure of 1.8 MPa, the wall breaking temperature of 70-75 ℃, the wall breaking time of 15-20 min and the wall breaking rotating speed of 30000-40000 r/min, and performing ultrahigh pressure wall breaking to obtain wall broken lotus powder;
Step three, putting the wall-broken lotus pollen prepared in the step two and 100-120 parts by weight of pollen protein modifier into a reaction kettle with the power of 5.5-6.5 kW, the reaction temperature of 40-45 ℃ and the reaction time of 1.2-1.4 h and the reaction rotating speed of 130-150 r/min, and reacting to obtain a pretreated lotus powder solution;
Weighing 60-70 parts by weight of polylactic acid, putting the polylactic acid into the pretreated pollen solution prepared in the third step, reacting at 50-60 ℃ for 2-3 h hours at 120-140 r/min to form an aldehyde polymer solution;
step five, weighing 120-140 parts by weight of film forming agent, putting the film forming agent into the aldehyde group polymer solution prepared in the step four, reacting at 35-45 ℃ for 2-2.5 h and at 110-120 r/min to obtain a treated solution;
step six, placing the treated solution obtained in the step five into a rapid extraction instrument with the power of 1.5-2.2 kW, wherein the rapid extraction temperature is 100-120 ℃, the rapid extraction time is 15-20 min, and performing rapid extraction to obtain hypoallergenic extract solution;
Step seven, the hypoallergenic extract solution prepared in the step six is put into a high-efficiency thickener of 3.5-4.5 kW, the concentration temperature is 40-50 ℃, the concentration time is 1.2-1.5 h, and the hypoallergenic extract concentrated solution is obtained;
And step eight, placing the hypoallergenic extract concentrated solution prepared in the step seven into an ultralow temperature freeze dryer with the power of 1.5-1.8 kW, wherein the low temperature freeze drying temperature is-70 ℃, the freeze drying time is 20-22 h, and heating to 25-28 ℃ after the ultralow temperature drying to obtain the hypoallergenic lotus powder extract.
Preferably, the preparation method of the pollen protein modifier specifically comprises the following steps:
S1, weighing 20-30 parts by weight of citral and 120-140 parts by weight of absolute ethyl alcohol, putting the citral and the absolute ethyl alcohol into a stirring pot with the power of 1.8-2.2 kW, stirring at the temperature of 25-28 ℃ for 8-12 min and the stirring speed of 130-150 r/min, and mixing and dissolving to obtain a citral solution;
s2, weighing 30-40 parts by weight of methemoglobin, 5-8 parts by weight of sodium bicarbonate and 110-120 parts by weight of absolute ethyl alcohol, putting the mixture into a stirring pot with the power of 1.8-2.2 kW, stirring at the temperature of 30-40 ℃ for 10-15 min and the stirring speed of 120-130 r/min, and mixing to obtain a methemoglobin solution;
S3, adding the hydroxyl methemoglobin solution prepared in the S2 into the citral solution prepared in the S1, stirring at 20-25 ℃ for 13-18 min, stirring at 120-130 r/min, and uniformly mixing to obtain the pollen protein modifier.
Preferably, the preparation method of the film forming agent specifically comprises the following steps:
L1, weighing 100-110 parts by weight of lac resin and 250-280 parts by weight of absolute ethyl alcohol, placing the lac resin and the absolute ethyl alcohol into a stirring pot with the power of 1.8-2.2 kW, stirring at the temperature of 30-36 ℃ for 10-15 min and the stirring speed of 100-120 r/min, and uniformly mixing to obtain a lac resin solution;
and L2, weighing 30-45 parts of mandelic acid and 15-20 parts of paraoxybenzaldehyde by weight, adding the mixture into the lac resin solution prepared by L1, stirring at the temperature of 30-33 ℃ for 15-20 min and the stirring speed of 130-150 r/min, and stirring to obtain the film forming agent.
