CN1369306A - 'Huajuhong' preparation and its preparing process - Google Patents
'Huajuhong' preparation and its preparing process Download PDFInfo
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- CN1369306A CN1369306A CN 02114847 CN02114847A CN1369306A CN 1369306 A CN1369306 A CN 1369306A CN 02114847 CN02114847 CN 02114847 CN 02114847 A CN02114847 A CN 02114847A CN 1369306 A CN1369306 A CN 1369306A
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- citri grandis
- exocarpium citri
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- huajuhong
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Landscapes
- Medicines Containing Plant Substances (AREA)
Abstract
A phlegm-resolving antitussive medicine "Huajuhong" is prepared from whole pummelo fruit through pulverizing, water extracting 1-3 times while collecting volatile oil, filter, mixing the filtrate, adding organic solvent, separating, concentrating to obtain extract, drying, adidng auxiliaries and collected volatile oil, granulating, and preparing tablets or capsules. Its advantages are high utilization rate of its active components and high curative effect.
Description
Technical field:
The present invention relates to Chinese medicine Exocarpium Citri Grandis extraction of effective components, Exocarpium Citri Grandis preparation and production method thereof.
Background technology:
Exocarpium Citri Grandis, another nameization continent dried tangerine peel, red, the Citrus grandis Osbeck. Var.tomentosa Hort. of change are immaturity or the outer peel of maturescent drying of rutaceae continent Fructus Citri grandis Citrus grendis Tomentosa or Fructus Citri grandis Citrus grendis (L) Osbeck.Exocarpium Citri Grandis comprises the tangerine and secondary texturing dried tangerine peel of positive texturing.Warm in nature, hot, bitter, the effect of tool cold expelling, dampness, promoting the circulation of QI, expectorant, antiinflammatory.Be used for the cough due to wind and cold clinically, itching of the throat abundant expectoration, acute/chronic bronchitis, chronic obstructive emphysema etc.Contain alkaloids in the Exocarpium Citri Grandis, flavonoid, polysaccharide, volatilization wet goods number of chemical composition.Glycoside wherein, flavonoid and naringin have multiple effects such as relieving cough and resolving phlegm antiinflammatory.Chinese Pharmacopoeia is with the diagnostic characteristics of naringin as Exocarpium Citri Grandis.On the research and utilization in past, major part all is the compound recipe prescription according to ancient times, and is not enough to the research of wherein monarch drug Exocarpium Citri Grandis itself, and result of use is often little desirable; To play curative effect to disease, need bigger dosage, and onset time be longer.On its using method, be the skin zone that uses the Exocarpium Citri Grandis fruit, not seeing has the report that uses full fruit.On the method for its development and use, be compound preparation, use with other Chinese medicine configuration, do not see that folk prescription uses.Use compound recipe, fail Exocarpium Citri Grandis is carried out deep development.Owing to only use skin zone, often need to adopt maturescentization continent Fructus Citri grandis make raw material, raw material sources are limited, and need skin and meat are separated, and complex manufacturing fails to utilize fully the effective site of Exocarpium Citri Grandis, causes the authentic medicinal herbs wasting of resources of this Guangdong of Exocarpium Citri Grandis.
Summary of the invention
Purpose of the present invention utilizes degree low in order to overcome Exocarpium Citri Grandis exactly, the shortcoming that effective component extraction rate is low, the medical value of the full fruit of exploitation Exocarpium Citri Grandis, simplify production technology, use the Exocarpium Citri Grandis folk prescription separately, provide the full fruit of Exocarpium Citri Grandis to utilize degree height, preparation that extracting method that effective component extraction rate is high and result of use are good and production method.
The present invention realizes like this.
Exocarpium Citri Grandis immaturity or maturescent all-fruit powder is broken, through water extraction, collect volatile oil simultaneously, aqueous extract filters, and merging filtrate further adds organic solvent separation and purification or not with an organic solvent, be condensed into extractum, add adjuvant, mix, add the volatile oil of having collected, granulate tabletting, sugar coating is made tablet, or makes capsule, or electuary (granule), or make other oral formulations.
Can not collect volatile oil among the present invention, but its result of use descends slightly.
Exocarpium Citri Grandis of the present invention is good with positive texturing dried tangerine peel.Its active constituent content is higher than secondary texturing dried tangerine peel.
Exocarpium Citri Grandis of the present invention can single medicinal material as crude drug, also can make compound preparation with other Chinese medicine compound (compound).
