CN109007834A - A kind of Fructus psidii guajavae immaturus leaf extract cyclodextrin inclusion compound and the preparation method and application thereof - Google Patents
A kind of Fructus psidii guajavae immaturus leaf extract cyclodextrin inclusion compound and the preparation method and application thereof Download PDFInfo
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- CN109007834A CN109007834A CN201811012587.2A CN201811012587A CN109007834A CN 109007834 A CN109007834 A CN 109007834A CN 201811012587 A CN201811012587 A CN 201811012587A CN 109007834 A CN109007834 A CN 109007834A
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- China
- Prior art keywords
- cyclodextrin
- leaf extract
- psidii guajavae
- fructus psidii
- guajavae immaturus
- Prior art date
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Classifications
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- 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
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
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- 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
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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
- A23L5/00—Preparation or treatment of foods or foodstuffs, in general; Food or foodstuffs obtained thereby; Materials therefor
- A23L5/30—Physical treatment, e.g. electrical or magnetic means, wave energy or irradiation
- A23L5/32—Physical treatment, e.g. electrical or magnetic means, wave energy or irradiation using phonon wave energy, e.g. sound or ultrasonic waves
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- 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
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- 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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- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Food Science & Technology (AREA)
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Abstract
The invention discloses a kind of Fructus psidii guajavae immaturus leaf extract cyclodextrin inclusion compounds and the preparation method and application thereof.The present invention is by the way that by Fructus psidii guajavae immaturus and/or leaf, after extracting, vacuum concentration, concentrate is included using cyclodextrin, is filtered, and drying and crushing obtains Fructus psidii guajavae immaturus leaf extract cyclodextrin inclusion compound.The Fructus psidii guajavae immaturus leaf extract cyclodextrin inclusion compound can cover fruit/leaf bitter taste, increase the water solubility of the functional components such as flavones, polyphenol in extract, inclusion compound stabilization is not oxidizable, it is easily absorbed by the human body, the solid-state granules beverage and preparation of preparation are convenient, mouthfeel is various, with Fructus psidii guajavae immaturus/leaf anti diar rhea, antidiabetic function ingredient, it is the healthy food for being suitble to related sub-health population or patient, has a good application prospect.
Description
Technical field
The present invention relates to food processing field, in particular to a kind of Fructus psidii guajavae immaturus leaf extract cyclodextrin inclusion compound and its system
Preparation Method and application.
Background technique
Guava dry fruit and cured leaf are civil common beverage pouring and boiling materials, the general prematurity dried fruit for using guava
The cured leaf that piece, tender leaf bud or old leaf are dried.Studies have shown that Fructus psidii guajavae immaturus, leaf have terpene, flavones, polyphenol, microelement,
The healthy functions ingredient such as fiber shows positive effect at antibacterial, anti diar rhea, anticancer and hypoglycemic aspect, and has good
Therefore good inoxidizability is approved and is welcome, be widely used in South America and one band of Southeast Asia.
Fructus psidii guajavae immaturus/leaf is brewed with drying raw material as main eating method at present, still, abundant function contained therein
Ingredient, including polyphenol, flavones and terpene isoreactivity substance are water-soluble poor and unstable, and the resting period of chankings, leaf and
Condition, brewing conditions etc. will cause different degrees of influence to mouthfeel, flavor and auxiliary effect for brewing.
In recent years, cyclodextrin inclusion technique is in food and medicine using inclusion that is increasingly extensive, being formed using cyclodextrin
Object can increase its solubility and stability, and improve the physicochemical property of guest species to a certain extent, be easily absorbed by the human body, mention
The weatherability and bioavilability of high object.It also there have been no the cyclodextrin inclusion compound of Fructus psidii guajavae immaturus leaf extract currently on the market
Occur.
Summary of the invention
The primary purpose of the present invention is that the shortcomings that overcoming the prior art and deficiency, provide a kind of Fructus psidii guajavae immaturus leaf extract
The preparation method of cyclodextrin inclusion compound.
Another object of the present invention is to provide the Fructus psidii guajavae immaturus leaf extract cyclodextrin obtained by above-mentioned preparation method
Inclusion compound.
A further object of the present invention is to provide the applications of above-mentioned Fructus psidii guajavae immaturus leaf extract cyclodextrin inclusion compound.
