CN101703577B - Preparation method of guava leaf extract and traditional Chinese medicine preparation thereof - Google Patents
Preparation method of guava leaf extract and traditional Chinese medicine preparation thereof Download PDFInfo
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Abstract
The invention relates to a preparation method of guava leaf extract and a traditional Chinese medicine preparation thereof. The invention adopts the traditional technique 'water-extracting alcohol-sedimenting method' of the traditional Chinese medicine, optimizes the processing technique and establishes a preparation method of the guava leaf extract. The method has simple extraction technique, can extract the effective components in the guava leaf with high yield, therefore, the traditional Chinese medicine preparation product obtained by using the method has high drug effect and lower price.
Description
Technical field
The present invention relates to a kind of preparation method of Chinese medicine preparation, relate in particular to a kind of preparation method of guava leaf extract and Chinese medicine preparation thereof.
Background technology
Fructus psidii guajavae immaturus (Psidium guajava) is a Myrtaceae Psidium plant, originates in tropical America, and temperate zone of China and subtropical zone be existing plantation before more than 200 years.Fructus psidii guajavae immaturus enjoys scientist's concern owing to have stronger oxidation resistance in its leaf.Folium Psidii Guajavae has vessel softening, blood sugar lowering, blood fat and cholesterol; Effect with anoxia enduring, rapid allaying tiredness; Help to delay the peroxidating process of organism simultaneously, but other cardiovascular and cerebrovascular diseases such as prophylaxis of cancer, heart disease.In the middle of Folium Psidii Guajavae, at present find to contain multiple important polyphenol compound, experimental study shows the multiple efficacies that these polyphenol compounds are just given Folium Psidii Guajavae.
On the other hand, documents and materials show that the effective ingredient that extracts treatment traditional Chinese medical science diabetes from Folium Psidii Guajavae adopts " water extraction ", " alcohol dipping extraction method " to reach " enzymatic isolation method " mostly.
But wherein the total flavonoid yield that extracts of water extraction is higher, and flavone phenols (main component of performance curative effect) is relatively low; Adopt alcohol extracting method, flavone phenols component yield is higher, but the ethanol consumption is big, and the response rate is low, so cost is higher, and industrialization is produced inadvisable; Enzymatic Extraction requires enzyme that the specificity and the mild reaction conditions of high activity, height are arranged, and enzyme process is subjected to influence of various factors such as the kind, consumption, enzymolysis time, temperature, acid-base value, material fineness, stirring of enzyme, therefore the difficult control of production link finally influence extract yield.
Summary of the invention
In view of the foregoing, the present invention with
(1) gives full play to the effect of single medical material, from Folium Psidii Guajavae, extract a kind of Chinese medicine preparation that can treat diabetes and complication thereof preferably;
(2) providing preparation technology's (embody and influence the pass of extract yield key control main points in the process) of this Chinese medicine preparation is purpose,
Carry out test repeatedly, optimized processing technique, set up a kind of preparation method of guava leaf extract.This method extraction process is simple, and can be high yield extract effective ingredient (the total flavones phenols be that controlling index records with " Quercetin ") in the Folium Psidii Guajavae, so utilize tcm product drug effect height, the price of gained of the present invention lower.
The invention provides a kind of preparation method of guava leaf extract, comprising: pre-treatment step, decoction and concentration step, precipitate with ethanol, concentrated and drying steps.
Preparation method of guava leaf extract of the present invention adopts Chinese medicine traditional handicraft " decoction and alcohol sedimentation technique " that Folium Psidii Guajavae is extracted.
The capital equipment that uses: commercially available known equipment such as Chinese medicine medicine cutter, Chinese medicine multi-function extractor, triple effect vacuum concentration equipment, ethanol concentrating under reduced pressure equipment, vacuum drying oven, Chinese medicine grinder, fully-automatic capsule filling machine, therefore the foundation of production line is simple, no specific (special) requirements can reduce the initial stage funds.
The above steps of preparation method of guava leaf extract of the present invention is as follows in detail:
Pre-treatment step:
(1) for guaranteeing that effective ingredient leaches fully in the medical material, must carry out pretreatment to medical material before decocting: be about to Folium Psidii Guajavae and cut to becoming the filament shape.
