CN112106989A - Sweet potato stem leaf polyphenol and extraction method thereof - Google Patents
Sweet potato stem leaf polyphenol and extraction method thereof Download PDFInfo
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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
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/88—Liliopsida (monocotyledons)
- A61K36/894—Dioscoreaceae (Yam family)
- A61K36/8945—Dioscorea, e.g. yam, Chinese yam or water yam
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
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- A61P17/16—Emollients or protectives, e.g. against radiation
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- A61P31/04—Antibacterial agents
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- A—HUMAN NECESSITIES
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- A—HUMAN NECESSITIES
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- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P39/00—General protective or antinoxious agents
- A61P39/06—Free radical scavengers or antioxidants
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- 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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Abstract
The invention relates to polyphenol of sweet potato stem leaves and an extraction method thereof. The extraction method uses ethanol water solution to carry out ultrasonic extraction on dry stem and leaf powder of the sweet potato; centrifuging the obtained extract, and collecting supernatant; and, the method further comprises: and sequentially passing the supernatant through a microfiltration membrane with the aperture of 0.22-1.2 mu m, an ultrafiltration membrane with the molecular weight cutoff of 8-12KDa and a nanofiltration membrane with the molecular weight cutoff of 400-600 Da. The polyphenol from the stem and leaf of the sweet potato prepared by the method has stronger antioxidant activity and ultraviolet resistance activity, and has higher commercial application and development values.
Description
Technical Field
The invention relates to polyphenol of sweet potato stem leaves and an extraction method thereof.
Background
Sweet potato (Ipomoea batatas Lam.) is a perennial herbaceous plant of Convolvulaceae (Convolvulaceae), also called sweet potato, etc.
The sweet potato stem and leaf is the main byproduct of sweet potato production, can be harvested 3-4 times a year, and the yield is almost the same as that of underground parts. The sweet potato stem and leaf is rich in various nutrients, can be directly eaten as fresh vegetables, and can also be used as a raw material in the food industry to be processed into various desserts, beverages, solid beverages and functional foods. At present, only a small amount of sweet potato stems and leaves are used as animal feed, and most of the sweet potato stems and leaves are directly discarded as waste, so that huge waste of resources is caused. The most main bioactive substances in the stems and leaves of the sweet potatoes are several polyphenols, are rich in content, have various physiological activities such as stronger free radical scavenging activity, metal ion chelating activity, antioxidation, anticancer, anti-mutation, bacteriostasis and the like, and are widely applied to the industries such as daily chemicals, foods, medicines and the like.
Because the crude polyphenol extract of the sweet potato stem and leaf contains some impurities, such as insoluble solid, sugar, protein and the like, how to obtain the polyphenol of the sweet potato stem and leaf with higher purity becomes a technical problem which needs to be solved urgently in the field. In addition, the polyphenol substances in the sweet potato stem and leaf comprise phenolic acids and flavonoids, the molecular weight of the polyphenol substances with single components is different from 100-1000Da, and the difficulty is increased for extracting the polyphenol from the sweet potato stem and leaf to a certain extent.
CN103393882A discloses polyphenol of sweet potato stem leaves and a preparation method thereof. The method comprises the following steps: (1) picking fresh sweet potato stem leaves, and sequentially cleaning, drying and crushing the fresh sweet potato stem leaves to obtain dry sweet potato stem leaf powder; (2) carrying out ultrasonic extraction on the dry stem and leaf powder of the sweet potato by using an ethanol water solution a; centrifuging, collecting supernatant, and removing ethanol to obtain crude polyphenol extractive solution of stem and leaf of sweet potato; (3) adjusting the total phenol concentration and the pH value of the sweet potato stem leaf polyphenol crude extract, and then pumping the sweet potato stem leaf polyphenol crude extract into macroporous adsorption resin; after adsorption, washing the macroporous adsorption resin with water, desorbing the macroporous adsorption resin with ethanol water solution b, collecting desorption solution, and removing ethanol to obtain the adsorbent. The above method has the following defects: firstly, the organic residue is high, and the pretreatment difficulty is high; secondly, the strength is poor, the crushing is serious in the using process, and the service life is short; wide particle size distribution and poor separation effect; fourthly, the resins of the same model produced by the same production enterprise have large difference of specific surface area and functional group content among batches and poor repeatability in the purification of polyphenols.