The purpose of the invention is achieved by the following technical solution: a kind of system of Fructus psidii guajavae immaturus leaf extract cyclodextrin inclusion compound
Preparation Method includes the following steps:
(1) pretreatment of raw material: guava fruit tablet and/or leaf are cleaned and dried, is crushed；
(2) extract: the broken raw material that Extraction solvent and step (1) are obtained mixes, and extracts, is filtered to remove filter
Slag obtains extracting solution；
(3) it is concentrated by evaporation: the extracting solution that step (2) obtain being concentrated, concentrate is obtained；
(4) cyclodextrin encapsulated: cyclodextrin to be added in the concentrate that step (3) obtain, be uniformly mixed, obtain mixed liquor A；
Mixed liquor A is placed in dark place to include, is filtered, the concentrate not included is eluted, obtains filtrate；
(5) drying and crushing: the filtrate that step (4) is obtained is dry, crushes, and obtains Fructus psidii guajavae immaturus and/or leaf extract
Cyclodextrin inclusion compound.
The sodium bicarbonate aqueous solution that Extraction solvent is water, pH is 4.5 described in step (2) aqueous acetic acid, pH are 8.0
And concentration is at least one of the edible ethanol of percent by volume 40~95%；Preferably concentration is percent by volume 70%
Edible ethanol.
The water is preferably 70~100 DEG C of hot water；More preferably boiling water.
The dosage of Extraction solvent described in step (2) preferably press every 100g guava fruit tablet and/or leaf proportion 800~
1200mL Extraction solvent calculates；More preferably calculated by every 100g guava fruit tablet and/or leaf proportion 1000mL Extraction solvent.
The time of extraction described in step (2) is preferably 30~120min.
The mode of extraction described in step (2) includes ultrasonic extraction or standing extraction.
Ultrasonic power is preferably 300~400W in the ultrasonic extraction.
The mode of concentration described in step (3) includes dry, vacuum concentration；Preferably using vacuum rotary evaporator into
Row.
The degree of concentration described in step (3) is preferably concentrated into the 25~35% of extracting liquid volume.
Cyclodextrin described in step (4) is alpha-cyclodextrin, beta-cyclodextrin, gamma-cyclodextrin, hydroxypropyl-β-cyclodextrin, Portugal
One of grape saccharide ring dextrin, maltose cyclodextrin and carboxymethyl cyclodextrin or at least two；Preferably hydroxy propyl-Beta-ring paste
Essence.
The dosage of cyclodextrin described in step (4) preferably presses every 100g guava fruit tablet and/or leaf matches 10~20g
Cyclodextrin calculates.
Concentrate described in step (4) and feeding intake for cyclodextrin calculate according to mass ratio 1:1~25；Preferably 1:3~
5；More preferably 1:3.
The method of inclusion described in step (4) include polishing, supercritical ultrasonics technology, mechanical mixing method and mechanical stirring with
The method that supercritical ultrasonics technology combines；The preferably method that is combined with supercritical ultrasonics technology of mechanical stirring.
The specific steps for the method that the mechanical stirring is combined with supercritical ultrasonics technology are preferably as follows: first ultrasound inclusion, then
Stirring inclusion.
Ultrasonic power in the ultrasound inclusion is 100~200W；Preferably 120~160W.
Ultrasonic time in the ultrasound inclusion is 20~40min；Preferably 30min.
Ultrasonic temperature in the ultrasound inclusion is 25~80 DEG C；Preferably 25~35 DEG C.
Whipping temp in the stirring inclusion is preferably 20~70 DEG C；More preferably 20~60 DEG C.
Mixing speed in the stirring inclusion is 50~180rpm；Preferably 50~120；More preferably 100~
110rpm。
Mixing time in the described stirring inclusion is 5~for 24 hours；Preferably 5~10h；More preferably 6h.
The pH value of mixed liquor A is also maintained 3~10 in whipping process in the stirring inclusion；Preferably 3~5；
More preferably 3~4.
Filtering described in step (4) is preferably by 0.45~0.85 μm of water system membrane filtration；More preferably pass through
0.45 μm of water system membrane filtration.
Drying described in step (5) includes dry reduced vacuum, vacuum freeze drying and spray drying；It is optimized for cold
Freeze vacuum drying.