The beneficial effects obtained by the invention are as follows:
According to the invention, fresh lotus pollen is soaked by adopting aqueous solution of sodium sulfite, the polysaccharide structure in the pollen wall is loosened, the pollen wall is softened, and then the ultra-high pressure wall breaking is carried out, so that the content in the pollen wall is fully released, a pollen protein modifier containing citral and methemoglobin is added, under the oxidation effect of ferric ions in the methemoglobin, the electrophilic double bond in the citral is subjected to ring opening to generate electrophilic carbonium ions, and the sulfhydryl ions of cysteine residues in the pollen protein attack the electrophilic carbonium ions, so that the citral and the pollen protein are subjected to covalent bonding, the structure of the protein is changed, and the hydroformylation protein is generated; organic acid in the lotus powder cooperates with polylactic acid and aldehyde protein to react, aldehyde group in the aldehyde protein and amino group in the organic acid undergo nucleophilic addition reaction, the polylactic acid can introduce aldehyde group through the aldehyde reaction to form aldehyde-polylactic acid structure, aldehyde polymer formed by the reaction of the organic acid, polylactic acid and the aldehyde protein has good biocompatibility, and protein in the pollen and sensitization structure on the surface of the organic acid are modified, so that the identification of antibody to sensitization source is effectively interfered; cellulose in lotus powder is crosslinked with p-oxybenzaldehyde under the action of mandelic acid, and a stable and compact film structure is formed by cooperating with lac resin with biocompatibility to cover the surface of aldehyde group polymer, so that the recognition process between antigen and antibody is further blocked, meanwhile, citral and mandelic acid also have antibacterial property, and the growth of microorganisms is inhibited, so that the prepared hypoallergenic lotus powder extract has stable properties, the quality of the extract is not influenced by extraction conditions, the hypoallergenic lotus powder extract has low allergenicity, microorganisms cannot be bred after long-term storage, and the contained nutrients cannot be destroyed.
Drawings
In order to more clearly illustrate the invention or the technical solutions of the prior art, it will be apparent that the figures in the following description are only the invention, and that other figures can be obtained from these figures without inventive effort for a person skilled in the art, in a clearly understandable way.
FIG. 1 is a graph showing the results of the sensitization potential measurement according to the experimental example 2 of the present invention;
FIG. 2 is a graph showing the total number of colonies according to Experimental example 3 of the present invention;
FIG. 3 is an electron microscope image of the internal structure of the hypoallergenic lotus powder extract according to the present invention;
FIG. 4 is a diagram of the hypoallergenic lotus powder extract product according to the present invention.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and fully with reference to the accompanying drawings, in which it is evident that the embodiments described are only some, but not all embodiments of the invention; all other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art. In addition, any methods and materials similar or equivalent to those described herein can be used in the present application. The preferred methods and materials described herein are illustrative only and should not be construed as limiting the application.
The experimental methods in the following examples are all conventional methods unless otherwise specified; the test materials and test strains used in the examples described below, unless otherwise specified, were commercially available.
Example 1: the embodiment provides a preparation process of a hypoallergenic lotus powder extract, which comprises the following steps:
Weighing 400 parts by weight of fresh lotus powder, 30 parts by weight of sodium sulfite and 320 parts by weight of ultrapure water, putting into a stirring pot with the power of 1.6 kW for stirring at the temperature of 30 ℃ for 10 min and the stirring speed of 60 r/min, uniformly mixing, and soaking for 2h to obtain a lotus powder mixture;
Step two, placing the lotus powder mixture prepared in the step one into an ultrahigh pressure wall breaking machine with the power of 11.5 kW, the pressure of 1.8 MPa, the wall breaking temperature of 70 ℃, the wall breaking time of 15 min and the wall breaking rotating speed of 30000 r/min, and performing ultrahigh pressure wall breaking to obtain wall broken lotus powder;
step three, putting the wall-broken lotus pollen prepared in the step two and 100 parts by weight of pollen protein modifier into a reaction kettle with the power of 5.5 kW, wherein the reaction temperature is 40 ℃, the reaction time is 1.2 h, and the reaction rotating speed is 130 r/min, and reacting to obtain a pretreated lotus powder solution;
weighing 60 parts by weight of polylactic acid, putting the 60 parts by weight of polylactic acid into the pretreated pollen solution prepared in the third step, and reacting at 50 ℃ for 2h hours at a speed of 120 r/min to form an aldehyde polymer solution;
Weighing 120 parts by weight of film forming agent, putting the film forming agent into the aldehyde group polymer solution prepared in the fourth step, reacting at 35 ℃ for 2 h hours at 110 r/min to obtain a treated solution;
Step six, placing the treated solution obtained in the step five into a rapid extraction instrument with the power of 1.5 kW, wherein the rapid extraction temperature is 100 ℃, the rapid extraction time is 15 min, and performing rapid extraction to obtain a hypoallergenic extract solution;
Step seven, putting the hypoallergenic extract solution prepared in the step six into a high-efficiency thickener of 3.5 kW, concentrating at 40 ℃ for 1.2 h, and concentrating to obtain hypoallergenic extract concentrated solution;
and step eight, placing the hypoallergenic extract concentrated solution prepared in the step seven into an ultralow temperature freeze dryer with the power of 1.5 kW, wherein the low temperature freeze drying temperature is-70 ℃, the freeze drying time is 20 h, and heating to 25 ℃ after ultralow temperature drying to obtain the hypoallergenic lotus powder extract.
