CN111732616B - Method and system for separating out and recovering amygdalin in green plums - Google Patents
Method and system for separating out and recovering amygdalin in green plums Download PDFInfo
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Abstract
The invention belongs to the technical field of extraction and recovery of amygdalin, and particularly relates to a method and a system for separating out and recovering amygdalin from green plums. The method comprises the following steps: 1) cleaning green plum and pricking; 2) separating out amygdalin: coating a precipitated material of amygdalin on the surface of the green plum with the hole, and then immersing the green plum in a saline solution; 3) adsorbing amygdalin: separating the saline solution obtained in the step 2) and adsorbing amygdalin in the saline solution by adopting an adsorbing material column chromatography; 4) recovering amygdalin: eluting and resolving the adsorption material with saturated adsorption by adopting ethanol solution, adding the ethanol solution into the obtained eluent for repeated crystallization, then carrying out vacuum concentration and vacuum freeze drying to obtain a freeze-dried product, crushing the freeze-dried product to obtain the amygdalin product, reducing the waste water discharge and the loss of nutrient components in the processing process, and recycling the amygdalin in the bitter almond debitterizing water, thereby having important practical significance.
Description
Technical Field
The invention belongs to the technical field of extraction and recovery of amygdalin, and particularly relates to a method and a system for separating out and recovering amygdalin from green plums.
Background
The green plums are typical low-sugar high-acid fruits, are rich in natural citric acid, malic acid and oxalic acid, and also contain a small amount of tartaric acid, lactic acid, acetic acid and succinic acid, the content of the citric acid is the highest and reaches about 90% of the total acid content, the green plums are mainly used as processing products of preserved fruits (preserved fruits), however, due to the fact that the green plums contain amygdalin, the bitter and astringent taste of the green plums is serious, researches show that the content of the amygdalin in the flesh of the seven-ripe green plums reaches 784mg/kg, and the content of the nine-ripe green plums reaches 250-270 mg/kg.
The green plums are taken as preserved fruit (preserved fruit) products and are one of foods preferred by people, in the traditional processing process, the green plums need to be ground into skin and then dipped into salt water, and amygdalin can be separated out after long-time soaking, so that the purpose of debitterizing is achieved, but along with the outflow of natural organic acid and phenolic substances, the loss of the organic acid in the long-time debitterizing process of the green plums is up to 60 percent, the loss of natural nutrient components in the green plums is caused, the nutrient value of the green plums is reduced, and meanwhile, after the debitterizing process, a large amount of high-concentration salt water is discharged, so that the environmental pollution is easily caused. The research shows that the amygdalin has certain pharmacological effects, including immunoregulation effect, and can strengthen the organism; has antitussive, antiasthmatic, and antiinflammatory effects; has good anti-tumor effect, mainly affects the tumor cell cycle, induces apoptosis and cytotoxicity and enhances the anti-tumor activity through an immunological mechanism. Therefore, the recovery of amygdalin in the debitterizing process of the green plums can not only reduce the influence on the environment, but also improve the utilization value of the amygdalin.
Disclosure of Invention
In view of the above problems, the present invention aims at the precipitation and recovery of amygdalin in the green plum debitterizing process, and the reuse of saline water, reducing the loss of organic acids in green plums, and simultaneously reducing the discharge of saline water and pollution.
The technical content of the invention is as follows:
the invention provides a method for separating out and recovering amygdalin in green plums, which comprises the following steps:
1) removing impurities from fresh green plums, cleaning, grinding the cleaned green plums into skin, and pricking holes;
2) separating out amygdalin: coating a separating-out material of amygdalin on the surface of the green plums with holes, standing for 3-4 hours, then immersing the green plums with holes into a saline solution with the concentration of 40-60%, and circularly flowing the saline for 2-3 hours;
3) adsorbing amygdalin: separating the saline solution obtained in the step 2), adsorbing amygdalin in the saline solution by adopting an adsorbing material column chromatography, and circularly flowing the saline solution for 2-3 hours;
4) recovering amygdalin: eluting and resolving the adsorption material with saturated adsorption by using 60-80% ethanol solution, adding 90-95% ethanol solution into the obtained eluent for repeated crystallization, then performing vacuum concentration (concentrating until the water content is less than or equal to 30%) and vacuum freeze drying, and crushing the obtained freeze-dried product to obtain the amygdalin product.
