CN103565909A - Liquorice particles and preparation method thereof - Google Patents
Liquorice particles and preparation method thereof Download PDFInfo
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- CN103565909A CN103565909A CN201210283325.6A CN201210283325A CN103565909A CN 103565909 A CN103565909 A CN 103565909A CN 201210283325 A CN201210283325 A CN 201210283325A CN 103565909 A CN103565909 A CN 103565909A
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Abstract
The invention discloses veterinary liquorice particles, which are more convenient to store and transport. The veterinary liquorice particles are prepared from the following components in parts by weight: 170-200 parts of liquorice extractum (containing 1000 parts of crude drugs), 50-80 parts of polyvinylpyrrolidone, 50-80 parts of hydroxy propyl cellulose and 100-150 parts of maltodextrin. Cane sugar is added to the components to reach 1000 parts. The preparation method of the liquorice particles comprises the following steps: carrying out low-temperature reflux extraction on the liquorice crude drugs, and adding the polyvinylpyrrolidone, the hydroxy propyl cellulose, the cane sugar and the like; and pelletizing and drying, so as to obtain the liquorice particles, which are high in effective ingredients, stable in ingredients, not easy to absorb moisture, good in stability and long in storage time.
Description
Technical field
The present invention relates to a kind of licorice root particles and preparation method thereof, belong to the field of Chinese medicines.
Background technology
Glycyrrhiza preparation refers to that the active component that extraction obtains from the root and rhizome of pulse family herbaceos perennial Radix Glycyrrhizae adds the Chinese medicine preparation that pharmaceutic adjuvant is prepared from.Glycyrrhiza preparation has the effect of antiviral, antiinflammatory, removing toxic substances, enhancing human body immunity, has effect widely in the treatment of respiratory tract and gastroenteropathy.In veterinary clinic, glycyrrhiza preparation is mainly used in asthma and cough that the various causes of disease cause, laryngopharynx swelling and pain etc.
The chemical composition of Radix Glycyrrhizae is very complicated, contains number of chemical composition, and main component has glycyrrhizic acid, liquiritin etc.From Radix Glycyrrhizae, isolated compound has the tens of kinds of compounds such as glycyrrhizin, enoxolone, liquiritin, isoliquiritin, neoliquriitin, neoisoliquiritin, glycyrrhizin, isoliquiritigenin and licoricidin (+)-Licoricidin., glycyrol, isoglycyrol, 7-methylcoumarin essence, umbelliferone so far.At present, glycyrrhiza preparation mainly detects the content that index is glycyrrhizic acid, and research shows, the glycyrrhizin in Radix Glycyrrhizae and Flavonoid substances are most important biological active substanceies, flavonoid has the effect of similar adrenocortical hormone, has removing toxic substances, antiacid and alleviate the effect of mild muscular spasm.
People's Republic of China's veterinary drug allusion quotation (version was two in 2010) discloses a kind of method of preparing licorice root particles: extracting liquorice, moistening, section decocts with water 3 times, each 2h, collecting decoction.Placement is spent the night and is made precipitation, gets supernatant concentration to thick paste shape, and taking-up is appropriate, by the method under (assay) item, measures the content of glycyrrhizic acid, and adjusting makes up to specification, obtains Radix Glycyrrhizae extractum.Extracting liquorice extractum, adds appropriate sucrose, dextrin, mixes, and granulates, dry, obtains.But the extraction process extraction efficiency that use the method is prepared licorice root particles is low, extracts active ingredients is insufficient, and the production cycle is longer, and sugar content is high, and easily moisture absorption caking, has relatively high expectations to packaging material and storage condition.The patent of CN 102319283A discloses a kind of method that reflux is prepared veterinary licorice root particles, but its effective ingredient does not reach the disclosed standard of People's Republic of China's veterinary drug allusion quotation (version was two in 2010), is not suitable for the application in reality.
Summary of the invention
In view of this, main purpose of the present invention be to provide a kind of store and the veterinary licorice root particles of transportation with and preparation method thereof, the licorice root particles that utilizes the method to make, active constituent content is high, finished product stability good.
Technical scheme
The present invention has obtained a kind of licorice root particles by low temperature reflux method, consist of the following composition: Radix Glycyrrhizae extractum 170-200 weight portion (containing crude drug 1000 weight portions), polyvinylpyrrolidone 50-80 weight portion, hydroxypropyl cellulose 50-80 weight portion, maltodextrin 100-150 weight portion, with sucrose to 1000 weight portion.