Water extraction among the present invention can adopt in room temperature or under the ebuillition of heated condition and carry out.Extraction time should be one to three time at least.The consumption of water is that water can not have the full fruit of Exocarpium Citri Grandis medical material at least, and water consumption is not too much limit.
The organic solvent that the present invention adds can adopt ethanol, chloroform, ethyl acetate, petroleum ether etc.Ethanol can adopt dehydrated alcohol or various concentration ethanol, and petroleum ether can adopt petroleum ether-30, petroleum ether-60 or petroleum ether-90.
It is an amount of to get the full fruit of the Exocarpium Citri Grandis extractum that the said extracted method makes, an amount of with the extract extractum of the same quadrat method of Exocarpium Citri Grandis skin, add high performance liquid chromatography mobile phase: methanol-acetic acid-water (35: 4: 61) dilution, filter, filtrate places volumetric flask, and is quantitative with mobile phase, after reuse microporous filter membrane (0.45um) filters, inject the high performance liquid chromatogram instrument, external standard method is quantitative, gets the content of naringin in full fruit of Exocarpium Citri Grandis or the extractum.Found that the content of naringin is higher than Exocarpium Citri Grandis skin extractum in the full fruit extractum, shows the extraction ratio height of the extraction ratio of full fruit than skin.Can better develop the Exocarpium Citri Grandis raw material resources with full fruit.Simultaneously, the full fruit of Exocarpium Citri Grandis is more extensive than its raw material sources of Exocarpium Citri Grandis skin, and technique for producing raw material is simpler.
Chromatographic condition: Agilent1100 high performance liquid chromatograph (manual injector, 20ul quantitatively encircles, vacuum degassing machine, quaternary pump, column oven, diode array detector), chromatographic column: Hypersil ODS post (5um, 4.0 * 250mm); Mobile phase: methanol-acetic acid-water (35: 4: 61); Detect wavelength: 283nm; 40 ℃ of column temperatures, flow velocity: 1ml/min.
Exocarpium Citri Grandis is the Chinese medicine of preventing phlegm from forming and stopping coughing, we test by pharmacological effect, to the experimentize relieving cough and resolving phlegm of animal white mice of Exocarpium Citri Grandis preparation of the present invention, the result shows: the basic, normal, high dosage gastric infusion of Exocarpium Citri Grandis preparation of the present invention causes the tolerance time of cough to stimulating mice, compare with the blank group, significant prolongation is all arranged, and there were significant differences statistically.Compare with positive control medicine dromethan sheet, tolerance time prolongs, and curative effect is remarkable than the positive drug dromethan.
Exocarpium Citri Grandis preparation of the present invention shows the experiment of reducing phlegm of laboratory animal mice, the basic, normal, high dosage gastric infusion of Exocarpium Citri Grandis preparation of the present invention increases the mouse bronchial juice, compare with the blank group, remarkable increase is all arranged, there were significant differences statistically.Compare with positive control medicine TANKEJING, the mouse bronchial juice is all had remarkable increase, there were significant differences statistically.The pharmacological effect effect of pointing out Exocarpium Citri Grandis preparation of the present invention to have relieving cough and resolving phlegm, and better than positive control curative effect.
Simultaneously, Exocarpium Citri Grandis preparation of the present invention has following characteristics:
(1) convenient drug administration, the patient can finish voluntarily.(2) dose is little, and curative effect is rapid.(3) easy to carry.(4) quality is more stable.
In a word, the young fruit of Exocarpium Citri Grandis preparation employingization of the present invention continent Fructus Citri grandis is fruit or the nearly ripe full medicinal raw material of really making a living entirely, possesses good relieving cough and resolving phlegm effect, and its production method is simple, active ingredient extraction ratio height.Exocarpium Citri Grandis preparation of the present invention adult using dosage be equivalent to 6～9 gram Chinese crude drugs/time, every day 2～3 times.
The specific embodiment
The present invention will be further described below in conjunction with embodiment.
Embodiment 1
The Exocarpium Citri Grandis all-fruit powder is broken, crosses 20 mesh sieves, adds 100 ℃ of water and does not have medical material, extract three times, and each one hour, filter, collect volatile oil simultaneously, merging filtrate and volatile oil add correctives, add the water pondage, make oral liquid.