(2) guarantee the abundant moistening of medical material, should give enough amount of water, at the 10-12 of medical material weight doubly, and before decocting with about 80 ℃ hot-water soak more than 12 hours.
(3) in decoction process, must add salad wet goods defoamer, be convenient to not have in the concentration process behind triple effect and the precipitate with ethanol and spume phenomenon and influence production.
Decoct and concentration step:
The Folium Psidii Guajavae of needs is decocted with water in multi-function extractor, because of the Folium Psidii Guajavae food value of leaf thicker, easily expand in the suction back, therefore need to strengthen and decoct water consumption, be that each decoction adds the water that 10-12 doubly measures respectively, and use hot-water soak about 12 hours, because of the Folium Psidii Guajavae food value of leaf is thicker,, need to decoct 2 times continuously for guaranteeing that the composition in the Folium Psidii Guajavae is more fully extracted, each about 3 hours, merge decoction liquor, filter, carry out vacuum concentration in the triple effect concentrator, the control thickening temperature is not higher than 80 ℃. and consider that triple effect concentrates the suitable water content in the extractum of back, help no longer thin up of the used high concentration ethanol of next step precipitate with ethanol.Consider that triple effect concentrates the suitable water content in the extractum of back, help no longer thin up of the used high concentration ethanol of next step precipitate with ethanol, so preferably extractum density is controlled at 1.15-1.20g/mL (80 ℃ of surveys) during receipts cream.
Precipitate with ethanol, concentrated and drying steps:
The spissated extractum of triple effect is added 95% an amount of ethanol in Alcohol-settling tank, about about 2 times of extractum weight, and heated and stirred is even, the supernatant concentration of alcohol was at 55-60% before survey was left standstill, left standstill 24-48 hour, and extracted supernatant and carry out vacuum decompression and be condensed into the thick paste that density is 1.30-1.35g/mL, through vacuum drying below 80 ℃ to moisture about 4%, rewinding, carry out 80 mesh sieves again and be ground into fine powder, directly make required preparation form, as capsule charge, pelletize etc., promptly.
In the precipitate with ethanol process:
(1) need during precipitate with ethanol to concentrate the extractum weight that the back is received according to triple effect, require the supernatant concentration of alcohol that reaches behind the concentration of alcohol of density, moisture and adding and the precipitate with ethanol, Theoretical Calculation goes out needed amount of alcohol, generally 2-3 times of receipts extractum weight.
(2) wanting powerful in the ethanol adition process and stir, and the vacuum recoil, fully guarantee the ethanol mixing of extractum and adding, the higher phenomenon of local concentration of alcohol can not occur, is different because Different concentrations of alcohol is sunk the material that will get off.
(3) the precipitate with ethanol process of leaving standstill need add cooling water circulation, room temperature or under subambient situation the precipitate with ethanol effect better.
(4) the precipitate with ethanol time is preferably in 24-48 hour, because think that by observation material is more floating in the alcohol deposit fluid, sedimentation velocity is slower.
(5) begin to leave standstill during precipitate with ethanol before concentration of alcohol preferably be controlled at 55-60%, because after test finds that all time of repose reaches several times, survey the supernatant concentration of alcohol and all rise about 10%, meet the concentration (about 70%) that we require, if concentration of alcohol is controlled at about 70% before beginning to leave standstill, can cause the supernatant determining alcohol about 80, concentrate back extractum yield lower (because concentration of alcohol material high more, that settle down is just many more).
(6) should carry out the secondary precipitate with ethanol, with the medicinal residues adding suitable quantity of water heated and stirred of a precipitate with ethanol, (or a precipitate with ethanol reclaims ethanol to add 95% ethanol again, concentration is about 85%) addition half of amount of alcohol when a precipitate with ethanol, left standstill 24-48 hour, and drew up clear liquid and concentrate drying.