Main purpose of the present invention is a kind of preparation method of licorice root particles, it is characterized in that, comprises the following steps:
A, extracting liquorice crude drug add organic solvent low temperature to soak, and carry out low temperature reflux extraction in hot reflux low-temperature extracting tank, the concentrated Radix Glycyrrhizae clear paste that obtains;
Leaching supernatant is clarified, crossed to b, the Radix Glycyrrhizae clear paste that step a is obtained;
C, supernatant concentrating under reduced pressure that step b is obtained, to obtain Radix Glycyrrhizae extractum, add polyvinylpyrrolidone, hydroxypropyl cellulose, and maltodextrin and sucrose are granulated, dry, obtain licorice root particles.
In preparation method of the present invention, when the extraction to Radix Glycyrrhizae crude drug, the mixed solution of choice for use organic solvent or organic solvent and water soaks extraction, can use the conventional organic solvent in this area, as ethanol, ether etc., preferably, the organic solvent using in described step a is ethanol, and under cryogenic conditions, carry out extraction and concentration, to contribute to the stripping of effective ingredient in Radix Glycyrrhizae, the active component that has retained to greatest extent medicine, makes to extract more fully, more thorough, and gained finished product active constituent content is high; More preferably, in described step a, the ratio of ethanol is 50-60v/v%; Most preferably, in described step a, the ratio of ethanol is 55v/v%.
In preparation method of the present invention, use the method for low temperature reflux to extract Radix Glycyrrhizae crude drug, to reduce the loss of effective ingredient, and farthest reclaim effective ingredient; Preferably, the extraction temperature that in described step a, low temperature reflux extracts is 60-80 ℃, thickening temperature 50-70 ℃; Most preferably, in described step a, extracting temperature is 70 ℃, and thickening temperature is 60 ℃.
In preparation method of the present invention, optionally use flocculate with chitosan fining process to process Radix Glycyrrhizae extract, saved the time of remove impurity, gained extracting solution is more clarified, and impurity content is low; Preferably, in the clear paste in described step b, added chitosan clarifier; More preferably, chitosan before use, is mixed with the solution of 0.5-1v/v% in advance with acetic acid.
Preferably, in preparation method of the present invention, in described step c, added polyvinylpyrrolidone, hydroxypropyl cellulose, so that licorice root particles moisture-proof is better, more difficult moisture absorption in environment; Unexpectedly, as subsequent embodiment of the present invention proves, add polyvinylpyrrolidone, hydroxypropyl cellulose, can effectively extend the storage life of licorice root particles, improved the stability of licorice root particles; Preferably, the addition of the polyvinylpyrrolidone in the present invention is respectively 5-8% weight, and the addition of hydroxypropyl cellulose is 5-8% weight.
Preferably, in preparation method of the present invention, comprise the following steps:
A, extracting liquorice crude drug 1000 weight portions add in the filling of traditional Chinese herbs by thermal reflux extract at low temperature, the 50-60v/v% ethanol that adds 12-15 times of weight, adjusts 40 ℃ of temperature, soaks 30-60min, control tank internal pressure 40-50KPa, temperature 60-80 ℃ is carried out extract at low temperature, concentrates, until extracting solution is substantially colourless in the time of extraction, extract and finish, extracting solution is delivered to concentration tank, control 50-70 ℃ of temperature and concentrate, be concentrated into the clear paste that proportion is 1.05-1.10;
B, above-mentioned clear paste is added in proportion to the chitosan clarifier of 0.5-1% weight, stir, standing 12h, filters, and gets supernatant;
C, above-mentioned supernatant is evaporated to the extractum that density is 1.25-1.3 (about 170-200 weight portion), adds polyvinylpyrrolidone, hydroxypropyl cellulose, with maltodextrin, sucrose, granulate, dry, obtain licorice root particles 1000 weight portions.
Preferably, the extraction time in above-mentioned steps a is 6-8 time, each 20-30min.
Preferably, the polyvinylpyrrolidone in above-mentioned steps c is that 50-80 weight portion, hydroxypropyl cellulose are 50-80 weight portion, and maltodextrin is 100-150 weight portion, with sucrose to licorice root particles 1000 weight portions.
As seen from the above, licorice root particles of the present invention has been used the method for low temperature reflux to extract, the organic solvent using is ethanol, and under cryogenic conditions, carry out extraction and concentration, to contribute to the stripping of effective ingredient in Radix Glycyrrhizae, the active component that has retained to greatest extent medicine, makes to extract more fully, more thorough, and gained finished product active constituent content is high; Secondly, licorice root particles of the present invention is placed and is difficult for moisture absorption and makes moist in environment; Finally, licorice root particles good stability of the present invention, the storage time is long.