Embodiment 2
The Exocarpium Citri Grandis all-fruit powder is broken, crosses 20 mesh sieves, adds water and does not have medical material for 100 ℃, extract three times, and each 1 hour, filter, collect volatile oil simultaneously, merging filtrate, the filtrate evaporate to dryness gets brownish black extractum.Extractum adds adjuvant, adds after the mixing again and collects the volatile oil that obtains, and mixing adds an amount of binding agent well known in the art, and it is dry to granulate, and adds lubricant, and tablet machine is pressed into tablet, sugar coating, and packing promptly gets the Exocarpium Citri Grandis sugar coated tablet; Also the granule of making can be added the encapsulated capsule of making of moderate lubrication agent; Also can the granule packing make granule.
Embodiment 3
The Exocarpium Citri Grandis all-fruit powder is broken, crosses 40 mesh sieves, through room temperature water supersound extraction three times, each 30 minutes, filter, merging filtrate, the filtrate Rotary Evaporators boils off solution, brownish black extractum.Extractum is spray dried to powder, crosses about the 100-120 order and sieve, encapsulated, packing promptly gets capsule.
Embodiment 4
The Exocarpium Citri Grandis all-fruit powder is broken, without sieving, boils twice through 60 ℃ of decoctings, and each one day, filter, merging filtrate, filtrate adds chloroform extraction, leaves standstill, and filtrate is divided into two-layer, water layer and chloroform layer, the layer that anhydrates gets chloroform layer.
Fling to chloroform, get blackish green extractum, extractum adds again collects the volatile oil that obtains, mixing, vacuum drying or normal pressure oven dry (crossing the 80-100 mesh sieve).Add debita spissitudo ethanol and make soft material, the system granule, drying adds lubricant, mixing, the tablet machine tabletting becomes tablet, sugar coating, packing promptly gets sugar coated tablet.
Embodiment 5
The Exocarpium Citri Grandis all-fruit powder is broken, crosses 20 mesh sieves, boil three times through 75 ℃ of decoctings, and each 2 hours, filter, merging filtrate, filtrate adds petroleum ether extraction, leaves standstill, and filtrate is divided into two-layer, water layer and petroleum ether layer, the layer that anhydrates gets petroleum ether layer.
Fling to petroleum ether, get blackish green extractum, extractum adds again collects the volatile oil that obtains, mixing, and extractum nature evaporate to dryness is dried to powder.Cross the 100-120 mesh sieve, encapsulated, packing promptly gets capsule.
Embodiment 6
The Exocarpium Citri Grandis all-fruit powder is broken, crosses 40 mesh sieves, boil three times through 75 ℃ of decoctings, and each 3 hours, filter, merging filtrate, filtrate adds ethyl acetate extraction, leaves standstill, and filtrate is divided into two-layer, water layer and ethyl acetate layer, the layer that anhydrates gets ethyl acetate layer.
Rotary Evaporators is flung to ethyl acetate, gets blackish green extractum, and extractum adds collects the volatile oil that obtains, and behind the mixing, extractum normal pressure oven dry again adds the moderate lubrication agent and makes soft material, granulate, and drying, the tablet machine tabletting becomes tablet, film coating, packing promptly gets coated tablet.
Embodiment 7
The Exocarpium Citri Grandis all-fruit powder is broken, do not sieve, and through ultrasound wave water extraction three times, each 1 hour, filtration, merging filtrate, filtrate adds ethanol, leaves standstill, and the filtrate precipitation gets water layer and precipitation, goes to precipitate, and gets water layer.
Heating evaporate to dryness water layer gets brownish black extractum, and extractum adds collects the volatile oil that obtains, mixing.Extractum spray drying again is steamed into powder.Add mixing behind an amount of excipient, packing becomes powder.
Embodiment 8
The Exocarpium Citri Grandis all-fruit powder is broken, does not sieve, and water logging is steeped and extracted three times under the room temperature, and each three days, filter, merging filtrate, filtrate adds ethanol, leaves standstill, and the filtrate precipitation gets water layer and precipitation, and the layer that anhydrates must precipitate.
Precipitation volatilizes, and gets extractum, and extractum adds collects the volatile oil that obtains, mixing.Extractum directly adds excipient again, and behind the correctives etc., mix homogeneously is made granule, and the 8-10 mesh sieve is crossed in dry back, and packing promptly gets granule.
Embodiment 9
The Exocarpium Citri Grandis all-fruit powder is broken, crosses 40 mesh sieves, adds 70% ethanol (percent by volume) reflux, extract, three times, does not have raw medicinal herbs at every turn, filters, merging filtrate leaves standstill, and reclaims ethanol, concentrate extractum, extractum adds excipient, granulate, drying is crossed 8～10 mesh sieves, and granule is made in packing.
