CN117530443A - Preparation method of artemisia selengensis leaf microcapsule - Google Patents

Preparation method of artemisia selengensis leaf microcapsule Download PDF

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CN117530443A
CN117530443A CN202311551874.1A CN202311551874A CN117530443A CN 117530443 A CN117530443 A CN 117530443A CN 202311551874 A CN202311551874 A CN 202311551874A CN 117530443 A CN117530443 A CN 117530443A
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leaf
artemisia selengensis
solution
preparing
microcapsule
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徐晓云
向琳
吴婷
贾静茹
潘思轶
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Zhiren Wuhan Health Industry Co ltd
Huazhong Agricultural University
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Zhiren Wuhan Health Industry Co ltd
Huazhong Agricultural University
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    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
    • A23L33/10—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
    • A23L33/105—Plant extracts, their artificial duplicates or their derivatives
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L29/00—Foods or foodstuffs containing additives; Preparation or treatment thereof
    • A23L29/30—Foods or foodstuffs containing additives; Preparation or treatment thereof containing carbohydrate syrups; containing sugars; containing sugar alcohols, e.g. xylitol; containing starch hydrolysates, e.g. dextrin
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L29/00—Foods or foodstuffs containing additives; Preparation or treatment thereof
    • A23L29/30—Foods or foodstuffs containing additives; Preparation or treatment thereof containing carbohydrate syrups; containing sugars; containing sugar alcohols, e.g. xylitol; containing starch hydrolysates, e.g. dextrin
    • A23L29/35—Degradation products of starch, e.g. hydrolysates, dextrins; Enzymatically modified starches
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23P—SHAPING OR WORKING OF FOODSTUFFS, NOT FULLY COVERED BY A SINGLE OTHER SUBCLASS
    • A23P10/00—Shaping or working of foodstuffs characterised by the products
    • A23P10/30—Encapsulation of particles, e.g. foodstuff additives
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
    • A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs

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  • Chemical & Material Sciences (AREA)
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  • Polymers & Plastics (AREA)
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  • Molecular Biology (AREA)
  • Botany (AREA)
  • Mycology (AREA)
  • Medicines Containing Plant Substances (AREA)

Abstract

The invention discloses a preparation method of artemisia selengensis leaf microcapsule with XOD inhibition activity, which is characterized in that artemisia selengensis leaf is extracted and purified, most of impurities are removed, dicaffeoylquinic acid is enriched, the formability of the medicine is improved, and meanwhile, the uric acid reducing effect is improved.

Description

Preparation method of artemisia selengensis leaf microcapsule
Technical Field
The invention relates to a preparation method of artemisia selengensis leaf microcapsules, and belongs to the field of health-care foods.
Background
Chenopodium album, also called as Artemisia selengensis, artemisia rupestris, etc., has a faint scent, is a plant of Artemisia genus of Compositae family, and is rich in nutrition. Tender stems of artemisia selengensis are often consumed, and leaves thereof are often discarded as waste due to their bitter taste. The research shows that the artemisia selengensis leaf extract has XOD inhibitory activity in vitro and in vivo, has potential prevention and treatment effects on hyperuricemia and gout, and the dicaffeoylquinic acid (di-CQAs) rich in the extract is a main active ingredient which plays an active role. However, artemisia selengensis leaves are rich in flavonoids, polyphenols, volatile oils, polysaccharides and triterpenes, and di-CQAs in extracts are low in purity and have a strong bitter taste. In addition, phenolic acid compounds such as di-CQAs have poor solubility in water and are easily degraded and converted under the influence of environmental factors such as oxygen, pH and the like, so that the development of deep-processed products of artemisia selengensis leaves is limited.
Microencapsulation is an effective way of embedding protective active ingredients, can convert liquid, gas or semisolid substances into fine powder, has the advantages of masking taste, improving medicine stability, fluidity, stability and the like, and extracts and purifies artemisia selengensis leaves and prepares the artemisia selengensis leaves into microcapsules, so that the artemisia selengensis leaves can be better applied to uric acid-reducing health-care foods.