The precipitation material in the step 2) is a mixture of salt and pepper particles, citric acid and xylitol, and the use ratio of the salt and pepper particles, the citric acid and the xylitol is (2-3): 1: 1; the separated salt-pepper granules and xylitol in the material can improve the osmotic pressure on the surface of the green plum and promote the dissolution of amygdalin, and simultaneously, according to the principle of similarity and intermiscibility, the xylitol and the amygdalin have similar structures and stronger adsorption capacity to the amygdalin and can also promote the separation of the amygdalin. In addition, the green plums are also rich in citric acid, and the citric acid is added into a separated material to inhibit the separation of the citric acid and other nutrient components;
the mixing volume ratio of the green plums to the saline solution is 1 (1-1.5).
The adsorbing material in the step 3) is prepared from styrene, propylene organic matters, tea stem powder, a pore-forming agent, an initiator and a catalyst, wherein the propylene organic matters comprise acrylonitrile, methyl acrylate and acrylamide; according to the mass fraction, the styrene accounts for 30-35%, the propylene organic matter accounts for 8-15%, and the tea stem powder accounts for 5-10%; the surface of the adopted tea stem powder is provided with adsorption holes, which is beneficial to improving the specific surface area and the adsorption capacity of the formed adsorbent, and the tea stem has biological activity close to the activity of the amygdalin, so that the adsorption of the amygdalin can be enhanced.
The preparation method of the adsorbing material refers to a patent CN201510833870.1, namely an adsorbing resin with an ultra-large specific surface area and a preparation method thereof, and comprises the following steps:
a) adding a sodium chloride aqueous solution into a reaction kettle, heating to 45 ℃, mixing styrene, propylene organic matters, tea stem powder, a pore-forming agent, an initiator and a catalyst component, stirring at 45 ℃ for 10-15min, adding into the reaction kettle, uniformly stirring, heating the reaction kettle to 65 ℃ at the speed of 2-3 ℃/min, preserving heat for 3-4 hours, heating to 80 ℃ at the speed of 1 ℃/min, preserving heat for 3-5 hours, and cooling to obtain a white gray ball;
b) putting the white-gray balls into a washing kettle for washing, then sending the white-gray balls into a dryer for drying, and screening the white-gray balls with qualified particle size after drying;
c) adding appropriate amount of styrene, propylene organic matters and tea stem powder into the white gray ball obtained in the step b), stirring for 30min, adding appropriate amount of pore-forming agent, initiator and catalyst, stirring and mixing for 10-15min at 45 ℃ to obtain a mixed raw material; adding a sodium chloride solution into a reaction kettle, heating to 45 ℃, adding the mixed raw materials, uniformly stirring, heating to 65 ℃ at the speed of 2-3 ℃/min, preserving heat for 3-4 hours, then heating to 80 ℃ at the speed of 1 ℃/min, preserving heat for 3-5 hours, and cooling to obtain resin balls;
d) and c) cleaning the resin balls obtained in the step c) by using ethanol, then washing with water, then drying in a dryer, and obtaining the adsorbing material after drying.
Further, the vacuum degree of the vacuum concentration in the step 4) is 60-70 kPa, and the vacuum degree of the vacuum freeze drying is 5-10 Pa.