Embodiment 10 positive texturing is tangerine and the Exocarpium Citri Grandis extract preparation is produced in Guangxi antitussive pharmacological research 1, laboratory animal: NIH mice, male and female half and half, cleaning grade standard, totally 40.By the ordering of body weight size, select the healthy animal of body weight 17.3～21.5g for use, be divided into four groups at random, 10 every group.If negative control, positive control and the tangerine water extract A of positive texturing, experimental grouies such as Exocarpium Citri Grandis water extract are produced in Guangxi.2, sample source and preparation:
(1) embodiment 1 positive texturing Exocarpium Citri Rubrum extract water solution A: the tangerine extractum water solution A (be equivalent to crude drug content 300mg/ml, dosage is equivalent to crude drug 3000mg/kg body weight) of extracting of positive texturing.
(2) Guangxi is produced Exocarpium Citri Grandis and extracted the extractum aqueous solution: Guangxi is produced Exocarpium Citri Grandis and is extracted extractum aqueous solution (be equivalent to crude drug content 300mg/ml, dosage is equivalent to crude drug 3000mg/kg body weight).
(3) dromethan: tablet, dromethan content are the 15mg/ sheet.Get 2 and be dissolved in 20 ml physiological salines, make suspension, concentration is 3mg/ml, and dosage is the 30mg/kg body weight.
(4) normal saline (sodium chloride injection), NaCl content 0.9%.3, experimental technique: (strong aqua ammonia nebulization)
Behind the mouse stomach 1 hour, begin to accept the strong aqua ammonia spraying.Spray into the strong aqua ammonia aerosol by certain hour, spraying finishes, and takes out mice immediately, observes to have or not the cough reaction.Observe the number of times of coughing in a minute,, can be regarded as " cough is arranged " if occur typical case's cough action (abdominal muscle shrinks or the breast that contracts, and magnifies mouth simultaneously, can cough sound sometimes) person more than 3 times in 1 minute.Otherwise can be regarded as " not having cough ".4, experimentation:
Obtain the spray time (EDT that causes the half mouse cough with sequential method (going up purgation)
50).Calculate the R value, if the R value greater than 130%, illustrates that medicine has antitussive action.If the R value is greater than 150%, then showing has significant antitussive action.Computing formula is as follows:
EDT
50=log
-1(n is a number of animals to c/n in the formula, and c is the summation of rx value, and r is every dosage
The number of animals of group, x is a dosage
The logarithm of (being spray time).)
5, experimental result:
By statistics, positive texturing dried tangerine peel and Guangxi product Exocarpium Citri Grandis extract group half cough time and cough suppressing effect see the following form 1.
Tangerine water extraction gains are produced in tangerine water extract of embodiments of the invention 1 positive texturing and Guangxi, gastric infusion causes that to stimulating mice the tolerance time of cough compares, the tangerine water extract of embodiment 1 positive texturing has significant prolongation to the mice tolerance time, and there were significant differences statistically.And Guangxi product Exocarpium Citri Grandis water extract does not have significant prolongation to the mice tolerance time, does not have significant difference statistically.The full fruit of positive texturing dried tangerine peel of the present invention water extract is described, causes that to stimulating mice the tolerance time of cough and Guangxi product Exocarpium Citri Grandis water extract compare, tolerance time prolongs, and is evident in efficacy.The tangerine made extractum of positive texturing of the present invention, cough suppressing effect is better than Guangxi and produces Exocarpium Citri Grandis extractum.So the above embodiment of the present invention all adopts positive texturing dried tangerine peel.
The positive texturing of table 1. cough suppressing effect tangerine and Guangxi product Exocarpium Citri Grandis extract compares
Group
Dosage (mg/kg) EDT50 (second) R value (%) cough suppressing effect
Code name sample name
1 normal saline 0 11.98--
The tangerine water extract 3,000 17.23 111.7 of 2 positive texturings is invalid
It is effective that Exocarpium Citri Grandis water extract 3,000 13.38 144.2 is produced in 3 Guangxi
4 dromethans 30 18.28 153.0 are effective
Antitussive pharmacological research 1, the laboratory animal of embodiment 11 Exocarpium Citri Grandis different parts extract formulations: the NIH mice, male, cleaning grade standard, totally 75.By the ordering of body weight size, select the healthy animal of body weight 18.9～22.4g for use, be divided into five groups at random, 15 every group.If negative control, positive control and embodiment 1 full fruit water extract, skin B water extract, experimental grouies such as skin C water extract.2, sample source and preparation:
(1) the full fruit of embodiment 1 Exocarpium Citri Grandis is extracted extractum aqueous solution (be equivalent to crude drug content 300mg/ml, dosage is equivalent to crude drug 3000mg/kg body weight).