The preparation method of the pollen protein modifier specifically comprises the following steps:
S1, weighing 20 parts by weight of citral and 120 parts by weight of absolute ethyl alcohol, putting the citral and the absolute ethyl alcohol into a stirring pot with the power of 1.8 kW, stirring at 25 ℃ for 8 min and the stirring speed of 130 r/min, and mixing and dissolving to obtain a citral solution;
S2, weighing 30 parts by weight of methemoglobin, 5 parts by weight of sodium bicarbonate and 110 parts by weight of absolute ethyl alcohol, putting the mixture into a stirring pot with the power of 1.8 kW, stirring at the temperature of 30 ℃ for 10min and the stirring speed of 120 r/min, and mixing to obtain a methemoglobin solution;
S3, adding the hydroxyl methemoglobin solution prepared in the S2 into the citral solution prepared in the S1, stirring at 20 ℃ for 13 min hours at 120 r/min, and uniformly mixing to obtain the pollen protein modifier.
The preparation method of the film forming agent specifically comprises the following steps:
weighing 100 parts by weight of lac resin and 250 parts by weight of absolute ethyl alcohol, putting the lac resin and the absolute ethyl alcohol into a stirring pot with the power of 1.8 kW, stirring at the temperature of 30 ℃ for 10min and the stirring speed of 100 r/min, and uniformly mixing to obtain a lac resin solution;
And L2, weighing 30 parts of mandelic acid and 15 parts of paraoxybenzaldehyde by weight, adding the mixture into the lac resin solution prepared by L1, stirring at the temperature of 30 ℃ for 15 min hours at the stirring speed of 130 r/min, and stirring to obtain the film forming agent.
Example 2: the embodiment provides a preparation process of a hypoallergenic lotus powder extract, which comprises the following steps:
Firstly, weighing 450 parts by weight of fresh lotus powder, 35 parts by weight of sodium sulfite and 340 parts by weight of ultrapure water, putting the fresh lotus powder and the 35 parts by weight of sodium sulfite into a stirring pot with the power of 1.7 kW for stirring at the temperature of 33 ℃ for 13 min and at the stirring speed of 70 r/min, and soaking the mixture in 2.5 h after uniform mixing to obtain a lotus powder mixture;
step two, placing the lotus powder mixture prepared in the step one into an ultrahigh pressure wall breaking machine with the power of 12.5 kW, the pressure of 1.8 MPa, the wall breaking temperature of 73 ℃, the wall breaking time of 18 min and the wall breaking rotating speed of 35000 r/min, and performing ultrahigh pressure wall breaking to obtain wall broken lotus powder;
Step three, placing the wall-broken lotus pollen prepared in the step two and 110 parts by weight of pollen protein modifier into a reaction kettle with the power of 6 kW, wherein the reaction temperature is 43 ℃, the reaction time is 1.3 h, and the reaction speed is 140 r/min, and reacting to obtain a pretreated lotus powder solution;
Weighing 65 parts by weight of polylactic acid, putting the 65 parts by weight of polylactic acid into the pretreated pollen solution prepared in the third step, and reacting at a temperature of 55 ℃ for 2.5 h hours at a speed of 130 r/min to form an aldehyde polymer solution;
Step five, weighing 130 parts by weight of film forming agent, putting the film forming agent into the aldehyde group polymer solution prepared in the step four, reacting at 40 ℃ for 2.3 h hours at 110 r/min to obtain a treated solution;
step six, placing the treated solution obtained in the step five into a rapid extraction instrument with the power of 1.8 kW, wherein the rapid extraction temperature is 110 ℃, the rapid extraction time is 18 min, and performing rapid extraction to obtain a hypoallergenic extract solution;
step seven, putting the hypoallergenic extract solution prepared in the step six into a high-efficiency thickener of 4 kW, concentrating at 45 ℃ for 1.3 h, and concentrating to obtain hypoallergenic extract concentrated solution;
and step eight, placing the hypoallergenic extract concentrated solution prepared in the step seven into an ultralow temperature freeze dryer with the power of 1.6 kW, wherein the low temperature freeze drying temperature is-70 ℃, the freeze drying time is 21 h, and heating to 27 ℃ after ultralow temperature drying to obtain the hypoallergenic lotus powder extract.