In view of the above, the present invention is particularly proposed.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a method for extracting polyphenol from stem and leaf of sweet potato and the polyphenol from stem and leaf of sweet potato obtained by the method.
As a first object of the invention, the invention provides a method for extracting polyphenol from stem and leaf of sweet potato, so as to obviously improve the quality of the polyphenol from stem and leaf of sweet potato.
Specifically, the extraction method provided by the invention uses an ethanol water solution to carry out ultrasonic extraction on dry powder of the stem and leaf of the sweet potato; centrifuging the obtained extract, and collecting supernatant; and, the method further comprises: and sequentially passing the supernatant through a microfiltration membrane with the aperture of 0.22-1.2 mu m, an ultrafiltration membrane with the molecular weight cutoff of 8-12KDa and a nanofiltration membrane with the molecular weight cutoff of 400-600 Da.
The invention unexpectedly discovers that after the supernatant sequentially passes through a microfiltration membrane with the aperture of 0.22-1.2 mu m, an ultrafiltration membrane with the molecular weight cutoff of 8-12KDa and a nanofiltration membrane with the molecular weight cutoff of 400-600Da, the polyphenol part with stronger biological activity can be concentrated and enriched, and further the additional value of the polyphenol part is improved.
As a better technical scheme of the invention, the supernatant fluid sequentially passes through a microfiltration membrane with the aperture of 0.45 mu m, an ultrafiltration membrane with the molecular weight cutoff of 10KDa and a nanofiltration membrane with the molecular weight cutoff of 400-600 Da.
Preferably, when the operating pressure of the ultrafiltration membrane is 0.1-0.15MPa (especially 0.1MPa), the removal of macromolecular substances such as pectin and protein in the supernatant is facilitated.
Preferably, when the operating pressure of the nanofiltration membrane is 0.2-0.6MPa (especially 0.3MPa), the method is favorable for enriching the polyphenol from the stem and leaf of the sweet potato with stronger biological activity.
Preferably, the particle size of the dry powder of the stem and leaf of the sweet potato is 80-100 meshes;
further, the dry powder of the stem leaves of the sweet potato is prepared by the method comprising the following steps: cleaning, freeze drying and pulverizing the stems and leaves of the sweet potato in sequence;
furthermore, the stem and leaf of the sweet potato are taken from the part of 10-15 cm from the top of the cirrus of the sweet potato.
In the technical scheme, the sweet potato stem and leaf is preferably fresh sweet potato stem and leaf, and the picking period can be any growth stage of the sweet potato stem and leaf, such as the earlier stage of potato block harvest or the time of potato block harvest, so as to reduce the influence on the yield of the potato block.
Preferably, the mass concentration of the ethanol aqueous solution is 60-80% (especially 70%);
preferably, the feed-liquid ratio of the dry powder of the stem and leaf of the sweet potato to the aqueous solution of ethanol is 1 g: 10-30 mL; wherein, 1 g: 20mL is particularly preferred.
In the technical scheme, the ethanol aqueous solution and the dry sweet potato stem leaf powder are mixed according to the material-liquid ratio, so that the ethanol aqueous solution and the dry sweet potato stem leaf powder can be fully mixed and contacted, and the dissolution of polyphenol substances is further improved.
Preferably, the ultrasonic leaching time is 20-50 min; preferably 30 min; furthermore, the power of the ultrasonic wave is controlled to be 450-500W. The invention discovers that the introduction of ultrasonic treatment not only greatly shortens the soaking time, but also unexpectedly and obviously changes the combination state of active ingredients in the dry powder of the stem and leaf of the sweet potato (mainly the ideal intervention on cell walls), and promotes the full dissolution of polyphenol substances.
Preferably, the centrifugation is carried out for 10-15 min at the rotating speed of 4000-7500 r, and particularly for 10min at the rotating speed of 7500 r; under the conditions, the related impurities generated by centrifugation can be more adsorbed on the solid matters, so that the subsequent purification is facilitated.
Preferably, the method further comprises the step of carrying out ultrasonic leaching on the residue after centrifugation for 1-3 times so as to ensure that all polyphenol substances are dissolved out to the maximum extent.
The extraction method provided by the invention has the advantages of simple process, high extraction efficiency and less loss of active ingredients, and the biological activity of the polyphenol of the stem leaves of the sweet potatoes is obviously higher than that of the prior art.