(2) Exocarpium Citri Grandis skin B the water extracted immersing paste aqueous solution group: skin B the water extracted immersing paste aqueous solution (be equivalent to crude drug content 300mg/ml, dosage is equivalent to crude drug 3000mg/kg body weight).
(3) Exocarpium Citri Grandis skin C the water extracted immersing paste aqueous solution group: skin C the water extracted immersing paste aqueous solution (be equivalent to crude drug content 300mg/ml, dosage is equivalent to crude drug 3000mg/kg body weight).
(4) dromethan: tablet, dromethan content are the 15mg/ sheet.Get 2 and be dissolved in 20 ml physiological salines, make suspension, concentration is 3mg/ml, and dosage is the 30mg/kg body weight.
(5) normal saline (sodium chloride injection) NaCl content 0.9%.3, experimental technique: adopt the strong aqua ammonia nebulization with embodiment 10.4, experimental result:
By statistics, the Exocarpium Citri Grandis skin sees the following form 2 with full berry extract group half cough time and cough suppressing effect.
The cough suppressing effect of the full fruit of table 2. Exocarpium Citri Grandis and the extract of skin relatively
Group
Dosage (mg/kg) EDT50 (second) R value (%) cough suppressing effect
Code name sample name
1 normal saline 0 26.1--
2 embodiment, 1 3,000 45.60 174.7 produce effects
3 skin B water extracts 3,000 33.93 130.0 are effective
4 skin C water extracts 3,000 34.32 131.5 are effective
5 dromethans 30 38.86 148.9 are effective
The embodiments of the invention 1 Exocarpium Citri Grandis full fruit water extract and the Exocarpium Citri Grandis severe edema due to hypofunction of the spleen extract gains, and gastric infusion causes that to stimulating mice the tolerance time of cough and blank group compare, and significant prolongation is all arranged, and there were significant differences statistically.The full fruit of embodiments of the invention 1 Exocarpium Citri Grandis water extract, to stimulating mice to cause that the tolerance time of cough and positive drug contrast dromethan sheet compare, tolerance time prolongs, curative effect is remarkable than positive drug group dromethan, compare with Exocarpium Citri Grandis severe edema due to hypofunction of the spleen extract group, tolerance time prolongs, and it is remarkable that curative effect is extracted the extractum group than the severe edema due to hypofunction of the spleen.
Antitussive pharmacological research 1, the laboratory animal of embodiment 12 different dosing dosage: the NIH mice, female, body weight 17.4～21.3g, cleaning grade standard, totally 75.By the ordering of body weight size, be divided into five groups at random, 15 every group.If negative control, high, medium and low three dosage groups of positive control and Exocarpium Citri Grandis preparation A.2, sample source and preparation:
(1) embodiment 1 Exocarpium Citri Grandis preparation A: the Exocarpium Citri Grandis aqueous extract is condensed into extractum, and amounting to crude drug content is 300mg/ml.
(2) high dose group: get the direct administration of Exocarpium Citri Grandis preparation A (be equivalent to crude drug content 300mg/ml, dosage is equivalent to crude drug 3000mg/kg body weight).
(3) dosage group in: get Exocarpium Citri Grandis preparation A, add normal saline, by dilution back administration (be equivalent to crude drug content 100mg/ml, dosage is equivalent to crude drug 1000mg/kg body weight) in 1: 2.
(4) low dose group: get Exocarpium Citri Grandis preparation A, add normal saline, by dilution in 1: 8, dilution back administration (be equivalent to crude drug content 33mg/ml, dosage is equivalent to crude drug 330mg/kg body weight).
(5) positive thing adopts dromethan: tablet, dromethan content are the 15mg/ sheet.Get 2 and be dissolved in 20 ml physiological salines, make suspension, concentration is 3mg/ml, and dosage is the 30mg/kg body weight.
(6) normal saline (sodium chloride injection), NaCl content 0.9%.3, experimental technique: adopt the strong aqua ammonia nebulization with embodiment 10.4, experimental result:
By statistics, each dosage group half cough time and cough suppressing effect see the following form 3.