The preparation method of the pollen protein modifier specifically comprises the following steps:
s1, weighing 25 parts by weight of citral and 130 parts by weight of absolute ethyl alcohol, putting the citral and the absolute ethyl alcohol into a stirring pot with the power of 2 kW, stirring at the temperature of 27 ℃ for 10min and the stirring speed of 140 r/min, and mixing and dissolving to obtain a citral solution;
S2, weighing 35 parts by weight of methemoglobin, 6 parts by weight of sodium bicarbonate and 115 parts by weight of absolute ethyl alcohol, putting into a stirring pot with the power of 2 kW, stirring at 35 ℃ for 13 min and at the stirring speed of 120 r/min, and mixing to obtain a methemoglobin solution;
S3, adding the hydroxyl methemoglobin solution prepared in the S2 into the citral solution prepared in the S1, stirring at the temperature of 23 ℃ for 16 min hours at the stirring speed of 120 r/min, and uniformly mixing to obtain the pollen protein modifier.
The preparation method of the film forming agent specifically comprises the following steps:
weighing 105 parts by weight of lac resin and 265 parts by weight of absolute ethyl alcohol, putting the lac resin and the 265 parts by weight of absolute ethyl alcohol into a stirring pot with the power of 2 kW, stirring at the temperature of 33 ℃ for 13 min and the stirring speed of 110 r/min, and uniformly mixing to obtain a lac resin solution;
and (2) weighing 35 parts of mandelic acid and 18 parts of paraoxybenzaldehyde by weight, adding the mixture into the lac resin solution prepared by the L1, stirring at the temperature of 32 ℃ for 18 min hours at the stirring speed of 140 r/min, and stirring to obtain the film forming agent.
Example 3: the embodiment provides a preparation process of a hypoallergenic lotus powder extract, which comprises the following steps:
Weighing 500 parts by weight of fresh lotus powder, 40 parts by weight of sodium sulfite and 360 parts by weight of ultrapure water, putting into a stirring pot with the power of 1.8 kW for stirring at the temperature of 35 ℃ for 15 min and the stirring speed of 80 r/min, uniformly mixing, and soaking for 3h to obtain a lotus powder mixture;
Step two, placing the lotus powder mixture prepared in the step one into an ultrahigh pressure wall breaking machine with the power of 13.5 kW, the pressure of 1.8 MPa, the wall breaking temperature of 75 ℃, the wall breaking time length of 20 min and the wall breaking rotating speed of 40000 r/min, and performing ultrahigh pressure wall breaking to obtain wall broken lotus powder;
Step three, putting the wall-broken lotus pollen prepared in the step two and 120 parts by weight of pollen protein modifier into a reaction kettle with the power of 6.5 kW, wherein the reaction temperature is 45 ℃, the reaction time is 1.4 h, and the reaction rotating speed is 150 r/min, and reacting to obtain a pretreated lotus powder solution;
Weighing 70 parts by weight of polylactic acid, putting the 70 parts by weight of polylactic acid into the pretreated pollen solution prepared in the third step, and reacting at a reaction temperature of 60 ℃ for 3 h hours at a reaction speed of 140 r/min to form an aldehyde polymer solution;
step five, weighing 140 parts by weight of film forming agent, putting the film forming agent into the aldehyde group polymer solution prepared in the step four, reacting at 45 ℃ for 2.5 h hours at 120 r/min, and reacting to obtain a treated solution;
Step six, placing the treated solution obtained in the step five into a rapid extraction instrument with the power of 2.2 kW, wherein the rapid extraction temperature is 120 ℃, the rapid extraction time is 20 min, and performing rapid extraction to obtain a hypoallergenic extract solution;
step seven, putting the hypoallergenic extract solution prepared in the step six into a high-efficiency thickener of 4.5 kW, concentrating at 50 ℃ for 1.5 h, and concentrating to obtain hypoallergenic extract concentrated solution;
and step eight, placing the hypoallergenic extract concentrated solution prepared in the step seven into an ultralow temperature freeze dryer with the power of 1.8 kW, wherein the low temperature freeze drying temperature is-70 ℃, the freeze drying time is 22 h, and heating to 28 ℃ after ultralow temperature drying to obtain the hypoallergenic lotus powder extract.
The preparation method of the pollen protein modifier specifically comprises the following steps:
S1, weighing 30 parts by weight of citral and 140 parts by weight of absolute ethyl alcohol, putting the citral and the absolute ethyl alcohol into a stirring pot with the power of 2.2 kW, stirring at 28 ℃ for 12 min and the stirring speed of 150 r/min, and mixing and dissolving to obtain a citral solution;
s2, weighing 40 parts by weight of methemoglobin, 8 parts by weight of sodium bicarbonate and 120 parts by weight of absolute ethyl alcohol, putting the mixture into a stirring pot with the power of 2.2 kW, stirring at 40 ℃ for 15 min and the stirring speed of 130 r/min, and mixing to obtain a methemoglobin solution;
S3, adding the hydroxyl methemoglobin solution prepared in the S2 into the citral solution prepared in the S1, stirring at 25 ℃ for 18 min hours at 130 r/min, and uniformly mixing to obtain the pollen protein modifier.