The specific embodiment
Below in conjunction with specific embodiment, further describe the present invention, advantage and disadvantage of the present invention will be more clear along with describing.But these embodiment are only exemplary, scope of the present invention are not formed to any restriction.It will be understood by those skilled in the art that lower without departing from the spirit and scope of the present invention and can the details of technical solution of the present invention and form be modified or be replaced, but these modifications and replacement all fall within the scope of protection of the present invention.
The preparation example 1 of embodiment 1, licorice root particles
Radix Glycyrrhizae 10kg is added in hot reflux extract at low temperature fills with, add 12 times of 55% alcoholic solution, soak 30min and make medical material drenched.Pass into vapours, control tank internal pressure 40-50Kpa, 65 ℃ of temperature are carried out extract at low temperature, extract 8 times, and each 20min, concentrates in the time of extraction, until extracting solution is substantially colourless, extracts and finishes.Extract whole extracting solution out to concentration tank, controlling temperature 60 C, to be concentrated into proportion be 1.10 clear paste.In concentrated solution, add 0.5%(v/v) chitosan clarifier, stir, standing 12h, filters, and gets supernatant.It is 1.25 thick paste that supernatant is evaporated to relative density, adds polyvinylpyrrolidone 500g, hydroxypropyl cellulose 500g, maltodextrin 1000g, mix homogeneously.With sucrose, to 10kg, granulate, dry, obtain.
The preparation example 2 of embodiment 2, licorice root particles
Radix Glycyrrhizae 10kg is added in hot reflux extract at low temperature fills with, add 15 times of 50% alcoholic solution, soak 30min and make medical material drenched.Pass into vapours, control tank internal pressure 40-50Kpa, temperature 70 C carries out extract at low temperature, extracts 6 times, and each 30min, concentrates in the time of extraction, until extracting solution is substantially colourless, extracts and finishes.Extract whole extracting solution out to concentration tank, controlling 65 ℃ of temperature, to be concentrated into proportion be 1.10 clear paste.In concentrated solution, add 1%(v/v) chitosan clarifier, stir, standing 12h, filters, and gets supernatant.It is 1.25 thick paste that supernatant is evaporated to density, adds polyvinylpyrrolidone 600g, hydroxypropyl cellulose 600g, maltodextrin 1200g, mix homogeneously.With sucrose, to 10kg, granulate, dry, obtain.
The preparation example 3 of embodiment 3, licorice root particles
Radix Glycyrrhizae 10kg is added in hot reflux extract at low temperature fills with, add 14 times of 60% alcoholic solution, soak 30min and make medical material drenched.Pass into vapours, control tank internal pressure 40-50Kpa, temperature 60 C carries out extract at low temperature, extracts 6 times, and each 30min, concentrates in the time of extraction, until extracting solution is substantially colourless, extracts and finishes.Extract whole extracting solution out to concentration tank, controlling temperature 70 C, to be concentrated into proportion be 1.10 clear paste.In concentrated solution, add 1% chitosan clarifier, stir, standing 12h, filters, and gets supernatant.It is 1.3 thick paste that supernatant is evaporated to density, adds polyvinylpyrrolidone 600g, hydroxypropyl cellulose 650g, maltodextrin 1500g, mix homogeneously.With sucrose, to 10kg, granulate, dry, obtain.
The comparison of the licorice root particles that embodiment 4, preparation method of the present invention and other preparation methoies obtain
Sample 1: embodiment 1 prepares the sample of gained.
Sample 2: adopt the method for the People's Republic of China's veterinary drug allusion quotation (version was two in 2010) to prepare licorice root particles sample: extracting liquorice 10kg, add 100L water soaking 30min, decoct each 2h, collecting decoction 3 times.Placement is spent the night and is made precipitation, gets supernatant concentration to the thick paste that relative density is 1.25, adds the maltodextrin of 10kg, with sucrose, to 10kg, mixes, and granulates, dry, obtains licorice root particles 10kg.
Sample 3: adopt the method for the People's Republic of China's veterinary drug allusion quotation (version was two in 2010) to extract, concentrated, it is 1.25 thick paste that extracting solution is concentrated into density, adds polyvinylpyrrolidone 500g, hydroxypropyl cellulose 500g, maltodextrin 1000g, mix homogeneously.With sucrose, to 10kg, granulate, dry, obtain.
Sample D: according to Chinese patent CN102319283A embodiment 1 preparation.