The invention also provides a system for separating out and recovering amygdalin of green plums, which comprises:
1) amygdalin precipitation device: comprises saline solution and a circulating component, which is used for soaking the green plums coated with precipitation materials to further precipitate amygdalin in the green plums;
2) amygdalin adsorption equipment: comprises an adsorption material and a circulating component, which are used for adsorbing the amygdalin in the saline solution from the precipitation device;
3) amygdalin recovery device
The method and the system for separating out and recovering the amygdalin in the green plums are combined as follows:
A) taking fresh green plums, removing impurities, cleaning, grinding the cleaned green plums into skin and pricking holes;
B) separating out amygdalin: coating a separating-out material of amygdalin on the surface of the green plums with holes, standing for 3-4 hours, then soaking the green plums with holes in an amygdalin separating-out device, wherein the concentration of a saline solution in the separating-out device is 40-60%, a circulating component comprises a circulating pump, the circulating pump is started to enable the flow rate of the saline solution to be 8-12 mL/min, and the saline solution circularly flows for 2-3 hours;
C) adsorbing amygdalin: opening a valve between the precipitation device and the adsorption device, allowing the saline solution in the precipitation device to flow into the adsorption device, adsorbing amygdalin in the saline solution by adopting an adsorbing material column chromatography, wherein the circulating component comprises a circulating pump, the circulating pump is started to allow the flow rate of the saline solution to be 10-15 mL/min, and the saline solution circularly flows for 2-3 hours;
D) recovering amygdalin: taking out the adsorption material with saturated adsorption, soaking the adsorption material in 60-80% ethanol solution for elution and analysis, adding 90-95% ethanol solution into the obtained eluent for repeated crystallization, carrying out vacuum concentration (concentration is carried out until the water content is less than or equal to 30%) and vacuum freeze drying on the obtained crystallization solution, and crushing the obtained freeze-dried product to obtain the amygdalin product.
The invention has the following beneficial effects:
compared with the traditional method, the method and the system for separating out and recovering the amygdalin in the green plums shorten the time of the green plum debitterizing process, can simultaneously recover the separated amygdalin on line, and have the recovery rate of 40 percent or more.
The method and the system device adopted by the invention have the advantages of easily available raw materials, low cost and capability of changing waste into valuable, and the process has important reference value for separating out and recovering amygdalin in green plums and even other foods containing amygdalin.
Detailed Description
The present invention is described in further detail in the following detailed description with reference to specific embodiments, which are intended to be illustrative only and not to be limiting of the scope of the invention, as various equivalent modifications of the invention will become apparent to those skilled in the art after reading the present invention and are intended to be included within the scope of the appended claims.
All the raw materials and reagents of the invention are conventional market raw materials and reagents unless otherwise specified.
Example 1
A process for separating out and recovering amygdalin from mume fructus comprises:
A) taking 100 fresh green plums with uniform size and average gram weight of 25g, removing impurities, cleaning, grinding the cleaned green plums, and pricking holes on the surfaces of the green plums by using a pricking needle, wherein the holes are uniformly distributed;
B) separating out amygdalin: coating a separating-out material of amygdalin (the mixing ratio of pepper salt particles, citric acid and xylitol is respectively 2:1:1) on the surface of the green plum with holes, standing for 3-4 hours, then soaking the green plum with holes in an amygdalin separating-out device, wherein the mixing volume ratio of the green plum and a saline solution is 1:1, the concentration of the saline solution in the separating-out device is 40%, starting a circulating pump to enable the flow rate of the saline solution to be 8-12 mL/min, and enabling the saline solution to circularly flow for 2-3 hours;
C) adsorbing amygdalin: after the circulation flow in the precipitation device is finished, opening a valve between the precipitation device and the adsorption device, enabling the saline solution in the precipitation device to completely flow into the adsorption device, closing the valve, filling the adsorption device with an adsorption material, adopting adsorption material column chromatography to adsorb amygdalin in the saline solution, starting a circulating pump to enable the flow rate of the saline solution to be 10-15 mL/min, and enabling the saline solution to circularly flow for 2-3 hours so as to enable the adsorption material to be in saturated adsorption;
D) recovering amygdalin: discharging saline solution after the adsorbing material is adsorbed and saturated, taking out the adsorbing material, soaking the adsorbing material in 60-80% ethanol solution, stirring, eluting and resolving, adding 90-95% ethanol solution into the obtained eluent for repeated crystallization, then carrying out vacuum concentration on the obtained crystallized solution until the vacuum degree is 60kPa (the water content is less than or equal to 30%), carrying out vacuum freeze drying at the vacuum degree of 5Pa and the temperature of-25 ℃ to-15 ℃, and crushing the obtained freeze-dried product to obtain an amygdalin product, wherein the weight of the amygdalin product is 526.57 mg.