Preparation method of guava leaf extract of the present invention adopts the traditional handicraft decoction and alcohol sedimentation technique, and operating equipment and technological process are simple.Decoction liquor concentrates and adopts the multiple-effect concentrator, and an effect, two is imitated the steam reusable edible that produces, and energy savings has reduced cost.It is alcoholic acid recyclable that precipitate with ethanol uses, and wherein the concentration of alcohol of a precipitate with ethanol recovery can directly be used by the secondary precipitate with ethanol about 85%, avoided high concentration ethanol dilution back to use the trouble of bringing, later on all capable of circulation the applying mechanically of ethanol of recovery.And, " water extract-alcohol precipitation " method that adopts is controlling index than the total flavones phenols that other method (alcohol dipping method, decocting method and enzymatic isolation method etc.) extracts with " Quercetin ", content is higher, between the 0.7-0.8mg/ grain, the quality standard that all meets formulation requires (standard is for being not less than the 0.56mg/* grain).The extractum that extracts is guaranteeing that because of carrying out repeatedly precipitate with ethanol extract dry product yield also other method is higher under the satisfactory prerequisite of content, and the dry product yield is 8-10%.
In addition, the present invention also provides a kind of Chinese medicine preparation of Folium Psidii Guajavae extract, it is characterized in that, is the preparation method of guava leaf extract preparation by the invention described above.
Preparation prescription of the present invention derives from the single medical material, does not have other adjuvant and adds, and extract directly prepares, and processing technology is simple, do not have other herbal species extraction extractum, add complicated procedures of forming such as adjuvant granulation, so price is lower.Because of deriving from the single medical material, effective ingredient is simple, does not have the interaction between other medicinal ingredient, and curative effect is direct.
The Chinese medicine preparation of Folium Psidii Guajavae extract of the present invention is preferably made capsule preparations.
This product has steady hypoglycemic effect for treatment pure tcm product diabetes and complication.It is vessel softening fully few in number in the market, trophic nerve, microcirculation improvement reaches the economic benefits and social benefits product that steady blood sugar lowering can well improve its complication again, but also can allow diabetics relax diet and ideal extra-nutrition improves immunity indirectly, this rule of origin is in the single medical material simultaneously, through water boiling and extraction, the precipitate with ethanol method for refining obtains extractum, vacuum drying (not having other adjuvants adds) back is capsule charge directly, extraction process is simple, therefore retail price is biased low in the middle of the like product, has alleviated patient's financial burden to a certain extent.
The present invention also provides the application of the above-mentioned preparation method of guava leaf extract in the Chinese medicine preparation preparation that contains Folium Psidii Guajavae extract.
Description of drawings
Fig. 1 is the detailed implementing process flow chart of preparation method of guava leaf extract of the present invention.
The specific embodiment
Following examples are used to illustrate the present invention, but are not used for limiting the scope of the invention.Fig. 1 is the detailed implementing process flow chart of preparation method of guava leaf extract of the present invention.Describe the establishment foundation of preparation method of guava leaf extract of the present invention in detail in conjunction with Fig. 1.
Embodiment 1 (preliminary test)
Folium Psidii Guajavae medical material 64kg is pulverized, the pack of part fine powder drops into Decocting pot, adds the 640kg drinking water, heated and boiled, insulation is dipped to second day, and heating decocted 3 hours, decocts for the second time to add water 600kg, decocted 3 hours, decoction liquor merges triple effect and is concentrated into density 1.15g/mL, and the about 15kg of weight adds the about 60kg of 95% ethanol of 4 times of amounts then, the concentration of alcohol of surveying this moment is 75%, left standstill 72 hours, and drew up clear liquid, the concentration of alcohol of surveying this moment is about 88%, vacuum concentration is to density 1.30g/mL, receive cream 2.5kg, with precipitate precipitate with ethanol 1 time according to the method described above respectively, receive the about 1.5kg of extractum altogether again, dry, with above twice about 4 hours of 80 ℃ of vacuum dryings of the extractum of receiving (shop starch in the part drip pan), extract dry powder 1.5kg, capsule charge after crushed.
Result of the test: extract dry product yield 2.5% (yield is lower); Quercetin content is measured the 1.2mg/ grain, is higher than the standard of formulation.
Analysis of experiments: the supernatant concentration of alcohol is higher in the time of may be for precipitate with ethanol, though effective ingredient be extracted out, precipitated the going down of most of composition in the extractum and cause extract yield low, thus next step test when needing to precipitate with ethanol supernatant concentration adjust.