In the prior art, the membrane separation process can cause the problem of membrane pollution, which leads to the reduction of membrane flux, the reduction of production efficiency, the loss of key components and the like. Based on the method, the method also comprises the following steps of cleaning the ultrafiltration membrane and the nanofiltration membrane:
and sequentially cleaning the ultrafiltration membrane and the nanofiltration membrane by respectively adopting deionized water, 0.08-0.12% of HCl, 0.08-0.12% of NaOH and deionized water until the effluent liquid is neutral.
The ultrafiltration membrane and the nanofiltration membrane are cleaned by adopting the mode, so that the membrane flux can be recovered to a higher level, and the defects of the existing membrane separation technology in the using process are overcome.
In the technical scheme, the deionized water is used for washing for the second time until the effluent penetrating fluid is neutral, and the pH value can be measured by using disposable pH test paper.
Preferably, the cleaning time of the first deionized water is 0.5-2 h; preferably 1 h;
preferably, the cleaning time of 0.08-0.12% HCl is 0.5-2 h; preferably 1 h;
preferably, the cleaning time of 0.08-0.12% NaOH is 0.5-2 h; preferably 1 h.
In the invention, the method for cleaning the ultrafiltration membrane and the nanofiltration membrane can be used independently.
As a second object of the present invention, there is provided a sweet potato stem leaf polyphenol, which is produced by the above method.
The invention has the beneficial effects that:
(1) the extraction method is simple to operate, has low energy consumption, and can realize large-scale industrial production;
(2) the reagents, materials and instruments used by the method are all in common specifications, the production cost is low, and the method is non-toxic and environment-friendly;
(3) the polyphenol from the stem and leaf of the sweet potato prepared by the method has stronger antioxidant activity and ultraviolet resistance activity, and has higher commercial application and development values.
(4) The method has the advantages of convenient cleaning of the used equipment and long-term recycling.
Drawings
FIG. 1 is a flow chart of an ultrafiltration/nanofiltration membrane module apparatus according to example 5;
in the figure: 1. a raw material liquid tank; 2. an infusion pump; 3. a pressure gauge; 4. an ultrafiltration/nanofiltration assembly; 5. a flow meter; 6. a circulation valve; 7. a concentrate valve; 8. a flow meter valve.
FIG. 2 is a graph showing the change in membrane flux during ultrafiltration and 400-600Da nanofiltration in example 5.
Detailed Description
The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention.
Example 1: rejection rate of ultrafiltration membrane and nanofiltration membrane on polyphenol
(1) Collecting and pretreating raw materials: the stem and leaf of the sweet potato are picked in 11-month middle ten days, and the picking part is 10cm from the top end of the vine. Cleaning fresh sweet potato stem leaves, draining, pre-freezing in a refrigerator at-40 ℃ for 24h, taking out, putting into a freeze dryer, drying for 72h, and pulverizing with a universal pulverizer to obtain dry sweet potato stem leaf powder as the following experimental raw materials;
(2) crude extraction of polyphenol: weighing 10g of dry sweet potato stem leaf powder in the step (1), and mixing the dry sweet potato stem leaf powder with the feed-liquid ratio of 1: adding 200mL of 70% ethanol aqueous solution into 20, mixing, performing ultrasonic extraction in an ultrasonic cleaning machine for 30min, centrifuging for 10min at 7500r after extraction, collecting supernatant, extracting residues twice, mixing supernatants, and performing rotary evaporation to remove ethanol to obtain crude polyphenol extractive solution of stem and leaf of sweet potato;
(3) passing the crude polyphenol extract from stem and leaf of sweet potato through a 0.45 μm organic microfiltration membrane to obtain an ultrafiltration stock solution with a volume of 600 mL;
(4) passing the solution obtained in the step (3) through a 10KDa ultrafiltration membrane until the volume of the trapped fluid is 100mL, and the volume of the ultrafiltration penetrating fluid is 500 mL; the operating pressure is 0.1 MPa;
(5) the ultrafiltration penetrating fluid in the step (4) is respectively used as nanofiltration stock solutions of 200-; the operating pressure was 0.3 MPa.
(6) The Folin-Ciocalteu colorimetric method is adopted to determine the total phenol concentration in the ultrafiltration sample solution: 0.5mL of the solution to be measured, 1.0mL of Folin-Ciocalteu reagent diluted by 10 times, reacting at 30 ℃ for 30min, adding 10% (w/v) of sodium carbonate solution, reacting at 30 ℃ for 30min, and measuring the absorbance at 736 nm.