Example 2
A process for separating out and recovering amygdalin from mume fructus comprises:
A) taking 100 fresh green plums with uniform size and average gram weight of 25g, removing impurities, cleaning, grinding the cleaned green plums, and pricking holes on the surfaces of the green plums by using a pricking needle, wherein the holes are uniformly distributed;
B) separating out amygdalin: coating a separating-out material of amygdalin (the mixing ratio of pepper salt particles, citric acid and xylitol is respectively 2.5: 1:1, standing for 3-4 hours, then soaking the green plums with the holes in an amygdalin separating-out device, wherein the mixing volume ratio of the green plums to the saline solution is 1:1.3, the concentration of the saline solution in the separating-out device is 50%, starting a circulating pump to ensure that the flow rate of the saline solution is 8-12 mL/min, and the saline solution circularly flows for 2-3 hours;
C) adsorbing amygdalin: after the circulation flow in the precipitation device is finished, opening a valve between the precipitation device and the adsorption device, enabling the saline solution in the precipitation device to completely flow into the adsorption device, closing the valve, filling the adsorption device with an adsorption material, adopting adsorption material column chromatography to adsorb amygdalin in the saline solution, starting a circulating pump to enable the flow rate of the saline solution to be 10-15 mL/min, and enabling the saline solution to circularly flow for 2-3 hours so as to enable the adsorption material to be in saturated adsorption;
D) recovering amygdalin: discharging a saline solution after the adsorption material is saturated, taking out the adsorption material, soaking the adsorption material in a 60-80% ethanol solution, stirring, eluting and resolving, adding a 90-95% ethanol solution into the obtained eluent for repeated crystallization, performing vacuum concentration on the obtained crystallized solution until the vacuum degree is 65kPa (the water content is less than or equal to 30%), performing vacuum freeze drying at the vacuum degree of 7.5Pa and the temperature of-25 ℃ to-15 ℃, and crushing the obtained freeze-dried product to obtain an amygdalin product, wherein the weight of the amygdalin product is 527.63 mg.
Example 3
A process for separating out and recovering amygdalin from mume fructus comprises:
A) taking 100 fresh green plums with uniform size and average gram weight of 25g, removing impurities, cleaning, grinding the cleaned green plums, and pricking holes on the surfaces of the green plums by using a pricking needle, wherein the holes are uniformly distributed;
B) separating out amygdalin: coating a separating-out material of amygdalin (the mixing ratio of pepper salt particles, citric acid and xylitol is respectively 3: 1:1, standing for 3-4 hours, then soaking the green plums with the holes in an amygdalin separating-out device, wherein the mixing volume ratio of the green plums to a saline solution is 1:1.5, the concentration of the saline solution in the separating-out device is 60%, starting a circulating pump to enable the flow rate of the saline solution to be 8-12 mL/min, and enabling the saline to circularly flow for 2-3 hours;
C) adsorbing amygdalin: after the circulation flow in the precipitation device is finished, opening a valve between the precipitation device and the adsorption device, enabling the saline solution in the precipitation device to completely flow into the adsorption device, closing the valve, filling the adsorption device with an adsorption material, adopting adsorption material column chromatography to adsorb amygdalin in the saline solution, starting a circulating pump to enable the flow rate of the saline solution to be 10-15 mL/min, and enabling the saline solution to circularly flow for 2-3 hours so as to enable the adsorption material to be in saturated adsorption;
D) recovering amygdalin: discharging saline solution after the adsorbing material is adsorbed and saturated, taking out the adsorbing material, soaking the adsorbing material in 60-80% ethanol solution, stirring, eluting and resolving, adding 90-95% ethanol solution into the obtained eluent for repeated crystallization, then carrying out vacuum concentration on the obtained crystallized solution until the vacuum degree is 70kPa (the water content is less than or equal to 30%), carrying out vacuum freeze drying at the vacuum degree of 10Pa and the temperature of-25 ℃ to-15 ℃, and crushing the obtained freeze-dried product to obtain an amygdalin product, wherein the weight of the amygdalin product is 524.89 mg.