The preparation method of the film forming agent specifically comprises the following steps:
Weighing 110 parts by weight of lac resin and 280 parts by weight of absolute ethyl alcohol, putting the lac resin and the 280 parts by weight of absolute ethyl alcohol into a stirring pot with the power of 2.2kW, stirring at 36 ℃ for 15min and the stirring speed of 120 r/min, and uniformly mixing to obtain a lac resin solution;
and (2) weighing 45 parts of mandelic acid and 20 parts of paraoxybenzaldehyde by weight, adding the mixture into the lac resin solution prepared by the L1, stirring at 33 ℃ for 20 min hours at 150 r/min, and stirring to obtain the film forming agent.
Example 4: the embodiment provides a preparation process of a hypoallergenic lotus powder extract, which comprises the following steps:
Weighing 430 parts by weight of fresh lotus powder, 33 parts by weight of sodium sulfite and 330 parts by weight of ultrapure water, putting into a stirring pot with the power of 1.6 kW for stirring at the stirring temperature of 32 ℃ for 12 min and the stirring speed of 60 r/min, and soaking 2.3 h after uniformly mixing to obtain a lotus powder mixture;
Step two, placing the lotus powder mixture prepared in the step one into an ultrahigh pressure wall breaking machine with the power of 12 kW, the pressure of 1.8 MPa, the wall breaking temperature of 72 ℃, the wall breaking time of 16 min and the wall breaking rotating speed of 33000 r/min, and performing ultrahigh pressure wall breaking to obtain wall broken lotus powder;
step three, putting the wall-broken lotus pollen prepared in the step two and 105 parts by weight of pollen protein modifier into a reaction kettle with the power of 5.8 kW, wherein the reaction temperature is 42 ℃, the reaction time is 1.2 h, and the reaction rotating speed is 130 r/min, and reacting to obtain a pretreated lotus powder solution;
Weighing 62 parts by weight of polylactic acid, putting the polylactic acid into the pretreated pollen solution prepared in the third step, and reacting at 53 ℃ for 2.2 h hours at a speed of 120 r/min to form an aldehyde polymer solution;
Weighing 125 parts by weight of film forming agent, putting the film forming agent into the aldehyde group polymer solution prepared in the fourth step, reacting at 38 ℃ for 2.2 h hours at 110 r/min to obtain a treated solution;
step six, placing the treated solution obtained in the step five into a rapid extraction instrument with the power of 1.7 kW, wherein the rapid extraction temperature is 105 ℃, the rapid extraction time is 16 min, and performing rapid extraction to obtain a hypoallergenic extract solution;
step seven, putting the hypoallergenic extract solution prepared in the step six into a high-efficiency thickener of 3.8 kW, concentrating at the temperature of 43 ℃ for 1.2 h, and concentrating to obtain hypoallergenic extract concentrated solution;
and step eight, placing the hypoallergenic extract concentrated solution prepared in the step seven into an ultralow temperature freeze dryer with the power of 1.6 kW, wherein the low temperature freeze drying temperature is-70 ℃, the freeze drying time is 20 h, and heating to 26 ℃ after ultralow temperature drying to obtain the hypoallergenic lotus powder extract.
The preparation method of the pollen protein modifier specifically comprises the following steps:
S1, weighing 23 parts by weight of citral and 125 parts by weight of absolute ethyl alcohol, putting the citral and the absolute ethyl alcohol into a stirring pot with the power of 1.9 kW, stirring at 26 ℃ for 9 min and the stirring speed of 140 r/min, and mixing and dissolving to obtain a citral solution;
S2, weighing 33 parts by weight of methemoglobin, 6 parts by weight of sodium bicarbonate and 113 parts by weight of absolute ethyl alcohol, putting into a stirring pot with the power of 1.9 kW, stirring at the temperature of 33 ℃ for 12 min and the stirring speed of 120 r/min, and mixing to obtain a methemoglobin solution;
S3, adding the hydroxyl methemoglobin solution prepared in the S2 into the citral solution prepared in the S1, stirring at a temperature of 22 ℃ for 14 min hours at a stirring speed of 120 r/min, and uniformly mixing to obtain the pollen protein modifier.