VRF＝V0/V R ①
In the formula: VRF is volume concentration times;
V0volume of solution before ultrafiltration, mL;
VRthe volume of the ultrafiltration retentate is mL;
retention rate R (%) - (1-C)P/Cf)×100 ②
In the formula: cPThe concentration of the substance in the permeate, μ g/mL;
Cfthe concentration of the substance in the raw material liquid is [ mu ] g/mL;
the results are shown in Table 1, and it is clear that the retention rate of polyphenol from sweet potato stem leaves by the ultrafiltration membrane is low. The rejection rate of the nanofiltration membrane on the polyphenol of the stem and leaf of the sweet potato is higher, and the rejection rate of the nanofiltration membrane on the polyphenol of the stem and leaf of the sweet potato is increased along with the increase of the molecular weight cut off by the nanofiltration membrane. This is because the ultrafiltration membrane has a large pore size and a cut-off molecular weight of 10Kda, and therefore substances having a molecular weight of < 10KDa can pass through. The aperture of the nanofiltration membrane is smaller, so that the rejection rate of the polyphenol is higher.
TABLE 1 rejection of polyphenols by ultrafiltration and nanofiltration membranes
Example 2: concentration of polyphenols in ultrafiltration and nanofiltration components of different cut-off molecular weights
The total phenol content of the sample solution of each step of example 1 was determined by Folin-Ciocalteu colorimetry: 0.5mL of the solution to be measured, 1.0mL of Folin-Ciocalteu reagent diluted by 10 times, reacting at 30 ℃ for 30min, adding 10% (w/v) of sodium carbonate solution, reacting at 30 ℃ for 30min, and measuring the absorbance at 736 nm.
Establishing a standard curve with chlorogenic acid standard substance in the range of 0-0.1mg/mL to obtain a regression equationIs Y-8.7671X +0.0068, R2＝0.9994。
According to the standard curve, the absorbance photometric value is measured at 736nm from the sample solution to obtain the total phenol content of the sample solution, which is expressed as the equivalent concentration of chlorogenic acid in mg CAE/mL.
The results are shown in Table 2, and it can be seen from the results that the polyphenol of the stem and leaf of sweet potato is maximally enriched in the 400-plus 600Da nanofiltration membrane retentate, and the concentration of the polyphenol in the part is the highest and reaches 837.5 μ g CAE/mL, which is 2 times higher than that in the initial solution.
TABLE 2 Polyphenol concentrations of different ultrafiltration/nanofiltration components
Example 3: antioxidant activity of ultrafiltration and nanofiltration components of different cut-off molecular weights
The antioxidant activity in the sample solution of each step of example 1 was measured by the FRAP method. The preparation of the FRAP solution comprises the following steps: 10mmol/L TPTZ solution and 20mmol/L FeCl3The solution and 300mM acetic acid buffer solution (pH 3.6) were mixed in a volume ratio of 1: 1: 10, mixing well, placing in a water bath kettle at 37 ℃, and keeping the temperature for 30min to prepare the FRAP solution. Preparing the polyphenol crude extract of each part of the samples into solution with the same mass concentration by using distilled water, taking 0.15mL of sample solution, adding 2.85mL of FRAP solution, reacting for 30min in a dark place at room temperature, and immediately measuring the light absorption value at 593 nm. Distilled water was used as a blank instead of the sample. Establishing a standard curve by using water-soluble vitamin E standard substances with the concentrations of 10, 20, 50, 70, 100 and 200 mu g/mL to obtain a linear regression equation y of 0.0029x +0.017, wherein R is20.9918. The ferric ion reduction activity of the sample solution was expressed as μ g water-soluble vitamin E equivalent (TE) per mL of the sample solution.
The results are shown in Table 3, and it can be known that the 400-Da nanofiltration trapped fluid part has the strongest antioxidant activity, and the antioxidant activity is as high as 80.08 mu g TE/mL.
TABLE 3 antioxidant Activity of different Ultrafiltration/nanofiltration Components
Example 4: anti-UV Activity of different Ultrafiltration/nanofiltration Components
The sun Protection factor spf (sun Protection factor) of the sample solution of each step of example 1 was determined by in vitro uv spectrophotometry. Each sample was diluted to the same concentration. And (3) measuring the absorbance every 5nm by using an ultraviolet spectrophotometer within the wavelength range of 290-320 nm, and taking distilled water as a blank control. Ascorbic acid was used as a positive control. The Mansur equation was applied to calculate SPF.