The cough suppressing effect of table 3. Exocarpium Citri Grandis water extraction extractum
Group
Dosage (mg/kg) EDT50 (second) R value (%) cough suppressing effect
Code name sample name
1 normal saline 0 29.08--
2 dromethan sheets 30 38.98 134.04 are effective
3 Exocarpium Citri Grandis extractum high dose group, 3,000 45.14 155.27 produce effects
Dosage group 1,000 41.82 143.81 is effective in the 4 Exocarpium Citri Grandis extractum
5 Exocarpium Citri Grandis extractum low dose group 330 10.47 139.17 are effective
The basic, normal, high dosage gastric infusion of Exocarpium Citri Grandis preparation of the present invention causes that to stimulating mice the tolerance time of cough and blank group compare, and significant prolongation is all arranged, and there were significant differences statistically.Compare with positive drug contrast dromethan sheet, tolerance time prolongs, and curative effect is remarkable than positive drug group dromethan.
Embodiment 13 different antitussive pharmacological research 1, the laboratory animals of extracting composition: the NIH mice, female, cleaning grade standard, totally 105.By the ordering of body weight size, select the healthy animal of body weight 18.1-22.1g for use, be divided into six groups at random, 15 every group.If negative control, positive control becomes grouping with Petroleum ether extraction; Chloroform extraction becomes grouping; Ethyl acetate extraction becomes grouping; The water extracting component group.2, sample source and preparation:
(1) embodiment 5 Petroleum ether extraction become grouping: Petroleum ether extraction extractum aqueous solution (be equivalent to crude drug content 300mg/ml, dosage is equivalent to crude drug 3000mg/kg body weight).
(2) embodiment 4 chloroform extraction become grouping: chloroform extraction extractum aqueous solution (be equivalent to crude drug content 300mg/ml, dosage is equivalent to crude drug 3000mg/kg body weight).
(3) embodiment 6 ethyl acetate extractions become grouping: ethyl acetate extraction extractum aqueous solution (be equivalent to crude drug content 300mg/ml, dosage is equivalent to crude drug 3000mg/kg body weight).
(4) embodiment 1 water is extracted into grouping: water extraction solution (be equivalent to crude drug content 300mg/ml, dosage is equivalent to crude drug 3000mg/kg body weight).
(5) dromethan: tablet, dromethan content are the 15mg/ sheet.Get 2 and be dissolved in 20 ml physiological salines, make suspension, concentration is 3mg/ml, and dosage is the 30mg/kg body weight.
(6) normal saline (sodium chloride injection), NaCl content 0.9%.3, experimental technique: adopt the strong aqua ammonia nebulization with embodiment 10.4, experimental result:
By statistics, respectively be extracted into grouping half cough time and cough suppressing effect and see the following form 4.
Exocarpium Citri Grandis water extraction extractum of the present invention and through the separating obtained extractum of various organic solvents, gastric infusion causes the tolerance time and the comparison of blank group of cough to stimulating mice, and significant prolongation is all arranged, there were significant differences statistically.Compare with positive drug contrast dromethan sheet, tolerance time prolongs, and curative effect is remarkable than positive drug group dromethan.The same test of embodiment 9 shows that the result of the test of embodiment 9 for poor, shows the preparation poor effect of the effective ingredient of organic solvent extraction than embodiment 1.
Table 4. Exocarpium Citri Grandis respectively extracts the cough suppressing effect of composition
Group dosage
EDT50 (second) R value (%) cough suppressing effect
Code name sample name (mg/kg)
1 normal saline 0 27.54--
2 embodiment, 1 water is put forward solution 3,000 50.12 181.99 produce effects
3 embodiment, 5 petroleum ether deduction branch 3,000 35.80 129.99 is effective
4 embodiment, 6 ethyl acetate compositions 3,000 38.31 139.11 are effective
5 embodiment, 4 chloroform compositions, 3,000 41.82 151.85 produce effects
6 dromethans, 30 44.67 162.22 produce effects
Apophlegmatisant pharmacological research 1, the laboratory animal of embodiment 14 different dosing dosage: the NIH mice, male, body weight 17.9-22.1g, cleaning grade standard, totally 60.By the ordering of body weight size, be divided into five groups at random, 10 every group.If negative control, high, medium and low three the dosage groups of positive control and H7.All by oral administration of filling stomach amount of 10ml/kg body weight.2, sample source and preparation:
(1) embodiment 1 Exocarpium Citri Grandis preparation A: the Exocarpium Citri Grandis aqueous extract is condensed into extractum, and amounting to crude drug content is 300mg/ml.
(2) high dose group: get the direct administration of Exocarpium Citri Grandis preparation A (be equivalent to crude drug content 300mg/ml, dosage is equivalent to crude drug 3000mg/kg body weight).