The preparation method of the adsorbing material in the embodiment 1-3 comprises the following steps:
a) adding a sodium chloride aqueous solution into a reaction kettle, heating to 45 ℃, mixing components of styrene, propylene organic matters, tea stem powder (the particle size of the powder is about 100 mu m), a pore-forming agent of methylcyclopropane, an initiator of phthaloyl peroxide and a catalyst of zinc chloride, stirring for 10-15min at 45 ℃, adding into the reaction kettle, stirring uniformly, heating the reaction kettle to 65 ℃ at the speed of 2-3 ℃/min, preserving heat for 3-4 hours, heating to 80 ℃ at the speed of 1 ℃/min, preserving heat for 3-5 hours, and cooling to obtain a white gray ball;
b) putting the white-gray balls into a washing kettle for washing, then sending the white-gray balls into a dryer for drying, and screening the white-gray balls with qualified particle size after drying;
c) adding appropriate amount of styrene, propylene organic matters and tea stem powder into the white gray ball obtained in the step b), stirring for 30min, adding appropriate amount of pore-forming agent, initiator and catalyst, stirring and mixing for 10-15min at 45 ℃ to obtain a mixed raw material; adding a sodium chloride solution into a reaction kettle, heating to 45 ℃, adding the mixed raw materials, uniformly stirring, heating to 65 ℃ at the speed of 2-3 ℃/min, preserving heat for 3-4 hours, then heating to 80 ℃ at the speed of 1 ℃/min, preserving heat for 3-5 hours, and cooling to obtain resin balls;
d) washing the resin balls obtained in the step c) by using ethanol, then washing with water, then drying in a dryer, and obtaining the adsorbing material after drying;
the acrylic organic matter comprises acrylonitrile, methyl acrylate and acrylamide;
according to the mass fraction, the styrene accounts for 30-35%, the propylene organic matter accounts for 8-15%, the tea stem powder accounts for 5-10%, the pore-forming agent accounts for 0.5-1%, the initiator accounts for 10-15%, and the catalyst accounts for 1-5%.
1. Evaluating the precipitation effect of the precipitation material on amygdalin in green plums
Based on example 3, 7 control groups are arranged on the precipitated material, other conditions are not changed, the comparative example 1 is a blank control, the precipitated material is not coated, and the step B) is to immerse the green plums with holes in saline water, soak for 10 hours and dissolve out amygdalin;
the precipitated material of comparative example 2 is a mixture of salt and pepper particles and citric acid 3:1, and other steps are not changed;
the precipitated material of comparative example 3 is a mixture of salt and pepper granules and xylitol 3:1, and other steps are not changed;
the precipitated material of comparative example 4 was a mixture of citric acid and xylitol in a ratio of 1:1, with the other steps unchanged;
the precipitated material of comparative example 5 was spiced salt granules, and the other steps were unchanged;
the precipitated material of comparative example 6 was citric acid, and the other steps were unchanged;
the precipitated material of comparative example 7 was xylitol, and the other steps were unchanged.