Embodiment 2 (on the basis of preliminary test, the precipitate with ethanol process being improved)
Folium Psidii Guajavae 60.0kg is added the Chinese medicine extraction jar, add the about 600kg of water, drive steam valve and be heated to 80 ℃, soaked 14 hours.Heating decocts to boiling and keeps boiling time at 3 hours, squeezes into decoction liquor to the triple effect concentration tank; Two slags are added the about 600kg of water, and decocting to seething with excitement and keeping boiling time is 3 hours, filters feed liquid to concentration tank and is concentrated into density 1.18g/mL, receives cream, the about 40kg of weight.
A precipitate with ethanol: 40kg extractum is added in the Alcohol-settling tank, and heated and stirred adds 95% ethanol 82kg simultaneously, continue to stir, close steam valve, and open the chuck cooling water, continue stir about 20 minutes, survey precipitate with ethanol supernatant concentration 58%, stop to stir, left standstill 40 hours, draw up the clear liquid vacuum decompression and be concentrated into density 1.32g/mL, receive cream,, get extract dry product 3.8kg in 80 ℃ of dryings of vacuum drying oven.
The secondary precipitate with ethanol: the concentration that adds a precipitate with ethanol recovery in Alcohol-settling tank is 85% ethanol 45kg, agitating heating, and repeatedly recoil with vacuum, survey alcohol deposit fluid concentration 56%, left standstill 38 hours, draw up the clear liquid vacuum concentration, receive cream, density is 1.35g/mL, and vacuum drying gets extract dry product 2.1kg.
With once, weigh after the extract dry product of gained mixes behind the secondary precipitate with ethanol, total amount is that 5.9kg. becomes capsule through pulverizing filling.
Result of the test: total dry product yield is 9.8%, and the quercetin content determination data is: the 0.75mg/ grain.
Analysis of experiments: guaranteeing that total recovery has a more substantial increase, and meets preassigned under the satisfactory prerequisite of extract active constituent content.Therefore can confirm the extraction process basic feasible solution.
Embodiment 3 (scale-up is further confirmed the feasibility of technology)
1. Folium Psidii Guajavae 200kg is added extraction pot, add 2 tons in water and be heated to 80 ℃ of immersions 14 hours, decocting time 3 hours, leach decoction liquor to concentration tank, two slags continue to add 2 tons of decoctings and boiled 3 hours, and triple effect is concentrated into density and receives cream at 1.18g/mL, extractum weight 105kg.
2. precipitate with ethanol process
(1) precipitate with ethanol: 92% ethanol that adds about 50kg prior to Alcohol-settling tank, again in the disposable adding Alcohol-settling tank of extractum that triple effect is received, add ethanol while stirring, logical cooling water, add the about 210kg of 92% ethanol altogether, after adding, continue stirring, vacuum recoil, survey alcohol deposit fluid concentration of alcohol about 58%, left standstill 40 hours, and drew up clear liquid, survey concentration of alcohol this moment is about 70%, risen 12% with the initial concentration ratio, character is darker, dark red, limpider, is evacuated to pure concentration tank, and non-foam takes place, more easily concentrate, receive cream density 1.30g/mL.
(2) secondary precipitate with ethanol: the precipitate of a precipitate with ethanol stirred add the about 20kg of water simultaneously, add the about 150kg of ethanol (concentration is 85%) that reclaimed last time, after stirring, recoiling about 15 minutes, the survey concentration of alcohol is about 60%, leaves standstill 39 hours.Draw up clear liquid, survey concentration of alcohol, risen 10% with the initial concentration ratio 70%.Drawing up clear liquid to Alcohol-settling tank has frothing, puts to charging basket, and the back non-foam of refueling takes place, and more easily concentrates, and receives cream density 1.36g/mL at last.
(3) vacuum drying: dry with about 60 ℃ in vacuum drying oven, receive dried cream weight 19.5kg, filling after crushed becomes capsule.
(4) result of the test: quercetin content: 0.72mg/ grain; Extract yield: 9.7%.