In the formula: CF is the correction factor, 10; i (lambda) is the solar spectral intensity; EE (λ) is the erythematous effect of radiation at wavelength λ; abs (λ) is absorbance at wavelength λ; EE (λ). times.I (λ) are constants, determined by Sayre et al; the values of EE (λ) × I at different wavelengths were 290nm, 0.0150, respectively; 295nm, 0.0817; 300nm, 0.2874, 305nm, 0.3278; 310nm, 0.1864; 315nm, 0.0837; 320nm, 0.0180.
The results are shown in Table 4, and it can be seen that the part with the strongest anti-UV activity is 400-Da nanofiltration retentate, and the SPF value is 10.37. Group of ascorbic acid higher than positive control.
TABLE 4 anti-UV Activity of different Ultrafiltration/nanofiltration Components
Example 5: change of membrane flux and cleaning efficiency in ultrafiltration membrane and 400-plus-600 Da nanofiltration membrane processes
As shown in fig. 1, steps (4) and (5) in example 1 can be performed in an ultrafiltration/nanofiltration membrane module device;
the membrane flux of deionized water was taken as the initial flux. The volume of the sample penetrating fluid is recorded every 5 minutes in the membrane separation process, the membrane flux is calculated according to a formula (IV) and a membrane flux change curve is drawn, and the figure 2 shows.
And the cleaning step after the membrane separation is that firstly deionized water is used for cleaning for 1h, then 0.1% HCl is used for cleaning for 30min, then 0.1% NaOH is used for cleaning for 30min, and finally deionized water is used for cleaning until the effluent penetrating fluid is detected to be neutral by pH test paper. And measuring the membrane flux of the deionized water again after the cleaning is finished, and calculating the membrane flux fraction according to a formula.
Membrane flux J ═ Δ V/(A)m×t) ④
In the formula: j is the membrane flux, L/(m)2·h)；
Δ V is the volume of permeate collected, L;
am is the effective membrane area, m2；
t is time, h.
Membrane flux fraction I ═ J1/J 0 ⑤
In the formula: j. the design is a square1For initial flux, L/m2h；
J0For the membrane flux after washing, L/m2h。
As can be seen from fig. 2, as the membrane separation proceeds, the membrane flux of both ultrafiltration and nanofiltration gradually decreases. The possible reason is that the filter membrane shows an adsorption effect on polyphenols during filtration, and the flow resistance to the solvent increases with time, and thus the flux decreases. As can be seen from Table 5, the membrane flux of the ultrafiltration membrane is recovered to 89.24% of the initial flux after cleaning, and the membrane flux of the 400-Da nanofiltration membrane is recovered to 98% of the initial flux after cleaning. The flux of the ultrafiltration and nanofiltration membranes is recovered to be more than 80% of the initial flux, which shows that the cleaning method is convenient and effective and can ensure that the filter membranes can be repeatedly used for a long time.
TABLE 5 Membrane flux fractions after ultra/nanofiltration membrane washing
Example 6: preparation of polyphenol from stem and leaf of Typha angustifolia 53 sweet potato
(1) Collecting raw materials: picking up leaves and leaves of Ipomoea batatas Lam No. 53 in the middle ten days of 11 months, wherein the picking part is 15cm away from the top end of the vines;
(2) pretreatment: cleaning fresh Ipomoea batatas Lam No. 53 sweet potato stem and leaf, draining, placing into tray, pre-freezing at-40 deg.C for 24 hr, taking out, placing into freeze drier, drying for 72 hr, and pulverizing with universal pulverizer to obtain dry powder of sweet potato stem and leaf;
(3) extracting polyphenol: taking the dry powder of the stem leaves of the sweet potatoes in the step (2), and mixing the dry powder according to a material-liquid ratio of 1: adding 70% ethanol water solution into 20, mixing, ultrasonic extracting in ultrasonic cleaning machine for 30min, centrifuging at 7500r for 10min, collecting supernatant, extracting residue for 2 times, and mixing supernatants.