The step of described vacuum freeze drying, is preferably as follows: the filtrate is first cooled to 0~4 DEG C, then be refrigerated to-
20 DEG C carry out vacuum freeze drying hereinafter, being placed in vacuum freeze drier.
The degree of the freezing is preferably refrigerated to -80 DEG C.
A kind of Fructus psidii guajavae immaturus leaf extract cyclodextrin inclusion compound, is obtained by above-mentioned preparation method.
Above-mentioned Fructus psidii guajavae immaturus leaf extract cyclodextrin inclusion compound is preparing the application in anti diar rhea and blood sugar reducing food.
The dosage form of the food is preferably solid-state granules beverage or preparation.
The application, preferably includes following steps: using the Fructus psidii guajavae immaturus leaf extract cyclodextrin inclusion compound as
Raw material or addition appropriate amount of auxiliary materials, form solid-state granules beverage or tabletted, form preparation.
The present invention has the following advantages and effects with respect to the prior art:
1. the present invention selects cyclodextrin to include guava extract, fruit/leaf bitter taste can be covered, increase mentions
The water solubility of the functional components such as flavones in object, polyphenol is taken, product stabilization is not oxidizable, is easily absorbed by the human body, and has good answer
Use prospect.
2. electuary or oral preparation of the invention is convenient, mouthfeel is various, there is Fructus psidii guajavae immaturus/leaf anti diar rhea, drop blood
The functional component of sugar is a kind of healthy food for being suitble to related sub-health population or patient.
Detailed description of the invention
Fig. 1 is FTIR spectrum figure；Wherein, curve a is guava leaf extract, and curve b is hydroxy propyl-Beta-ring paste
Essence, curve c are the physical mixture of extract and hydroxypropyl-β-cyclodextrin, and curve d is the hydroxypropyl-of guava leaf extract
Benexate Hydrochloride.
Fig. 2 is thermogravimetric analysis (TGA)/difference quotient thermogravimetric analysis (DTG) figure of guava leaf extract.
Fig. 3 is guava leaf extract/hydroxypropyl-beta-cyclodextrin inclusion TGA/DTG figure.
Fig. 4 is the 1,1- diphenyl -2- trinitro- of guava leaf extract and inclusion compound under different time of ultraviolet irradiation
Phenylhydrazine (DPPH) free radical scavenging ability comparison diagram.
Fig. 5 is that the 2,2'- of guava leaf extract and inclusion compound under different time of ultraviolet irradiation joins bis- (the 3- ethylo benzenes of nitrogen
And thiazoline -6- sulfonic acid) di-ammonium salts (ABTS+) free radical scavenging ability comparison diagram.
Fig. 6 is the alpha-glucosidase rejection ability comparison diagram of Guava Leaf inclusion compound and acarbose (control).
Specific embodiment
Present invention will now be described in further detail with reference to the embodiments and the accompanying drawings, but embodiments of the present invention are unlimited
In this.
Embodiment 1
Guava Leaf 100g is weighed, cleans and dries, is broken into block, 1000mL 70% (v/v) edible ethanol is added,
30min is extracted with 300W power ultrasound, obtains extracting solution.Vacuum rotary evaporator is added in extracting solution, is concentrated by evaporation to volume
It is 30% or so of original volume, 10g hydroxypropyl-β-cyclodextrin is added, is uniformly mixed, is placed in dark place, it is continuous with 120W power
After ultrasonic 30min, 35 DEG C of ultrasonic temperature, temperature is controlled at 50 DEG C after ultrasound, with the revolving speed magnetic agitation 6h of 100rpm,
PH value of solution is adjusted in whipping process and maintains 3-4, then by 0.45 μm of water system membrane filtration, elutes the extract not included,
Filtrate is cooled to 4 DEG C, -80 DEG C of ultra low temperature freezers is put into later and continues to freeze 2h, be put into freeze drier, be freeze-dried
Night obtains the hydroxypropyl-beta-cyclodextrin inclusion dry-powder product of guava leaf extract.