1, the licorice root particles active constituent content measuring that the inventive method and additive method prepare
This experiment is measured according to two content of the veterinary drug allusion quotation > > of < < People's Republic of China (PRC) version in 2010: wherein glycyrrhizic acid, liquirtin are undertaken by operational approach under licorice root particles assay item, the mensuration of total flavones adopts rutin standard curve method, take rutin standard substance as contrast, with the colour developing of sodium nitrite-aluminum nitrate-sodium hydroxide, 510nm place measures absorbance, preparation rutin standard curve.Accurately weighed Chinese medicine flavone extract, prepares need testing solution, adds sodium nitrite, aluminum nitrate, the colour developing of sodium hydroxide chromophoric solution, and 510nm place measures absorbance.
Assay method: get each test sample (sample 1, sample 2) appropriate, take dextrose standard sample, liquirtin, ammonium glycyrrhizinate is reference substance, measures the content of glycyrrhizic acid, liquirtin, polysaccharide in licorice root particles.
Licorice root particles active constituent content measuring result prepared by table 1 Different Extraction Method
As can be seen from the above table, in the licorice root particles that prepared by the inventive method, the content of glycyrrhizic acid, liquirtin and total flavones is all higher than method described in official method and CN102319283A.
2, the inventive method and additive method prepare licorice root particles hygroscopicity mensuration
Assay method: take each 5g of test sample (sample 1, sample 2, sample 3), being placed in diameter is in the desiccation culture ware (the heavy M0 of ware) of 11mm, sample particle is evenly laid in ware, 60 ℃ of dry 12h in vacuum drying oven, taking-up takes plate and granule closes heavy M1.Plate is placed in 65% constant humidity incubator, gets heavily (M2, M3, M4) with 24h, 48h, 72h, and calculation sample hydroscopicity.
The hydroscopicity of 24h sample=(M2-M0)/(M1-M0) * 100%
The hydroscopicity of 48h sample=(M3-M0)/(M1-M0) * 100%
The hydroscopicity of 72h sample=(M4-M0)/(M1-M0) * 100%
Hygroscopicity measurement result in licorice root particles 72h prepared by table 2 Different Extraction Method
As can be seen from the above table, granule prepared by the inventive method hygroscopicity in 24-72h is poor, and with the Particle Phase ratio that traditional method prepares, the moisture being not easy in absorbing environmental makes moist.
3, the licorice root particles stability contrast that method of the present invention and traditional method prepare
This experiment is carried out according to the veterinary drug allusion quotation > > of < < People's Republic of China (PRC) veterinary drug stability test guideline accelerated test of version in 2010 and long-term stable experiment operational approach, investigates the stability of the licorice root particles that preparation method of the present invention and other preparation methoies make.
(1) accelerated test is investigated the stability of medicine under acceleration environment, for preparation designs a package, transports, stores the necessary data that provides.Test method: get each 3 batches of each test samples (sample 1, sample 2, sample 3), ordinary packing, under the condition of 40 ℃ ± 2 ℃ of temperature, relative humidity 75% ± 5%, place 6 months, the 1st, 2,3,6 month the end of month, sample respectively once, outward appearance and the character of observing each test sample, the results are shown in Table 4.
Each test sample accelerated test result contrast of table 4
(2) under the condition that long-term stable experiment is stored in reality, investigate the stability of medicine, for formulating the effect duration of medicine, provide foundation.Test method: get each 3 batches of each test samples (sample 1, sample 2, sample 3), ordinary packing, under the condition of 25 ℃ ± 2 ℃ of temperature, relative humidity 60% ± 10%, place 12 months, the 3rd, 6,9,12 month the end of month, sample respectively once, outward appearance and the character of observing each test sample, the results are shown in Table 5.
Each test sample long-term stable experiment result contrast of table 5
From table 4, table 5, can find out, by accelerated test, long term test, licorice root particles prepared by method of the present invention is under specific investigation condition, in official hour, there is not the change of appearance character, having there is cosmetic variation at later stage in the granule preparing by official method, but can keep appearance character after adding polyvinylpyrrolidone, hydroxypropyl cellulose in the granule that same method makes in adjuvant.Possible reason is that in traditional preparation method, in sample, sugar content is high, and hygroscopicity is strong, easily there is character and change in long-term storage, but add polyvinylpyrrolidone, hydroxypropyl cellulose, after the two is combined with adjuvant, effectively resisted the deliquescence of sample in environment.