Disclosure of Invention
The invention aims to provide a artemisia selengensis leaf microcapsule which takes artemisia selengensis leaves as a main raw material, improves formability and uric acid reducing activity by extracting and purifying the artemisia selengensis leaves, improves the taste and stability of a medicine by embedding the microcapsule, and finally enables a product to exert a better uric acid reducing function.
In order to achieve the above purpose, the invention adopts the following technical scheme:
a preparation method of artemisia selengensis leaf microcapsule comprises the following steps:
(1) Pulverizing herba chenopodii leaves, extracting with water, concentrating the extractive solution to obtain coarse extractive solution of herba chenopodii leaves;
(2) Purifying the coarse extractive solution with macroporous adsorbent resin column, eluting with water, eluting with 10-50% ethanol, collecting ethanol eluate, and concentrating to obtain herba chenopodii leaf purified solution rich in dicaffeoylquinic acid;
(3) Dissolving maltodextrin and acacia in water to obtain wall material solution, swelling and hydrating the wall material solution, adding herba chenopodii leaf purified solution, stirring, homogenizing, and spray drying to obtain herba chenopodii leaf microcapsule.
Preferably, the macroporous adsorbent resin is of the type HPD 722.
Preferably, the concentration of the ethanol eluent is 20-40%.
Preferably, the mass ratio of the maltodextrin to the Arabic gum is 1:1-3.
Preferably, the mass concentration of the wall material solution is 5-12%.
Preferably, the volume ratio of the artemisia selengensis leaf purification liquid to the wall material solution is 1:2-5.
Preferably, the air inlet temperature of the spray drying is 120-180 ℃, and the feeding flow is 500-800mL/h.
Preferably, the ratio of the extracted liquid in the step (1) is 1:10-30 (g/mL), the temperature is 70-90 ℃, and the extraction time is 30-60min.
According to one embodiment of the present invention, a preferred method of preparation is as follows:
(1) Extraction of artemisia selengensis leaves
Cleaning fresh herba chenopodii leaves, drying at 60 ℃, crushing and sieving with a 80-mesh sieve to obtain herba chenopodii leaf powder, weighing herba chenopodii leaf powder, extracting with 75 ℃ water for 40min according to a feed liquid ratio of 1:20 (g/mL), carrying out suction filtration, and concentrating the filtrate by rotary evaporation for 7 times to obtain herba chenopodii leaf crude extract;
(2) Purifying the extract
Loading HPD722 macroporous resin into a column, sampling the crude extract of herba chenopodii leaves, loading along the wall surface of a glass column, keeping the liquid level in the column at 2-3 cm, controlling a lower valve to enable the liquid to flow out at a flow rate of one drop per second, closing the valve after the loading is finished, standing for 2 hours, eluting with distilled water to remove impurities, eluting with 30% ethanol at the same flow rate when the effluent is colorless, collecting ethanol eluting components, concentrating under reduced pressure for 35 times to obtain herba chenopodii leaf purified liquid rich in di-CQAs;
(3) Preparation of microcapsules
Weighing maltodextrin and Arabic gum according to the mass ratio of 1:2, dissolving the weighed wall material in water, and uniformly stirring in a water bath at 50 ℃ until the wall material is completely dissolved to obtain a wall material solution with the total concentration of 10%; then placing the wall material solution in a refrigerator at the temperature of 4 ℃ to swell overnight so as to complete the hydration process; adding the artemisia selengensis leaf purified solution into the wall material solution according to the volume ratio of 1:3, and uniformly stirring; and finally, homogenizing the mixed solution at a high speed for 10min under 10000r/min, and then performing spray drying, wherein the air inlet temperature of the spray drying is 150 ℃, and the feeding flow is 600mL/h, so as to obtain the artemisia selengensis leaf extract microcapsule rich in di-CQAs.
The beneficial effects of the invention are as follows:
the artemisia selengensis leaves are extracted and purified, most of impurities are removed, di-CQAs are enriched, and exposed phenolic acid is more easily combined with a high polymer colloid material, so that the formability of the medicine is improved, and meanwhile, the uric acid reducing efficacy of the medicine is better exerted due to the increase of the di-CQAs content. The microcapsule prepared by the invention also has the advantages of high drug embedding rate, high yield, good XOD enzyme activity inhibition effect, good taste and stability, and the like.