Embodiment 2
Guava fruit tablet 100g is weighed, cleans and dries, is broken into block, 1000mL70% (v/v) edible ethanol is added,
30min is extracted with 300W power ultrasound, obtains extracting solution.Vacuum rotary evaporator is added in extracting solution, is concentrated by evaporation to volume
It is original 30% or so, 15g hydroxypropyl-β-cyclodextrin is added, is uniformly mixed, dark place is placed in, with 120W power continuous ultrasound
30min, controls temperature at 60 DEG C after ultrasound by 35 DEG C of ultrasonic temperature, stirred with the revolving speed magnetic agitation 6h of 100rpm
PH value of solution is adjusted in journey and maintains 3-4, then by 0.45 μm of water system membrane filtration, the extract not included is eluted, by filtrate
After being cooled to 4 DEG C, it is put into -80 DEG C of ultra low temperature freezers later and continues to freeze 2h, is put into freeze drier, lyophilized overnight,
Up to the hydroxypropyl-beta-cyclodextrin inclusion dry powder of Fructus psidii guajavae immaturus extract.
Embodiment 3
Guava fruit tablet 100g is weighed, cleans and dries, is broken into block, 100 DEG C of hot water of 1000mL are added, stands leaching
90min is mentioned, extracting solution is obtained.Vacuum rotary evaporator is added in extracting solution, being evaporated to and being concentrated into volume is a 30% original left side
10g gamma-cyclodextrin is added in the right side, is uniformly mixed, is placed in dark place, under room temperature with the revolving speed magnetic agitation of 100rpm for 24 hours after, pass through
0.45 μm of water system membrane filtration elutes the extract not included, filtrate is directly spray-dried, guava fruit tablet water is obtained
The gamma-cyclodextrin inclusion compound dry powder of extract.
The gamma-cyclodextrin inclusion compound dry powder of obtained guava fruit tablet water extract and citric acid, ammonium lacate are shone by matter
It measures the ratio than 5:2:1 to reconcile, dry, beverage granules are made in sealing pack.
Embodiment 4
Guava Leaf 100g is weighed, cleans and dries, is broken into block, it is water-soluble that the acetic acid that 1000mL pH is 4.5 is added
Liquid extracts 30min with 400W power ultrasound, obtains extracting solution.Vacuum rotary evaporator is added in extracting solution, is concentrated by evaporation to body
Product is original 30% or so, and 20g gamma-cyclodextrin is added, and is uniformly mixed, and is placed in dark place, with the revolving speed magnetic of 110rpm under room temperature
After power stirring for 24 hours, by 0.45 μm of water system membrane filtration, the extract not included is eluted, filtrate is directly spray-dried,
Obtain the gamma-cyclodextrin inclusion compound dry powder of Guava Leaf acid extract.
Embodiment 5
Guava fruit tablet 100g is weighed, cleans and dries, is broken into block, is added in 1000mL water and (is adjusted to sodium bicarbonate
PH is 8.0), to extract 80min, obtain extracting solution.It is 30% or so originally that extracting solution, which is concentrated into volume by rotary evaporation,
10g maltose cyclodextrin is added, is uniformly mixed, is placed in dark place, under room temperature with the revolving speed magnetic agitation of 110rpm for 24 hours after, pass through
0.45 μm of water system membrane filtration elutes the extract not included, filtrate is directly spray-dried to get Fructus psidii guajavae immaturus alkali carries
Take the maltose cyclodextrin inclusion compound dry powder of object.
The maltose cyclodextrin inclusion compound dry powder of obtained Fructus psidii guajavae immaturus alkali extract and citric acid, tartaric acid are reconciled mixed
It is even, 4 DEG C of dryings are placed in, compressing tablet process are carried out to mixed powder using tablet press machine, oral preparation is made in sealing pack.
The stability and biology for the Fructus psidii guajavae immaturus leaf extract cyclodextrin inclusion compound that effect example embodiment 1 is prepared
Activity determination
FTIR spectrum (FT-IR) analysis is carried out to cyclodextrin used and gained cyclodextrin inclusion compound dry powder, i.e., will
Sample (the hydroxypropyl-beta-cyclodextrin inclusion dry-powder product of guava leaf extract prepared by embodiment 1) presses 1 with potassium bromide:
10 mass ratio mixed pressuring plates measure 400-4000cm-1Spectrum, as a result as shown in Figure 1.As seen from Figure 1, Guava Leaf mentions
Take object after cyclodextrin encapsulated, infrared absorption peak is substantially identical as cyclodextrin, except a small amount of exposed in addition to cyclodextrin cavity
Functional group have a part absorption peak similar with extract, and the physical mixture of cyclodextrin and extract then have it is more with mention
Infrared absorption peak as taking species.The experimental results showed that guava leaf extract is wrapped in the cavity of hydroxypropyl-β-cyclodextrin
Interior, the two forms real inclusion compound.