(4) Filtering the supernatant from step (3) with a 0.45 μm microfiltration membrane to remove solid particles and insoluble impurities. Ultrafiltering the micro filtrate with 10KDa ultrafiltering membrane at 0.1MPa and room temperature. The ultrafiltration permeate is passed through a 400-Da nanofiltration membrane at the room temperature, and the operating pressure is 0.3 MPa. Retaining nanofiltration penetrating fluid, removing ethanol by rotary evaporation at 50 ℃, pre-freezing at-40 ℃ for 24 hours, and then performing freeze drying for 72 hours to obtain pure polyphenol products from stem leaves of the Ipomoea batatas 53 sweet potatoes.
Carrying out quantitative analysis on the polyphenol of the stem leaves of the Ipomoea batatas 53 Ipomoea batatas Lam by adopting high performance liquid chromatography; the specific method comprises the following steps:
dissolving the obtained polyphenol from stem and leaf of Ipomoea batatas 53 sweet potato in 80% methanol to obtain 200 μ g/mL sample solution, and performing chromatographic analysis after passing through 0.45 μm membrane under the following chromatographic conditions: ZORBAX Eclips Plus C18 chromatography column (4.6X 150mm, 5 μm), detection wavelength 326nm, flow rate 1min/mL, sample size 20 μ L, column temperature 30 ℃, mobile phase A: 0.5% (w/v) phosphoric acid solution, B: and (3) acetonitrile. Gradient elution procedure: 0-15 min: 20-65% B; 15-15.1 min: 65-80% B; 15.1-20 min: 80% of B. The results of quantitative analysis of each component in the sample based on the retention time and peak area of each absorption peak in the sample absorption spectrum are shown in table 6. Therefore, the polyphenol content of the stem leaves of the Ipomoea batatas Lam 53 is 59.02%.
TABLE 6 polyphenol component of sweet potato stem and leaf and composition
Although the invention has been described in detail hereinabove by way of general description, specific embodiments and experiments, it will be apparent to those skilled in the art that many modifications and improvements can be made thereto based on the invention. Accordingly, such modifications and improvements are intended to be within the scope of the invention as claimed.
Claims (10)
1. An extraction method of polyphenol from stem and leaf of sweet potato comprises ultrasonic extracting dry stem and leaf of sweet potato with ethanol water solution; centrifuging the obtained extract, and collecting supernatant; characterized in that the method further comprises: and sequentially passing the supernatant through a microfiltration membrane with the aperture of 0.22-1.2 mu m, an ultrafiltration membrane with the molecular weight cutoff of 8-12KDa and a nanofiltration membrane with the molecular weight cutoff of 400-600 Da.
2. The extraction process according to claim 1, wherein the operating pressure of the ultrafiltration membrane is 0.1 to 0.15 MPa.
3. The extraction process according to claim 1 or 2, wherein the operating pressure of the nanofiltration membrane is 0.2-0.6 MPa.
4. The extraction method according to claim 1, wherein the particle size of the dry powder of the stem and leaf of the sweet potato is 80-100 meshes;
preferably, the dry powder of the stem and leaf of the sweet potato is prepared by a method comprising the following steps: cleaning, freeze drying and pulverizing the stems and leaves of the sweet potato in sequence;
more preferably, the stem and leaf of the sweet potato are taken from the part of 10-15 cm from the top of the cirrus of the sweet potato.
5. The extraction method according to claim 1 or 4, wherein the mass concentration of the ethanol aqueous solution is 60-80%;
and/or the feed-liquid ratio of the dry sweet potato stem leaf powder to the ethanol water solution is 1 g: 10-30 mL.
6. The extraction method according to claim 5, wherein the ultrasonic leaching time is 20-50 min;
and/or centrifuging for 10-15 min at the rotating speed of 4000-7500 r.
7. The extraction method according to claim 1, further comprising the step of subjecting the centrifuged residue to ultrasonic leaching 1-3 times.
8. The extraction process according to claim 1, characterized in that it further comprises a step of washing the ultrafiltration membrane and the nanofiltration membrane:
and sequentially cleaning the ultrafiltration membrane and the nanofiltration membrane by respectively adopting deionized water, 0.08-0.12% of HCl, 0.08-0.12% of NaOH and deionized water until the effluent liquid is neutral.
9. The extraction process according to claim 8, wherein the first deionized water wash time is 0.5-2 hours;
and/or the cleaning time of 0.08-0.12% HCl is 0.5-2 h;
and/or the cleaning time of 0.08-0.12% NaOH is 0.5-2 h.
10. A polyphenol from stem and leaf of sweet potato, characterized by being produced by the method as claimed in any one of claims 1 to 9.
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