The preparation method of the film forming agent specifically comprises the following steps:
weighing 103 parts by weight of lac resin and 260 parts by weight of absolute ethyl alcohol, putting the lac resin and the absolute ethyl alcohol into a stirring pot with the power of 1.9 kW, stirring at the temperature of 32 ℃ for 12 min and the stirring speed of 100 r/min, and uniformly mixing to obtain a lac resin solution;
And (2) weighing 33 parts by weight of mandelic acid and 17 parts by weight of paraoxybenzaldehyde, adding the mixture into the lac resin solution prepared by the L1, stirring at 31 ℃ for 17 min hours at 130 r/min, and stirring to obtain the film forming agent.
Example 5: the embodiment provides a preparation process of a hypoallergenic lotus powder extract, which comprises the following steps:
Firstly, weighing 480 parts by weight of fresh lotus powder, 38 parts by weight of sodium sulfite and 350 parts by weight of ultrapure water, putting into a stirring pot with the power of 1.8 kW for stirring at the stirring temperature of 34 ℃ for 14 min and the stirring speed of 80 r/min, and soaking 2.8 h after uniformly mixing to obtain a lotus powder mixture;
Step two, placing the lotus powder mixture prepared in the step one into an ultrahigh pressure wall breaking machine with the power of 13 kW, the pressure of 1.8 MPa, the wall breaking temperature of 74 ℃, the wall breaking time of 19 min and the wall breaking rotating speed of 38000 r/min, and performing ultrahigh pressure wall breaking to obtain wall broken lotus powder;
step three, putting the wall-broken lotus pollen prepared in the step two and 115 parts by weight of pollen protein modifier into a reaction kettle with the power of 6.3 kW, wherein the reaction temperature is 44 ℃, the reaction time is 1.4 h, and the reaction speed is 150 r/min, and reacting to obtain a pretreated lotus powder solution;
Weighing 68 parts by weight of polylactic acid, putting the polylactic acid into the pretreated pollen solution prepared in the third step, and reacting at 58 ℃ for 2.7 h hours at 140 r/min to form an aldehyde polymer solution;
Step five, weighing 135 parts by weight of film forming agent, putting the film forming agent into the aldehyde group polymer solution prepared in the step four, reacting at 42 ℃ for 2.4 h hours at 120 r/min to obtain a treated solution;
Step six, placing the treated solution obtained in the step five into a rapid extraction instrument with the power of 2.1 kW, wherein the rapid extraction temperature is 115 ℃, the rapid extraction time is 19: 19 min, and performing rapid extraction to obtain a hypoallergenic extract solution;
Step seven, putting the hypoallergenic extract solution prepared in the step six into a high-efficiency thickener of 4.3 kW, concentrating at 48 ℃ for 1.4 h, and concentrating to obtain hypoallergenic extract concentrated solution;
and step eight, placing the hypoallergenic extract concentrated solution prepared in the step seven into an ultralow temperature freeze dryer with the power of 1.7 kW, wherein the low temperature freeze drying temperature is-70 ℃, the freeze drying time is 21 h, and heating to 28 ℃ after ultralow temperature drying to obtain the hypoallergenic lotus powder extract.
The preparation method of the pollen protein modifier specifically comprises the following steps:
s1, weighing 28 parts by weight of citral and 135 parts by weight of absolute ethyl alcohol, putting the citral and the absolute ethyl alcohol into a stirring pot with the power of 2.1 kW, stirring at 28 ℃ for 11 min and at the stirring speed of 150 r/min, and mixing and dissolving to obtain a citral solution;
s2, weighing 38 parts by weight of methemoglobin, 7 parts by weight of sodium bicarbonate and 118 parts by weight of absolute ethyl alcohol, putting the materials into a stirring pot with the power of 2.1 kW, stirring at 38 ℃ for 14 min and at the stirring speed of 130 r/min, and mixing to obtain a methemoglobin solution;
S3, adding the hydroxyl methemoglobin solution prepared in the S2 into the citral solution prepared in the S1, stirring at 24 ℃ for 17 min hours at 120 r/min, and uniformly mixing to obtain the pollen protein modifier.
The preparation method of the film forming agent specifically comprises the following steps:
Weighing 108 parts by weight of lac resin and 270 parts by weight of absolute ethyl alcohol, putting the lac resin and the 270 parts by weight of absolute ethyl alcohol into a stirring pot with the power of 2.1 kW, stirring at 35 ℃ for 14 min and at the stirring speed of 120 r/min, and uniformly mixing to obtain a lac resin solution;
And L2, weighing 40 parts of mandelic acid and 19 parts of paraoxybenzaldehyde by weight, adding the mixture into the lac resin solution prepared by L1, stirring at 33 ℃ for 19 min hours at 150 r/min, and stirring to obtain the film forming agent.