To extract used and gained cyclodextrin inclusion compound carry out thermogravimetric analysis (method referring to " Zhu, Z.Y., Luo, Y.,
Liu,Y.,Wang,X.T.,Liu,F.,Guo,M.Z.,Wang,Z.,Liu,A.J.,&Zhang,Y.M.(2016).Inclusion
of chrysin inβ-cyclodextrin and its biological activities.Journal of Drug
Delivery Science&Technology, 31,176-186. "), as a result as shown in Figure 2 and Figure 3, wherein Fig. 2 is guava
The thermogravimetric analysis (TGA) of leaf extract/difference quotient thermogravimetric analysis (DTG) figure, Fig. 3 are guava leaf extract/hydroxy propyl-Beta-ring paste
The TGA/DTG of inclusion compounds schemes.The TGA curve and DTG curve of Fig. 2 shows guava leaf extract when temperature closes on 100 DEG C
Start loss of stability, quality dramatic decrease.Fig. 3 show by hydroxypropyl-β-cyclodextrin inclusion after, the heat of extract
Stability is remarkably reinforced, and product quality just starts dramatic decrease when temperature is close to 300 DEG C.
To extract used and gained cyclodextrin inclusion compound carry out stability and inoxidizability measurement (method referring to
“Rakmai,J.,Cheirsilp,B.,Mejuto,J.C.,Torrado-Agrasar,A.,&Simal-Gándara,J.
(2016).Physico-chemical characterization and evaluation of bio-efficacies of
black pepper essential oil encapsulated in hydroxypropyl-beta-
cyclodextrin.Food Hydrocolloids,65,157-164.”、“Hammi,K.M.,Jdey,A.,Abdelly,C.,
Majdoub,H.,&Ksouri,R.(2015).Optimization of ultrasound-assisted extraction of
antioxidant compounds from Tunisian Zizyphus lotus fruits using response
Surface methodology.Food Chemistry, 184,80-89. "), by polyphenol contained in extract and inclusion compound
Flavones is diluted to same concentration, and the ultraviolet lamp of 15W is placed the position from sample distance 20cm, was irradiated for 1 week, is sampled daily
Its inoxidizability is measured, as a result as shown in Figure 4, Figure 5.Fig. 4 and Fig. 5 is respectively that guava leaf extract and Guava Leaf extract
DPPH free radical scavenging ability and ATBS of the object/hydroxypropyl-beta-cyclodextrin inclusion under different time of ultraviolet irradiation+Free radical
Scavenging activity.It can be seen from the figure that with the growth of time of ultraviolet irradiation, under the oxidation resistance straight line for not including extract
Drop, and the DPPH free radical scavenging ability and ATBS of cyclodextrin inclusion compound+Free radical scavenging ability fall is smaller, guava
Leaf extract/hydroxypropyl-beta-cyclodextrin inclusion can preferably retain the oxidation resistance of extract.
To gained cyclodextrin inclusion compound carry out alpha-glucosaccharase enzyme inhibition test (operation see " Wang, L., Liu,
Y.,Luo,Y.,Huang,K.,&Wu,Z.(2018).Quickly Screening for Potentialα-Glucosidase
Inhibitors from Guava Leaves Tea by Bioaffinity Ultrafiltration Coupled with
HPLC-ESI-TOF/MS Method.Journal of Agricultural&Food Chemistry, 66 (6) "), by market
On alpha-glucosidase restrainer acarbose as control, as a result as shown in Figure 6.Rejection ability (the IC of acarbose50=
2.974 ± 0.07mg/mL) it is significantly lower than guava leaf extract/hydroxypropyl-beta-cyclodextrin inclusion (IC50=0.197 ±
0.02mg/mL).The result shows that guava leaf extract/hydroxypropyl-beta-cyclodextrin inclusion has stronger inhibition α-glucose
The effect of glycosides enzyme has hypoglycemic potentiality.
Comparative example Fructus psidii guajavae immaturus/leaf active constituent extracting method, extracting solution and cyclodextrin encapsulated influence factor are tested
(1) Guava Leaf extraction process of active component:
Using 70% ethyl alcohol, the soda acid aqueous solution of hot water and different pH value extracts processing to 4g Guava Leaf, examines
Wherein polyphenol chromocor content is surveyed, the results are shown in Table 1, and the effect for extracting Guava Leaf active constituent using ethyl alcohol is optimal,
Secondary is acidic aqueous solution, and hot water extraction effect is poor, therefore ethyl alcohol is selected to carry out the extraction of Guava Leaf active constituent.