Drawings
Fig. 1: particle size detection graph of microcapsules.
Fig. 2: determination of the release rate of microcapsules in simulated gastrointestinal digesta.
Fig. 3: the static saturation adsorption capacity (left) and desorption rate (right) of the di-CQAs for 6 macroporous resins are expressed as mean.+ -. Standard deviation, and the different lowercase letters in the figures represent significant differences (P < 0.05).
Fig. 4: static adsorption (left) and desorption (right) kinetics curves for di-CQA with 3 macroporous resins.
Fig. 5: the di-CQAS inclusion rates for different wall material combinations, as expressed as mean.+ -. Standard deviation, were shown with significant differences (P < 0.05) in the figures in lower case letters.
Fig. 6: the results of the microcapsule yields for the different wall material combinations are expressed as mean ± standard deviation, with different lowercase letters in the figures showing significant differences (P < 0.05).
Detailed Description
In order to facilitate understanding of the present invention, the following description of specific embodiments of the present invention will be given, but the present invention is not limited to the following examples.
Example 1 preparation and evaluation of chenopodium album leaf microcapsules
1. Preparation of the product
1. Extraction of artemisia selengensis leaves
Cleaning fresh herba chenopodii leaves, drying in oven at 60deg.C, pulverizing with high-speed pulverizer, and sieving with 80 mesh sieve to obtain herba chenopodii leaf powder. Weighing herba chenopodii leaf powder, extracting with 75 deg.C distilled water at a feed liquid ratio of 1:20 (g/mL) for 40min, suction filtering, and concentrating the filtrate by rotary evaporation for 7 times to obtain herba chenopodii leaf crude extract.
2. Purifying the extract
After HPD722 type macroporous resin column is filled, the coarse extract of artemisia selengensis leaves which are subjected to filtration or centrifugation is sampled, the sample is added along the wall surface of a glass column, the liquid level in the column is kept at 2-3 cm, a valve is controlled to enable the liquid to flow out at the flow rate of about one drop per second, and when the effluent begins to leak, the sample is stopped. Closing the valve and standing for about 2 hours. Eluting with distilled water to remove soluble saccharide and protein, washing until the effluent is colorless, eluting with 30% ethanol at the same flow rate, collecting ethanol eluate, and concentrating under reduced pressure for 35 times to obtain herba chenopodii leaf extract rich in di-CQAs.
3. Preparation of microcapsules
Weighing maltodextrin and Arabic gum according to the mass ratio of 1:2, dissolving the weighed wall material in distilled water, and uniformly stirring in a water bath at 50 ℃ until the wall material is completely dissolved to obtain a wall material solution with the total concentration of 10%; then placing the wall material solution in a refrigerator at the temperature of 4 ℃ to swell overnight so as to complete the hydration process; adding the purified extracting solution into the wall material solution according to the volume ratio of 1:3, and uniformly stirring; and finally, homogenizing the mixed solution at a high speed for 10min under 10000r/min, and then performing spray drying, wherein the air inlet temperature of the spray drying is 150 ℃, and the feeding flow is 600mL/h, so as to obtain the artemisia selengensis leaf extract microcapsule rich in di-CQAs.
2. Product inspection and performance evaluation
1. Particle size detection
As shown in the microcapsule scanning electron microscope chart of FIG. 1, the average particle size of the prepared microcapsules is 6.26 μm and the microcapsules are uniformly distributed.
2. Evaluation of the embedding Effect of di-CQAs
And performing qualitative and quantitative analysis on the di-CQAs by adopting an ultra-high performance liquid chromatography. Chromatographic column: ACQUITYHSS T3.8 μm (2.1X100 mm Column); column temperature: 25 ℃, flow rate: 0.2mL/min. Mobile phase: 0.1% (volume fraction) formic acid/water a and acetonitrile B. The elution method comprises the following steps: 0-1 min,10% B; 1-4 min,15% B; 4-5 min,18% B; 5-18 min,18% B; 18-19 min,50% B; 19-21 min,80% B; 21-23 min,10% B; 23-25 min,10% B. Detection wavelength: 325nm, sample injection volume: 2. Mu.L. The microcapsule powder is prepared into a sample solution of 3mg/mL, 2mL is removed, and the sample solution is placed in a sample bottle after passing through a 0.22 mu m filter membrane.