Experimental example 1: and (5) testing the quality of the lotus pollen extract.
The quality measurement test steps of the hypoallergenic lotus powder extract prepared in the embodiments 1-5 of the invention are as follows:
(1) The hypoallergenic lotus powder extracts prepared in examples 1-5 of 5 g were weighed as experimental groups and the same common lotus powder extracts purchased at different times of 5 g were weighed as control groups 1-3, 3 in parallel, and observations in terms of color, aroma, purity, dryness and uniformity were made and recorded, and the results are shown in table 1 and fig. 4.
TABLE 1 extract quality appearance measurement Table
Analysis of results: FIG. 4 is a graph showing the products of the hypoallergenic lotus powder extracts of the present invention, wherein the hypoallergenic lotus powder extracts of examples 1-5 are bright and uniform in color, have faint scent, have no impurity, are properly dried, have fine and uniform particles, and the quality of the common lotus powder extracts of the control group is extremely unstable, as shown in Table 1 and FIG. 4, showing that the hypoallergenic lotus powder extracts of examples 1-5 are high in quality, are not affected by the extraction conditions, and maintain consistent extraction quality.
Experimental example 2: and (5) a lotus pollen extract sensitization measurement test.
The sensitization test steps of the hyposensitization lotus powder extract prepared in the embodiments 1-5 of the invention are that
(1) Weighing the hypoallergenic lotus powder extracts prepared in examples 1-5 with the weight of 1g respectively to prepare experimental group samples with the concentration of 500 mg/mL, weighing the common lotus powder extract with the weight of 1g as a CK control group to prepare control group samples with the concentration of 500 mg/mL, respectively adding the control group samples to an ELISA plate, and adding 0.1 mL of the control group samples at the temperature of 4 ℃ for overnight at each hole;
(2) Washing the plate with washing solution for 5 times, incubating for 5 min times at each time at 250 mL/hole and at 28 ℃, beating, adding 200 mL bovine serum albumin (5%) into each hole for sealing, incubating for 2h times at 37 ℃, and washing the plate for 5 times;
(3) Adding 100 mL/hole of mixed serum of allergic patient with lotus powder extract diluted 1:30, incubating at 37deg.C for 1:1 h, and washing the plate 5 times after the reaction;
(4) Adding biotin-marked sheep anti-human IgE 200 mL/hole at a dilution of 1:5000, incubating at 37 ℃ for 2: 2h, and washing the plate for 5 times; adding substrate color development liquid 100 mL/hole, and developing color at 37 ℃ in a dark place for 30 min; after development, the reaction was terminated by adding 50 mL/well of sulfuric acid solution at a concentration of 2 mol/L, and the absorbance (OD value) was measured at a wavelength of 450nm, the binding capacity of the experimental group sample to IgE was calculated according to the formula, igE binding capacity (%) = OD experimental group /OD control group X100%, the data were counted and analyzed by using IBM SPSS STATISTICS 22.0 software, and the graph was drawn using Origin2022.
Experimental example 3: and (5) preservation and measurement tests of lotus powder extracts.
The preservation and measurement test steps of the hypoallergenic lotus powder extract prepared in the embodiments 1-5 of the invention are as follows:
(1) The hypoallergenic lotus powder extracts prepared in examples 1-5 with a weight of 10 g were weighed as samples of the experimental group, the common lotus powder extract with a weight of 10 g was weighed as a CK control group, and 5 samples were taken in parallel;
(2) Preserving in a refrigerator at 4 ℃ and taking out samples of an experimental group and a control group at intervals of 15 d, respectively, inoculating 0.5 g to a test tube of 50 mL sterile liquid LB culture medium, and shake-culturing 24h in a shaking table at 37 ℃ and 120 r/min to obtain a cultured bacterial liquid;
(3) Diluting the cultured bacterial liquid by 100 times, taking 50 mu L of the cultured bacterial liquid on an LB solid medium plate by using a pipetting gun in an ultra-clean workbench, uniformly coating, and then, pouring the bacterial liquid into a 37 ℃ incubator for culturing 24 h to obtain the colony numbers of each group of plates, and calculating the colony numbers according to a formula: total colony count (cfu/g) =number of colonies per plate x total dilution, 1 was measured every 15 d times, 8 times in succession, and recordings were made.