The different influences for extracting reagent to guava active constituent in extracting solution of table 1.
| Extract reagent | Extraction time | Polyphenol content (mg/g) | Flavones content (mg/g) |
| 70% ethyl alcohol | 30min | 25.72 | 8.96 |
| 100 DEG C of hot water | 30min | 14.21 | 2.32 |
| The sodium bicarbonate aqueous solution of pH8 | 30min | 17.25 | 3.47 |
| The aqueous acetic acid of pH4.5 | 30min | 18.10 | 5.21 |
(2) inclusion compound preparation process:
1. there are many cyclodextrin encapsulated method, to obtain economical and practical inclusion compound preparation process, we are practical from production
It sets out, include and be compared its strengths and weaknesses using polishing, supercritical ultrasonics technology, mechanical mixing method these three methods.
Polishing, which refers to for 10g hydroxypropyl-β-cyclodextrin to be dissolved in the water for being equivalent to 5 times of quality of cyclodextrin, to be ground well, and is added
4g guava leaf extract prepared by embodiment 1, is placed in be sufficiently mixed in grinder and is ground into paste, after 4 DEG C of low temperature dryings,
It is cleaned with 75% ethyl alcohol, in 60 DEG C of oven dryings to get inclusion compound.
Supercritical ultrasonics technology, which refers to, is added to the saturation of hydroxypropyl-β-cyclodextrin containing 10g for 4g guava leaf extract in embodiment 1
In solution, 160W ultrasonic power is selected, 35 DEG C of temperature, continuous ultrasound 30min is filtered after being put into refrigerator cold-storage, with a small amount of anhydrous
Ethanol washing filter cake, being placed in baking oven dry, pulverize up to inclusion compound for 60 DEG C.
Mechanical mixing method refers to, and guava leaf extract and hydroxypropyl-β-cyclodextrin are added according to the feed ratio of 1:10
In 100ml aqueous solution, cyclodextrin saturated solution is formed.Fusion 6 hours is stirred with revolving speed 120rpm at 50 DEG C, after suction filtration
It is freeze-dried to get inclusion compound.
Experimental result measure guava leaf polyphenol content in different inclusion methods (operation see " Wang, L., Liu, Y., Luo,
Y.,Huang,K.,&Wu,Z.(2018).Quickly Screening for Potentialα-Glucosidase
Inhibitors from Guava Leaves Tea by Bioaffinity Ultrafiltration Coupled with
HPLC-ESI-TOF/MS Method.Journal of Agricultural&Food Chemistry, 66 (6) ") are as follows: it is mechanical
Paddling process > supercritical ultrasonics technology > polishing, wherein mechanical mixing method divides with polyphenol content contained by inclusion compound obtained by supercritical ultrasonics technology
It Wei not 25.78mg/g, 22.04mg/g, the significantly larger than polyphenol content (14.17mg/g) of inclusion compound obtained by polishing.
Based on experimental result, it is contemplated that the mechanical stirring time is longer, combined echocardiography wave method time shorter advantage, will be mechanical
Stirring is combined with supercritical ultrasonics technology.It is water-soluble that 4g guava leaf extract is added to the saturation containing 10g hydroxypropyl-β-cyclodextrin
In liquid, 120W ultrasonic power is selected, 35 DEG C of ultrasonic temperature, after ultrasonic 30min, is put into stirring in water bath instrument, 50 DEG C, 120rpm stirs
4h is mixed, is freeze-dried after suction filtration to get inclusion compound.
It is compared with inclusion compound obtained by above-mentioned mechanical mixing method, polyphenol, flavones in the ultrasonic resulting inclusion compound of mechanical mixing method
(" Wang, L., Liu, Y., Luo, Y., Huang, K., &Wu, Z. (2018) .Quickly Screening for is shown in operation
Potentialα-Glucosidase Inhibitors from Guava Leaves Tea by Bioaffinity
Ultrafiltration Coupled with HPLC-ESI-TOF/MS Method.Journal of Agricultural&
Food Chemistry, 66 (6) ") content is respectively 3.4 times, 2.5 times of inclusion compound obtained by mechanical mixing method, and includes produce
Rate is high, therefore optimizes technique and included using ultrasonic mechanical mixing method.