The foregoing is only preferred embodiment of the present invention, in order to limit the present invention, within the spirit and principles in the present invention not all, any modification of doing, be equal to replacement, improvement etc., within all should being included in protection scope of the present invention.
Claims (10)
1. a licorice root particles, it is characterized in that, consist of the following composition: Radix Glycyrrhizae extractum 170-200 weight portion (containing crude drug 1000 weight portions), polyvinylpyrrolidone 50-80 weight portion, hydroxypropyl cellulose 50-80 weight portion, maltodextrin 100-150 weight portion, with sucrose to 1000 weight portion.
2. a preparation method for licorice root particles, is characterized in that, comprises the following steps:
A, extracting liquorice crude drug add organic solvent low temperature to soak, and carry out low temperature reflux extraction in hot reflux low-temperature extracting tank, the concentrated Radix Glycyrrhizae clear paste that obtains;
Leaching supernatant is clarified, crossed to b, the Radix Glycyrrhizae clear paste that step a is obtained;
C, supernatant concentrating under reduced pressure that step b is obtained, to obtain Radix Glycyrrhizae extractum, add polyvinylpyrrolidone, hydroxypropyl cellulose, and maltodextrin and sucrose are granulated, dry, obtain licorice root particles.
3. method according to claim 2, is characterized in that, in described step a, organic solvent is ethanol.
4. method according to claim 3, is characterized in that, in described step a, the ratio of ethanol is 50-60v/v%.
5. method according to claim 2, is characterized in that, the extraction temperature that in described step a, low temperature reflux extracts is 60-80 ℃, thickening temperature 50-70 ℃.
6. method according to claim 6, is characterized in that, in described step a, extracting temperature is 70 ℃, and thickening temperature is 60 ℃.
7. method according to claim 2, is characterized in that, in the clear paste in described step b, has added chitosan clarifier.
8. method according to claim 2, is characterized in that, comprises the following steps:
A, extracting liquorice crude drug 1000 weight portions add in the filling of traditional Chinese herbs by thermal reflux extract at low temperature, the 50-60v/v% ethanol that adds 12-15 times of weight, adjusts 40 ℃ of temperature, soaks 30-60min, control tank internal pressure 40-50KPa, temperature 60-80 ℃ is carried out extract at low temperature, concentrates, until extracting solution is substantially colourless in the time of extraction, extract and finish, extracting solution is delivered to concentration tank, control 50-70 ℃ of temperature and concentrate, be concentrated into the clear paste that proportion is 1.05-1.10;
B, above-mentioned clear paste is added in proportion to the chitosan clarifier of 0.5-1% weight, stir, standing 12h, filters, and gets supernatant;
C, above-mentioned supernatant is evaporated to the extractum that density is 1.25-1.3 (about 170-200 weight portion), adds polyvinylpyrrolidone, hydroxypropyl cellulose, with maltodextrin, sucrose, granulate, dry, obtain licorice root particles 1000 weight portions.
9. method according to claim 8, is characterized in that, the extraction time in described step a is 6-8 time, each 20-30min.
10. method according to claim 8, is characterized in that, the polyvinylpyrrolidone in described step c is that 50-80 weight portion, hydroxypropyl cellulose are 50-80 weight portion, and maltodextrin is 100-150 weight portion, with sucrose to licorice root particles 1000 weight portions.
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| CN104280360A (en) * | 2014-09-26 | 2015-01-14 | 广东一方制药有限公司 | Preparation and quality control method of liquorice formula granules |
| CN104288217A (en) * | 2014-10-13 | 2015-01-21 | 洛阳惠中兽药有限公司 | Traditional Chinese medicine composition and application thereof |
| CN104367616A (en) * | 2014-08-18 | 2015-02-25 | 瓜州昊泰生物科技有限公司 | Licorice herb extraction method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104367616A (en) * | 2014-08-18 | 2015-02-25 | 瓜州昊泰生物科技有限公司 | Licorice herb extraction method |
| CN104367616B (en) * | 2014-08-18 | 2018-01-09 | 瓜州昊泰生物科技有限公司 | A kind of extracting method of licorice medicinal materials |
| CN104280360A (en) * | 2014-09-26 | 2015-01-14 | 广东一方制药有限公司 | Preparation and quality control method of liquorice formula granules |
| CN104288217A (en) * | 2014-10-13 | 2015-01-21 | 洛阳惠中兽药有限公司 | Traditional Chinese medicine composition and application thereof |
| CN104288217B (en) * | 2014-10-13 | 2018-09-11 | 洛阳惠中兽药有限公司 | A kind of Chinese medicine composition and purposes |
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