Analysis of results:
FIG. 1 is a graph showing the results of the sensitization potential measurement in experimental example 2 of the present invention, wherein the binding potential of the hypoallergenic lotus powder extract and IgE antibodies in examples 1-5 is respectively reduced by 82.6%, 85.3%, 87.4%, 84.3% and 84% compared with the control group, which indicates that the sensitization structure of the sensitization source surface in the hypoallergenic lotus powder extract prepared by the present invention is modified, effectively interferes with and blocks the recognition process of the antibodies to the sensitization source, and has obvious hyposensitization;
FIG. 3 is an electron microscope image of the internal structure of the hypoallergenic lotus powder extract, wherein the internal structure of the extract is compact, and the surface layer is covered with a film; FIG. 2 is a graph showing the change in the total number of colonies according to Experimental example 3 of the present invention, as shown in the graph, the hypoallergenic lotus powder extracts according to examples 1 to 5 contained colony numbers of 6 d/g, 12 d/g, 17 d/g, 22 d/g, 35 d/g, 42 d/g, 48 d/g, 54 d/g when 15 d, 30 d, 45 d, 60 d, 75 d, 90 d, 105 d, 120 d were stored, the colony numbers of the prepared hypoallergenic lotus powder extract are 289 d/g, 366 d/g, 486 d/g, 742 d/g, 963 d/g, 1168 d/g, 1324 d/g and 1685 d/g, which shows that the biocompatible shellac resin in the hypoallergenic lotus powder extract prepared by the invention forms a stable and compact film structure to cover the surface of aldehyde group polymer, and the citral and mandelic acid have antibacterial property, obviously inhibit the growth of microorganisms, and the components contained in the hypoallergenic lotus powder extract can not be destroyed after long-term storage.
Although embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made therein without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
The invention and its embodiments have been described above with no limitation, and the invention is illustrated in the figures of the accompanying drawings as one of its embodiments, without limitation in practice. In summary, those skilled in the art, having benefit of this disclosure, will appreciate that the invention can be practiced without the specific details disclosed herein.
Claims (1)
1. The preparation process of the hypoallergenic lotus powder extract is characterized by comprising the following steps of:
Weighing 400-500 parts by weight of fresh lotus powder, 30-40 parts by weight of sodium sulfite and 320-360 parts by weight of ultrapure water, uniformly mixing and soaking to obtain a lotus powder mixture;
Step two, carrying out ultrahigh pressure wall breaking on the lotus powder mixture prepared in the step one, and carrying out reaction modification on the lotus powder mixture and 100-120 parts by weight of pollen protein modifier to obtain a pretreated lotus powder solution;
Weighing 60-70 parts by weight of polylactic acid, putting the polylactic acid into the pretreated pollen solution prepared in the second step, adding 120-140 parts of film forming agent after polymerization reaction, and continuing reaction to obtain a treated solution;
step four, the solution prepared in the step three is subjected to quick extraction, concentration and ultralow-temperature drying and then is subjected to temperature return to obtain the hypoallergenic lotus powder extract;
The preparation method of the pollen protein modifier specifically comprises the following steps:
S1, weighing 20-30 parts by weight of citral, and dispersing the citral in 120-140 parts by weight of absolute ethyl alcohol to obtain a citral solution;
S2, weighing 30-40 parts by weight of methemoglobin, 5-8 parts by weight of sodium bicarbonate and 110-120 parts by weight of absolute ethyl alcohol, and heating and uniformly mixing to obtain a methemoglobin solution;
S3, adding the methemoglobin solution prepared in the step S2 into the citral solution prepared in the step S1, and stirring and mixing to obtain a pollen protein modifier;
The preparation method of the film forming agent specifically comprises the following steps:
L1, weighing 100-110 parts by weight of lac resin and 250-280 parts by weight of absolute ethyl alcohol, and uniformly mixing to obtain a lac resin solution;
And L2, weighing 30-45 parts of mandelic acid and 15-20 parts of paraoxybenzaldehyde by weight, adding the mixture into the lac resin solution prepared by L1, and stirring to obtain the film forming agent.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2005179246A (en) * | 2003-12-18 | 2005-07-07 | Morinaga & Co Ltd | Allergic hypersensitivity inhibitor |
| CN102948656A (en) * | 2012-10-26 | 2013-03-06 | 北京知蜂堂蜂产品有限公司 | Method for wall breaking, desensitization and water-soluble component extraction of pollen and water-soluble pollen cream prepared by the method |
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2005179246A (en) * | 2003-12-18 | 2005-07-07 | Morinaga & Co Ltd | Allergic hypersensitivity inhibitor |
| CN102948656A (en) * | 2012-10-26 | 2013-03-06 | 北京知蜂堂蜂产品有限公司 | Method for wall breaking, desensitization and water-soluble component extraction of pollen and water-soluble pollen cream prepared by the method |
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