2. influence of the feed ratio of consideration extract and cyclodextrin to inclusion effect, the Guava Leaf in embodiment 1 is mentioned
Feeding intake according to mass ratio 1:1,1:3,1:5,1:10,1:20 for object and hydroxypropyl-β-cyclodextrin is taken, using ultrasonic mechanical mixing method
(selection 120W ultrasonic power, after ultrasonic 30min, is put into stirring in water bath instrument by 35 DEG C of ultrasonic temperature, 50 DEG C, 120rpm stirring
4h is freeze-dried to get inclusion compound after suction filtration) it is embedded, polyphenol substance content in inclusion compound is measured, the results show that
Embedding effect is preferable when guava extract and cyclodextrin mass ratio are 1:3,1:5, and the polyphenol substance content embedded is higher,
Polyphenol content is respectively 86.24mg/ml, 91.75mg/ml；When mass ratio is 1:1, the surveyed minimum 34.11mg/ of polyphenol content
Ml, reason may be less for cyclodextrin content, and inclusion is incomplete；Mass ratio be 1:10 and 1:20 when, polyphenol content with feed intake
Mass ratio is close when being 1:3,1:5, considers cost and economic benefit, selective extraction object and feeding intake for cyclodextrin are according to mass ratio
1:3 is included.
3. influence of the mixing time to inclusion effect is considered, by extract and hydroxypropyl-β-cyclodextrin according to mass ratio 1:3
It feeds intake, is embedded using ultrasonic mechanical mixing method, wherein mixing time is respectively 1,2,3,5,8,10,15 hour, measurement packet
The polyphenol chromocor content in object is closed with the optimal mixing time of determination.As a result (table 2) shows the inclusion compound of stirring 5,8 and 10 hours
Completely, polyphenol chromocor content is higher for inclusion；It is when 1,2,3 hour between upon agitation, since mixing time is shorter, extract is not
It can include completely, polyphenol chromocor content is lower；Stirring 15 hours close with 5,8,10 hours effects, therefore selects mixing time
It is 5-10 hours.
Table 2. embeds influence of the mixing time to inclusion compound polyphenol chromocor content
| Mixing time (h) | 1 | 2 | 3 | 5 | 8 | 10 | 15 |
| Polyphenol content (mg/g) | 34.42 | 46.74 | 67.18 | 101.24 | 105.13 | 105.88 | 104.21 |
| Flavones content (mg/g) | 8.94 | 12.65 | 18.62 | 24.20 | 25.37 | 26.10 | 25.84 |
4. influence of the pH to inclusion effect in cyclodextrin and guava leaf extract mixed solution is considered, by extract and hydroxyl
Propyl-beta-cyclodextrin feeds intake according to mass ratio 1:3, is embedded using ultrasonic mechanical mixing method, and wherein mixing time is 5h, stirs
During mixing, using the pH of 2M NaOH solution and 2M HCl solution dynamic regulation mixed solution, its pH is made to maintain 3-5 (acid
Property) or 8-10 (alkalinity) between, measure inclusion compound in polyphenol content.The result shows that inclusion compound inclusion is completely, more under acid condition
Phenol content is higher (polyphenol content (TP)=115.27 mg/g)；Otherwise polyphenol content in inclusion compound obtained under alkaline condition
Lower (polyphenol content (TP)=93.85 mg/g).This may can promote point of guava leaf extract due to acid condition
Solution, the small-molecule substance resolved into is easier to enter in cyclodextrin cavity, so that inclusion effect is more excellent.Therefore tune when ultrasound embedding stirring
Saving mixed solution pH is that 3-5 range is more excellent.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, other any changes, modifications, substitutions, combinations, simplifications made without departing from the spirit and principles of the present invention,
It should be equivalent substitute mode, be included within the scope of the present invention.