The di-CQAs content in the microcapsules was measured to be 13.27mg/g and the entrapment rate was 95.89%.
3. In vitro XOD inhibition assay
Respectively sucking 20 mu L of sample solution to be detected into an ELISA strip, adding 100 mu L of XOD enzyme solution (0.06U/mL), placing into an ELISA reader, incubating at 37 ℃ for 2min, vibrating at intervals, adding 40 mu L of xanthine solution (1 mmol/L) into a row gun to start reaction, measuring the absorbance value of a 1-time reaction system every 10s at 295nm, detecting for 2min, taking Phosphate Buffer (PBS) as a blank control group, and calculating the inhibition rate of the sample on XOD enzyme activity according to the following formula:
wherein:
k0—change in absorbance of the blank group;
k1-change of absorbance value of the reaction system of the sample to be detected.
And weighing a proper amount of microcapsules to prepare a sample to be tested of 25mg/mL, wherein the in-vitro XOD inhibition rate of the microcapsules is 40.70%.
4. Evaluation of in vitro simulated digestion effect
Preparation of simulated gastric fluid: 1.44g of pepsin is accurately weighed, and 20mL of 0.01mol/L HCl solution is added to obtain the simulated gastric digestion working solution. Preparation of simulated intestinal juice: 4g of NaCl, 0.1g of KCl, 575mg of disodium hydrogen phosphate dodecahydrate and 0.1g of potassium dihydrogen phosphate are weighed, dissolved in distilled water and fixed to 500mL, and the pH is adjusted to 7.4 by 1mol/LNaOH to obtain a phosphate buffer solution. Then, 40mg of cholic acid was weighed and 20mL of phosphate buffer solution was added to obtain a bile salt solution. 400mg of trypsin is weighed, and 40mL of phosphate buffer solution is added to obtain the simulated small intestine digestion working solution. The simulated digestive juice needs to be prepared at present, and is put into a refrigerator at 4 ℃ for standby after the preparation is finished.
The release characteristics of the core material in vivo were determined by in vitro simulated gastrointestinal digestion using the prepared microcapsules as subjects, and the results are shown in fig. 2.
As can be seen from the figure, the di-CQAs microcapsules released at the simulated gastric juice digestion stage tend to stabilize after increasing, and the cumulative release rate is low, which may be released by the core material not embedded during the microcapsule preparation process. On the other hand, the di-CQAs are not easy to crack in the acidic gastric juice environment because the di-CQAs are covalently connected with the high polymer colloid materials in the wall materials, thereby preventing the release of the di-CQAs by gastric juice. The release rate of the purified sample without embedding in acidic gastric juice is continuously increased, and the release rate reaches 84.04% after 120 min. In the intestinal juice digestion stage, the release rate of the microcapsule is rapidly increased to 73.47% after 280min, probably because the solubility of the wall material is improved in the neutral caustic environment, and di-CQAs are broken by covalent bonds, so that the medicine is released more rapidly. From the above, the release rate of di-CQAs in the microcapsule in gastric juice is low, and the release rate in intestinal juice is obviously increased, which indicates that the wall material plays a role in protecting the core material, can realize the effect of slow release of intestinal tracts, and is beneficial to more medicines to be absorbed and metabolized in vivo.
5. Sensory evaluation
Sensory evaluation was performed according to national standards (GB/T15038-2006) and ISO 4121. Before evaluation, the sensory evaluation person uses distilled water to rinse the mouth, and 2-3 mL of the sample solution is kept in the mouth for 20s, so that the sample solution is fully dispersed in the whole oral cavity, the root part of the tongue is mainly enabled to feel the bitter taste of the sample, and the mouth is rinsed by the distilled water after the bitter taste is spitted. A rest interval of 5-10 min is arranged between every two samples, and the other sample is continuously evaluated after no bitter taste exists in the oral cavity. The bitterness value was classified into five classes. The evaluator determines the bitter degree level of the sample according to the taste feeling of the evaluator, gives a specific bitter degree value, and records the specific bitter degree value in a pre-designed bitter degree evaluation table. And determining the bitter value of different samples according to the bitter value measuring method by adopting the average score as the bitter value.