(3) dosage group in: get Exocarpium Citri Grandis preparation A, add normal saline, by dilution back administration (be equivalent to crude drug content 100mg/ml, dosage is equivalent to crude drug 1000mg/kg body weight) in 1: 2.
(4) low dose group: get Exocarpium Citri Grandis preparation A, add normal saline, by dilution in 1: 8, dilution back administration (be equivalent to crude drug content 33mg/ml, dosage is equivalent to crude drug 330mg/kg body weight).
(5) positive thing adopts TANKEJING: powder, and get 0.2 gram and be dissolved in 10 ml physiological salines, promptly get positive control TANKEJING solution, concentration is 20mg/ml.Dosage is the 200mg/kg body weight.
(6) normal saline (sodium chloride injection), NaCl content 0.9%.3, experimental technique: (phenol red method)
(1) water 12h is can't help in the mice fasting.
(2) gastric infusion.By the animal order, stopped behind every mouse stomach 3 minutes, irritate other one again, interval is 3 minutes, 10 every group are irritated the stomach time altogether is 30 minutes.
(3) half an hour behind each Mus filling stomach is through lumbar injection 5% phenol red normal saline solution 0.2ml.In order, promptly each mouse peritoneal was injected phenol red back 3 minutes, injected other one again, 10 mices totally 30 minutes.
(4) half an hour behind each Mus lumbar injection, take off cervical vertebra in order and put to death mice, put to death interval 3 minutes.Behind the sacrifice of animal, face upward the position and be fixed on the operation plate, cut off neck center skin, separate trachea, prop trachea with pincet.
(5) draw normal saline flushing trachea outer wall with big syringe, phenol red in flush away blood and the trachea outer wall, filter paper blots washing liquid.
(6) cut trachea prior to the trachea bifurcation, cut trachea (the ring-type thyroid cartilage is included) in other end thyroid cartilage upper end again.
(7) each trachea section is put into the 5%NaHCO that fills 1.5ml in advance
3In the solution test tube.
(8) in 3 minutes, finish above-mentioned tracheorrhaphy from shearing work.Reuse is handled second mice with quadrat method.Method as above.
(9) each test tube is put on the vortex mixer concussion 2 minutes, made phenol red the discharging in the trachea section.
(10) solution in each test tube is surveyed the OD value in 721 type spectrophotometer 546nm places.
(11) the OD value of resurveying behind the 24h is spent the night in each test tube gassiness pipeline section placement.
(12) with the phenol red aqueous solution that is mixed with different content, measure the OD value, calculate regression equation and be: Y=-0.135302794+14.19137583X.Range of linearity 0.1ng/ml～10ng/ml, r=0.9999.X is the OD value, and Y is phenol red content.X is the OD value, and Y is phenol red content.
(13) go out each animal trachea phenol red output (phenol red content) according to regression equation calculation.
(14) phenol red content and the weight of animals calculate and proofread and correct phenol red content, carry out variance analysis with the SPSS8.0 statistical software.Proofread and correct phenol red content=phenol red content (ng)/mice body weight (kg) 4, result's judgement:
Each group result is carried out variance analysis, when overall when variant,, determine that experiment reliably if positive drug and matched group relatively, are proofreaied and correct phenol red content and raise, and significant difference (P＜0.05) is arranged.With each dosage group and matched group relatively, proofread and correct phenol red content and obviously raise again, and when significant difference (P＜0.05) is arranged, think that this dosage group is effective.5, experimental result:
By statistics, each dosage group of water extraction extractum phenol red output, see the following form 5.
The effect of reducing phlegm of each dosage of table 5. Exocarpium Citri Grandis water extract (X ± S)
Group dosage animal trachea phenol is proofreaied and correct phenol red content
aThe rate of reducing phlegm
b
The red content of code name sample name (mg/kg) (ng) is P value (%) (ng/kg)
1 normal saline 0 1.6792 ± 0.4379 84.7774 ± 21.0409--
2 TANKEJING 200 2.6073 ± 0.5986 132.0956 ± 32.0495 P＜0.05 155.78
3 embodiment, 1 high dose group, 3,000 3.1702 ± 0.7423 158.6855 ± 34.8674 P＜0.01 187.15
Dosage group 1,000 3.1267 ± 1.4389 160.3666 ± 78.3494 P＜0.01 189.16 among 4 embodiment 1
5 embodiment, 1 low dose group 330 2.7414 ± 0.7917 139.6466 ± 42.4319 P＜0.05 164.72
A: proofread and correct phenol red content=phenol red content/the weight of animals
B: the rate of reducing phlegm=administration group/blank group * 100%
Phenol red cubage method (ng): OD value * 14.19137583-0.135302794
Exocarpium Citri Grandis preparation of the present invention shows the experiment of reducing phlegm of laboratory animal mice, the mouse bronchial juice is increased the basic, normal, high dosage gastric infusion of Exocarpium Citri Grandis preparation of the present invention and the blank group compares, remarkable increase is all arranged, and there were significant differences statistically.Compare with the positive drug TANKEJING, embodiment height, middle dosage group have remarkable increase to the mouse bronchial juice, and there were significant differences statistically.Show that embodiment 1 effect of reducing phlegm is better than the positive control TANKEJING.Through test, other embodiment of the present invention show to possess similar effect to embodiment 1.