Claims (10)
1. a kind of preparation method of Fructus psidii guajavae immaturus leaf extract cyclodextrin inclusion compound, characterized by the following steps:
(1) pretreatment of raw material: guava fruit tablet and/or leaf are cleaned and dried, is crushed；
(2) extract: the broken raw material that Extraction solvent and step (1) are obtained mixes, and extracts, is filtered to remove filter residue,
Obtain extracting solution；
(3) it is concentrated by evaporation: the extracting solution that step (2) obtain being concentrated, concentrate is obtained；
(4) cyclodextrin encapsulated: cyclodextrin to be added in the concentrate that step (3) obtain, be uniformly mixed, obtain mixed liquor A；It will mix
Conjunction liquid A is placed in dark place and is included, and filters, and elutes the concentrate not included, obtains filtrate；
(5) drying and crushing: the filtrate that step (4) is obtained is dry, crushes, and obtains the ring paste of Fructus psidii guajavae immaturus and/or leaf extract
Inclusion compounds.
2. the preparation method of Fructus psidii guajavae immaturus leaf extract cyclodextrin inclusion compound according to claim 1, it is characterised in that:
Sodium bicarbonate aqueous solution that Extraction solvent is water, pH is 4.5 described in step (2) aqueous acetic acid, pH are 8.0 and
Concentration is at least one of the edible ethanol of percent by volume 40~95%；
The dosage of cyclodextrin described in step (4) is based on every 100g guava fruit tablet and/or leaf proportion 10~20g cyclodextrin
It calculates.
3. the preparation method of Fructus psidii guajavae immaturus leaf extract cyclodextrin inclusion compound according to claim 2, it is characterised in that:
The hot water that the water is 70~100 DEG C；
The edible ethanol is the edible ethanol that concentration is percent by volume 70%.
4. the preparation method of Fructus psidii guajavae immaturus leaf extract cyclodextrin inclusion compound according to claim 1, it is characterised in that:
The dosage of Extraction solvent described in step (2) matches 800~1200mL by every 100g guava fruit tablet and/or leaf and mentions
Solvent is taken to calculate；
The degree of concentration described in step (3) is be concentrated into extracting liquid volume 25~35%；
Cyclodextrin described in step (4) is alpha-cyclodextrin, beta-cyclodextrin, gamma-cyclodextrin, hydroxypropyl-β-cyclodextrin, glucose
One of cyclodextrin, maltose cyclodextrin and carboxymethyl cyclodextrin are a variety of；
The water system membrane filtration by 0.45~0.85 μm is filtered into described in step (4).
5. the preparation method of Fructus psidii guajavae immaturus leaf extract cyclodextrin inclusion compound according to claim 1, it is characterised in that:
The time of extraction described in step (2) is 30~120min；
Specific step is as follows for the method 4 of inclusion described in step (4): first ultrasound inclusion is stirred for including.
6. the preparation method of Fructus psidii guajavae immaturus leaf extract cyclodextrin inclusion compound according to claim 5, it is characterised in that:
Ultrasonic power in the ultrasound inclusion is 100~200W；
Ultrasonic time in the ultrasound inclusion is 20~40min；
Ultrasonic temperature in the ultrasound inclusion is 25~80 DEG C；
Whipping temp in the stirring inclusion is 20~70 DEG C；
Mixing speed in the stirring inclusion is 50~180rpm；
Mixing time in the described stirring inclusion is 5~for 24 hours；
The pH value of mixed liquor A is also maintained 3~10 in whipping process in the stirring inclusion.
7. a kind of Fructus psidii guajavae immaturus leaf extract cyclodextrin inclusion compound, it is characterised in that: pass through the preparation described in claim 1~6
Method obtains.
8. Fructus psidii guajavae immaturus leaf extract cyclodextrin inclusion compound as claimed in claim 7 is in preparing anti diar rhea and blood sugar reducing food
Using.
9. Fructus psidii guajavae immaturus leaf extract cyclodextrin inclusion compound according to claim 8 is preparing anti diar rhea and blood sugar reducing food
In application, it is characterised in that: the dosage form of the food be solid-state granules beverage or preparation.
10. Fructus psidii guajavae immaturus leaf extract cyclodextrin inclusion compound according to claim 8 is preparing anti diar rhea and hypoglycemic food
Application in product, it is characterised in that: the application includes the following steps: the Fructus psidii guajavae immaturus leaf extract cyclodextrin packet
Object is closed as raw material or addition appropriate amount of auxiliary materials, solid-state granules beverage or tabletted is formed, forms preparation.
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| CN114848601A (en) * | 2022-03-09 | 2022-08-05 | 广东药科大学 | Guava leaf extract effervescent tablet and preparation method and application thereof |
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