By purifying and embedding the artemisia selengensis leaf extract, the bitter taste of the product is reduced and the mouthfeel is improved, and the results are shown in table 1.
Table 1 results of sensory evaluation of different samples
Sample of Bitter value
Crude extract 4.08±0.57 a
Purified product 3.68±0.69 b
Microcapsule 1.15±0.12 c
6. Stability evaluation
The prepared microcapsules were placed in an incubator at 40 ℃ ± 2 ℃ and 75% ± 5% humidity for 6 months, periodically sampled to detect di-CQAs content, and the retention rate was calculated from the initial content, and the results are shown in table 2. The di-CQAs are unstable in chemical properties and have a significant tendency to degrade during storage, while the stability of the di-CQAs is improved by microencapsulation.
TABLE 2 stability test of microcapsules
Di-CQAS retention rate 1 month 3 months of 6 months of
Microcapsule 94.75％ 92.66％ 89.68％
Unencapsulated 92.84％ 81.25％ 74.39％
EXAMPLE 2 macroporous resin purification Process screening test
1. Screening of resin types
And (3) measuring the static saturated adsorption quantity and the desorption rate of the macroporous adsorption resin:
(1) Accurately weighing 2g of the pretreated resin into 50mL conical flasks, respectively adding 20mL of artemisia selengensis leaf crude extract (prepared according to the method of example 1) into each conical flask, sealing a bottle mouth by using a preservative film, carrying out constant-temperature static adsorption for 12h under the conditions of 25 ℃ and 120r/min of a water bath shaking table, carrying out suction filtration, and storing filtrate in a 10mL centrifuge tube (marked as filtrate after adsorption) and storing at 4 ℃.
(2) Washing the surface of the macroporous adsorption resin with distilled water respectively (shaking for 2-3 times), suction-filtering to remove surface moisture, placing in a conical flask, accurately adding 20mL of ethanol with 95% volume fraction, performing constant-temperature desorption for 12h at the temperature of 120r/min on a water bath table 25 ℃, suction-filtering, storing filtrate in a 10mL centrifuge tube (marked as "desorbed filtrate"), and storing at 4 ℃.
(3) The saturated adsorption and desorption rates of the different resins were calculated by taking the appropriate "filtrate after adsorption" and "filtrate after desorption" and measuring the content of di-CQAs, and the results are shown in FIG. 3.
The saturated adsorption amount reflects the adsorption capacity of the resin, and the desorption rate reflects the desorption capacity, and it can be seen from the figure that the AB-8 resin has the maximum saturated adsorption amount to di-CQAs, but the desorption rate is smaller. If a resin has a strong adsorption capacity for a target compound, but elution is difficult, the yield of the product is reduced, so that comprehensive judgment is required from the aspects of adsorption capacity and desorption capacity of the resin. The saturated adsorption capacity and desorption rate of the three resins HPD100, HPD600 and HPD722 are high. Therefore, three types of resins of HPD100, HPD600, and HPD722 were selected for the next experiments.
And (3) carrying out static adsorption and desorption kinetic experiments on macroporous adsorption resin:
(1) The preliminary screened HPD100, HPD600 and HPD722 resins are subjected to static adsorption and desorption kinetics experiments. Accurately weighing 2g of 3 kinds of pretreated resins respectively in 50mL conical flasks, respectively adding 20mL of artemisia selengensis leaf crude extract (prepared according to the method of example 1) into each conical flask, sealing a bottle mouth by using a preservative film, carrying out constant-temperature static adsorption for 12h under the conditions of a water bath shaking table of 25 ℃ and 120r/min, respectively extracting 0.5mL of solution at 0, 0.5, 1, 1.5, 2, 3, 5, 7, 9 and 12h, and storing the solution in a 1.5mL centrifuge tube (marked as filtrate after adsorption), and storing at 4 ℃.