In sum, illustrate that Exocarpium Citri Grandis preparation of the present invention agent has good relieving cough and resolving phlegm effect.
Claims (10)
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101129536B (en) * | 2006-08-21 | 2010-09-08 | 广东环球制药有限公司 | Membrane separation method for preparing flavone extractive of Huazhou pummelo |
| CN101279002B (en) * | 2007-04-03 | 2011-09-14 | 化州市绿色生命有限公司 | Medicament for relieving cough and eliminating phlegm and method of preparing the same |
| CN106721864A (en) * | 2016-12-15 | 2017-05-31 | 广东石油化工学院 | A kind of clearing Exocarpium Citri Grandis effervescent tablet |
| CN108740677A (en) * | 2018-06-22 | 2018-11-06 | 化州化橘红药材发展有限公司 | A kind of Exocarpium Citri Grandis slow-release solid beverage and preparation method thereof |
| CN109330016A (en) * | 2018-11-14 | 2019-02-15 | 河南中烟工业有限责任公司 | A kind of Exocarpium Citri Grandis medicinal extract, preparation method and the application in cigarette |
| CN109512880A (en) * | 2019-01-14 | 2019-03-26 | 广州市香雪制药股份有限公司 | A kind of sucking preparation and preparation method thereof, application |
| CN112998265A (en) * | 2021-05-13 | 2021-06-22 | 广东南粤药业有限公司 | Exocarpium citri grandis composition with cough relieving and phlegm reducing effects and preparation method thereof |
| CN114452326A (en) * | 2022-02-21 | 2022-05-10 | 广东粤微食用菌技术有限公司 | Exocarpium Citri Grandis extract with cough relieving and phlegm eliminating effects and high yield extraction method |
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2002
- 2002-02-08 CN CNB021148473A patent/CN1186051C/en not_active Expired - Lifetime
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101129536B (en) * | 2006-08-21 | 2010-09-08 | 广东环球制药有限公司 | Membrane separation method for preparing flavone extractive of Huazhou pummelo |
| CN101279002B (en) * | 2007-04-03 | 2011-09-14 | 化州市绿色生命有限公司 | Medicament for relieving cough and eliminating phlegm and method of preparing the same |
| CN106721864A (en) * | 2016-12-15 | 2017-05-31 | 广东石油化工学院 | A kind of clearing Exocarpium Citri Grandis effervescent tablet |
| CN108740677A (en) * | 2018-06-22 | 2018-11-06 | 化州化橘红药材发展有限公司 | A kind of Exocarpium Citri Grandis slow-release solid beverage and preparation method thereof |
| CN109330016A (en) * | 2018-11-14 | 2019-02-15 | 河南中烟工业有限责任公司 | A kind of Exocarpium Citri Grandis medicinal extract, preparation method and the application in cigarette |
| CN109512880A (en) * | 2019-01-14 | 2019-03-26 | 广州市香雪制药股份有限公司 | A kind of sucking preparation and preparation method thereof, application |
| CN109512880B (en) * | 2019-01-14 | 2021-07-09 | 广州市香雪制药股份有限公司 | Inhalation preparation and preparation method and application thereof |
| CN112998265A (en) * | 2021-05-13 | 2021-06-22 | 广东南粤药业有限公司 | Exocarpium citri grandis composition with cough relieving and phlegm reducing effects and preparation method thereof |
| CN114452326A (en) * | 2022-02-21 | 2022-05-10 | 广东粤微食用菌技术有限公司 | Exocarpium Citri Grandis extract with cough relieving and phlegm eliminating effects and high yield extraction method |
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| CN1186051C (en) | 2005-01-26 |
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