Comparative example
The extraction of Folium Psidii Guajavae employing " water extract-alcohol precipitation " method is refining once repeatedly adopted other method to carry out the extraction of Folium Psidii Guajavae before implementing, as: " decocting in water " method, " alcohol dipping method " etc. are all in existing problems aspect extractum yield and the effective control composition (quercetin content), adopt " alcohol dipping method " ethanol consumption bigger simultaneously, cause cost higher, all inadvisable, the concrete operations example is as follows:
(1) water-boiling method:
Get Folium Psidii Guajavae 60.0kg, the equipment of use: Chinese medicine extraction jar, triple effect concentrator, vacuum decompression concentrator
Technical process: add about 600kg drinking water (10 times of amounts that are equivalent to medical material) in the Chinese medicine extraction jar, be heated to about 80 ℃ and soaked 12 hours, heating decocts, kept boiling time 3 hours, through filtering, emit decoction liquor, continue to add the drinking water of about 8 times of amounts in medicinal residues, decoct, kept boiling time 2 hours, after filtration, emit decoction liquor, decoction liquor is merged, be concentrated into extractum density approximately in triple effect concentration tank vacuum decompression: 1.35g/ml, receive the about 14kg of cream weight, in 80 ℃ of dryings of vacuum drying oven, the weight that gets dry extract 7.3kg, yield is: 12%, get extract and be: 0.12mg (criterion of acceptability: be not less than 0.56mg) according to the standard detection quercetin content of formulating
Conclusion is analyzed: adopt water-boiling method, though the extractum yield is higher, quercetin content is lower, and gained extractum viscosity is stronger, is difficult to drying, may be not relevant through making with extra care with a large amount of impurity that extract, so active constituent content is lower.
(2) alcohol dipping method (adding ultrasonic wave concussion): with Folium Psidii Guajavae 10kg, be cut into the spire shape through medicine cutter, in ultrasonic cleaner, add 95% ethanol 90kg, soak more than 24 hours, ultrasonic then 40 minutes, emit impregnation liquid, through vacuum decompression concentrate the about 1.0kg of extractum, about 0.4kg after the vacuum decompression drying detects quercetin content: content 1.9mg/ grain.
Conclusion is analyzed: by the test of alcohol dipping ultrasonic wave concussion method, though active ingredient of meletin content is higher, the extractum extract yield is lower, only is about 4%, and the ethanol large usage quantity, it is low to reclaim the back concentration of alcohol, can not be recycled, little, time-consuming, inadvisable in batches.
Claims (4)
1. a preparation method of guava leaf extract comprises: pre-treatment step, decoction and concentration step, precipitate with ethanol, concentrated and drying steps; Described pre-treatment step is that Folium Psidii Guajavae is cut the 10-12 water yield extraordinarily that gives medical material weight behind the filament shape to becoming, with the processing of 80 ℃ hot-water soaks more than 12 hours;
Described decoction and concentration step are to decoct 2 times continuously, carry out vacuum concentration in the triple effect concentrator, and thickening temperature is controlled at and is not higher than 80 ℃, and extractum density is controlled at 1.15-1.20g/mL;
Described precipitate with ethanol, the concentrated drying steps that reaches are, 2 times 95% ethanol that the spissated extractum of triple effect is added cream weight in Alcohol-settling tank, and heated and stirred is even, the supernatant concentration of alcohol is controlled at 55-60% before leaving standstill, left standstill 24-48 hour, the medicinal residues of a precipitate with ethanol are added the suitable quantity of water heated and stirred, reclaim ethanol after adding a precipitate with ethanol again, addition half of amount of alcohol when a precipitate with ethanol, left standstill 24-48 hour, extract supernatant and carry out vacuum decompression and be condensed into the thick paste that density is 1.30-1.35g/mL, through vacuum drying below 80 ℃ to moisture 4%.
2. according to the Folium Psidii Guajavae extract of the preparation method of guava leaf extract described in the claim 1 preparation.
3. the application of Folium Psidii Guajavae extract according to claim 2 in the Chinese medicine preparation of preparation treatment diabetes and complication thereof.
4. application according to claim 3 is characterized in that, described Chinese medicine preparation is a capsule preparations.
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| CN102210747A (en) * | 2011-06-02 | 2011-10-12 | 深圳清华大学研究院 | Hypoglycemic pharmaceutical preparation and preparation method thereof |
| CN111329938A (en) * | 2020-04-21 | 2020-06-26 | 李德潮 | Zhuang Yao medicine preparation for treating diabetes |
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