(2) Washing the surface of the macroporous adsorption resin which is adsorbed and saturated by distilled water (shaking for 2-3 times), suction filtering to dry the surface water, placing the surface water into a conical flask, accurately adding 20mL of ethanol with the volume fraction of 95%, desorbing the surface water for 12h at a constant temperature of 120r/min on a water bath shaking table at 25 ℃, extracting 0.5mL of solution at 0.5, 1, 1.5, 2, 3, 5, 7, 9 and 12h respectively, storing the solution in a 1.5mL centrifuge tube (marked as "desorbed filtrate"), and storing the solution at 4 ℃.
(3) The "filtrate after adsorption" and "filtrate after desorption" in each period were taken, the di-CQAs content was measured, the saturated adsorption amount and desorption rate thereof were calculated with the di-CQAs content, and the static adsorption kinetics curve and the static desorption kinetics curve were drawn with the detection time as the abscissa, and the results are shown in FIG. 4.
As can be seen from the adsorption kinetics curve (left side of FIG. 2), the adsorption of the di-CQAs by the three resins reaches saturation within 2h, and the adsorption speed is high, and the adsorption belongs to the fast equilibrium type. The adsorption capacity of the three resins to di-CQAs is rapidly increased within the first 0.5h, and after 2h, the adsorption capacity reaches equilibrium, and the saturated adsorption capacity of the three resins is about 30mg/g without obvious difference. As can be seen from the desorption kinetics curves (right of fig. 2), three resins are rapidly desorbed in the 0-0.5 h stage, and the desorption gradually reaches equilibrium after 1h, and since the desorption rate of the HPD722 resin is greater than that of the other two resins, the HPD722 resin is selected as the optimal resin for purifying di-CQAs.
2. Screening of elution solvents
After HPD722 resin is filled into a column, the crude extract of artemisia selengensis leaves which are subjected to filtration or centrifugation is sampled, the sample is added along the wall surface of a glass column, the liquid level in the column is kept at 2-3 cm, a valve is controlled to enable the liquid to flow out at the flow rate of about one drop per second, and the sample adding is stopped when the effluent begins to leak. Closing the valve and standing for about 2 hours. Eluting with distilled water to remove soluble saccharide and protein, eluting with 10%, 30% and 50% ethanol at the same flow rate, collecting different concentration ethanol eluates, concentrating herba chenopodii crude extract, 10% ethanol eluate, 30% ethanol eluate and 50% ethanol eluate under reduced pressure, and lyophilizing to obtain lyophilized powder.
The lyophilized powder was prepared into a sample solution to be tested, and the purity, yield and XOD in vitro inhibition of di-CQAs before and after purification were determined, and the results are shown in table 3.
The purity, yield and yield of the samples were calculated according to the following formula:
TABLE 3 purity, yield of di-CQAs before and after purification and XOD inhibition IC 50 Value of
Note that: different lower case letters in the same column represent significant differences (P < 0.05).
The results show that the di-CQAs of the 30% ethanol eluted component have higher purity and stronger inhibitory activity on XOD. Compared with the crude extract, the di-CQAs purity of the 30% ethanol eluted component is improved by 4.35 times. Thus, a 30% ethanol elution fraction was chosen as the eluent for macroporous resin purification.
Example 3 microcapsule preparation Process screening test
1. Screening of wall material types
The selection of microcapsule wall materials is closely related to the types of core materials, di-CQAs belong to phenolic acid compounds, and are easy to form stable combined phenolic acid through covalent connection of ester bonds and high polymer colloid materials. The different viscosity and dispersibility of the various wall materials can directly influence the embedding rate and the yield of the microcapsules. The applicant finds that a single wall material is difficult to meet the requirements of a microencapsulation process and a product through preliminary experiments, so that several commonly used microcapsule wall material combinations are selected for experiments in the experiments. The results show that the four groups of wall material combinations have good powdering property, and the products of the three groups of wall material combinations are milky white except that the products prepared by compounding maltodextrin and Arabic gum are yellowish. The maltodextrin and gum arabic combination (MD+GA) product has less wall sticking and less material loss during spray drying. The combination of Arabic gum and soy protein isolate (GA+SPI) has serious wall sticking and high product loss. The other two combinations are liable to separate layers during spray drying and unstable. To more objectively and comprehensively evaluate the properties of the wall materials, the embedding rate and the microcapsule yield were measured and calculated, and the results showed that the embedding rate of di-CQAs was higher by the combination of maltodextrin and gum arabic (MD+GA) and the combination of gum arabic and soy protein isolate (GA+SPI) (FIG. 5). The yields of maltodextrin and gum arabic combination (md+ga), maltodextrin+whey protein isolate combination (md+wpi) were higher and the yields of gum arabic+whey protein isolate combination (ga+wpi) were lower (fig. 6). After the comprehensive analysis, maltodextrin and gum arabic were selected as the optimal wall materials.