Fresh green plums, the green plums obtained by the circulation process of the embodiments 1 to 3 and the comparative examples 1 to 7 are taken, and the nutritional ingredients before and after debittering of the green plums are detected by adopting a high performance liquid chromatography (equipped with a diode array detector or an ultraviolet detector) and a spectrophotometry method, and the results are as follows:
TABLE 1 comparison of nutritional ingredients of green plums
As can be seen from the above table, the method and system for extracting and recovering amygdalin from greengage in this embodiment helps to preserve the nutrient components in greengage, and through the data analysis of the examples and comparative examples, the extracted material is used to help to reduce the amygdalin content in greengage, and simultaneously preserve the nutrient components in greengage, and the mixture of the extracted material is not acceptable.
2. Evaluation of the adsorption effect of the adsorption material on amygdalin in the invention
Based on example 3, two sets of controls were set up according to the preparation of the adsorbent material, one set being blank control comparative example 8 (using macroporous adsorbent resin) and one set being control comparative example 9 excluding tea stem powder.
The concentrations of amygdalin obtained in steps D) of examples 1 to 3 and comparative examples 8 to 9 were measured by high performance liquid chromatography (equipped with diode array detector or uv detector), respectively, with the results as follows:
TABLE 2 changes in amygdalin concentrations
And (3) calculating the recovery rate: average content of amygdalin in fresh green plums: 51.2mg/100g, the average total content of the green plums obtained in the examples and comparative examples is 100 × 25-2500 g, that is, the total content of amygdalin in each batch of green plums is 51.2 × 25-1280 mg, and the recovery rate is the ratio of the content of amygdalin to 1280.
As can be seen from the above table, the adsorbing material used in this embodiment can effectively adsorb amygdalin substances in the solution, and the recovery rate of amygdalin can reach above 40%, compared with the two comparative examples, the tea stem powder is more conducive to amygdalin adsorption, so that the process has important reference value for the precipitation and recovery of amygdalin in green plums even from other amygdalin-containing foods, and can also realize the high-efficiency recovery of amygdalin, and improve the environmental pollution caused by the discharged water in the conventional process.
Claims (5)
1. A method for separating out and recovering amygdalin from green plums is characterized by comprising the following steps:
1) cleaning green plum and pricking;
2) separating out amygdalin: coating a precipitated material of amygdalin on the surface of the green plum with the hole, and then immersing the green plum in a saline solution;
the precipitation material is a mixture of salt and pepper particles, citric acid and xylitol, and the use ratio of the salt and pepper particles to the citric acid to the xylitol is (2-3): 1: 1;
3) adsorbing amygdalin: separating the saline solution obtained in the step 2) and adsorbing amygdalin in the saline solution by adopting an adsorbing material column chromatography;
the adsorbing material is prepared from styrene, propylene organic matters, tea stem powder, a pore-forming agent, an initiator and a catalyst;
the acrylic organic matter is selected from acrylonitrile, methyl acrylate and acrylamide;
4) recovering amygdalin: eluting and resolving the adsorption material with ethanol solution, adding ethanol solution into the obtained eluate, repeatedly crystallizing, vacuum concentrating and vacuum freeze drying to obtain lyophilized product, and pulverizing to obtain amygdalin product.
2. The method for separating out and recovering amygdalin according to claim 1, wherein the mixing volume ratio of the green plums and the saline solution in the step 2) is 1 (1-1.5).
3. The method for separating out and recovering amygdalin as claimed in claim 1, wherein in the adsorbing material of step 3), styrene accounts for 30-40% by mass, propylene organic matters account for 10-15% by mass, and tea stem powder accounts for 5-10% by mass.
4. The method for separating out and recovering amygdalin as claimed in claim 1, wherein the concentration of the former is 60 to 80% and the concentration of the latter is 90 to 95% in the ethanol solution of step 4).
5. The method for separating out and recovering amygdalin as claimed in claim 1, wherein the vacuum degree of the vacuum concentration in step 4) is 60 to 70kPa, and the vacuum degree of the vacuum freeze drying is 5 to 10 Pa.
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