2. Optimization of process conditions
According to the pre-test result, selecting three investigation factors including wall material quality ratio, wall material quality fraction and core-wall ratio, and adopting L 9 (3 3 ) Orthogonal table orthogonal tests were performed to determine the optimal process conditions for spray drying to prepare microcapsules using di-CQAs entrapment as an indicator.
TABLE 4 level of orthogonal test factors
TABLE 5 orthogonal test design and results for microcapsules
Test number Wall material mass ratio A B wall material quality score C core to wall ratio Embedding ratio (%)
1 1 1 1 88.15±0.05
2 1 2 2 90.49±0.08
3 1 3 3 92.16±0.44
4 2 1 2 92.09±0.11
5 2 2 3 93.24±0.09
6 2 3 1 91.81±0.01
7 3 1 3 94.49±0.12
8 3 2 1 93.16±0.05
9 3 3 2 95.78±0.09
K 1 90.267 91.577 91.040
K 2 92.380 92.297 92.787
K 3 94.477 93.250 93.297
R 4.210 1.673 2.257
As can be seen from Table 5, the range R A ＞R C ＞R B The size of the effect of three factors on di-CQAs is: a is more than C and more than B, namely the proportion of the composite wall material has the greatest influence on the embedding rate, and the optimal technological parameter combination for preparing the microcapsule is A 3 B 3 C 3 Namely, the ratio of maltodextrin to Arabic gum is 1:2, the mass fraction of the wall material is 10%, and the ratio of the core material to the wall material is 1:3.

Claims (8)

1. A preparation method of artemisia selengensis leaf microcapsules is characterized by comprising the following steps:
(1) Pulverizing herba chenopodii leaves, extracting with water, concentrating the extractive solution to obtain coarse extractive solution of herba chenopodii leaves;
(2) Purifying the coarse extractive solution with macroporous adsorbent resin column, eluting with water, eluting with 10-50% ethanol, collecting ethanol eluate, and concentrating to obtain herba chenopodii leaf purified solution rich in dicaffeoylquinic acid;
(3) Dissolving maltodextrin and acacia in water to obtain wall material solution, swelling and hydrating the wall material solution, adding herba chenopodii leaf purified solution, stirring, homogenizing, and spray drying to obtain herba chenopodii leaf microcapsule.
2. The method for preparing the artemisia selengensis leaf microcapsule according to claim 1, which is characterized in that: the macroporous adsorption resin is HPD 722.
3. The method for preparing the artemisia selengensis leaf microcapsule according to claim 1, which is characterized in that: the concentration of the ethanol eluent is 20-40%.
4. The method for preparing the artemisia selengensis leaf microcapsule according to claim 1, which is characterized in that: the mass ratio of the maltodextrin to the Arabic gum is 1:1-3.
5. The method for preparing the artemisia selengensis leaf microcapsule according to claim 1, which is characterized in that: the concentration of the wall material solution is 5-12%.
6. The method for preparing the artemisia selengensis leaf microcapsule according to claim 1, which is characterized in that: the volume ratio of the artemisia selengensis leaf purifying liquid to the wall material solution is 1:2-5.
7. The method for preparing the artemisia selengensis leaf microcapsule according to claim 1, which is characterized in that: the air inlet temperature of the spray drying is 120-180 ℃, and the feeding flow is 500-800mL/h.
8. The method for preparing the artemisia selengensis leaf microcapsule according to claim 1, which is characterized in that: the ratio of the extracted liquid in the step (1) is 1:10-30 (g/mL), the temperature is 70-90 ℃, and the extraction time is 30-60min.
CN202311551874.1A 2023-11-17 2023-11-17 Preparation method of artemisia selengensis leaf microcapsule Pending CN117530443A (en)

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