CN108997472A - The preparation method of chonglou saponin XI and its application in treatment tonsillitis - Google Patents
The preparation method of chonglou saponin XI and its application in treatment tonsillitis Download PDFInfo
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Abstract
The invention proposes the preparation methods of chonglou saponin XI a kind of, it prepares in accordance with the following methods: S1, weighing Paris polyphylla coarse powder, buffer solution, hyperbaric heating extraction is added, it is cooling, cellulase and amylase, ultrasonic wave assisted extraction, the extraction of ethyl acetate-light petrol mixed solution is added, filtering, it is concentrated under reduced pressure, is mixed with silica gel, obtain Paris polyphylla silica white；S2, by silicagel column on Paris polyphylla silica white, eluted with the mixed liquor of chloroform and methanol, obtain eluted product, thin layer chromatography analysis merges mutually same, obtains chonglou saponin XI study, is concentrated under reduced pressure, obtains chonglou saponin XI and study is concentrated；S3, reverse phase silica gel column on study is concentrated in chonglou saponin XI, is eluted with methanol solution, thin layer chromatography analysis, mutually same to merge, after petroleum ether degreasing, ethyl acetate-acetone extraction is concentrated under reduced pressure to get chonglou saponin XI.Chonglou saponin XI prepared by the present invention is applied to treatment tonsillitis, is had a significant effect.
Description
Technical field
The present invention relates to technical field of traditional Chinese medicine pharmacy, and in particular to the preparation method of chonglou saponin XI a kind of and its is treating
Application in tonsillitis.
Background technique
Tonsillitis typically refer to positioned at throat tonsillotome occur nonspecific inflammation, be mostly due to virus or
Caused by bacterium infection.It is clinically to show as antiadoncus, hyperemia more, there is an a large amount of neutrophil infiltration, and with
It the symptoms such as generates heat, have sore throat.Clinically tonsillitis is treated using antibiotics, due to drug-fast bacteria instantly
Be continuously increased, remission is slower, and therapeutic effect is unsatisfactory, is easy to cause various complication, cause neighbouring organ by
To infection.
Hug again be Liliaceae (Lilliaccae) Paris (Paris) various plants rhizome, have it is clearing heat and detoxicating, detumescence
The effect of analgesic, cool liver arresting convulsion, modern pharmacological research its with more antitumor, the pharmacological activity such as hemostasis, anti-inflammatory, active constituent
For Chinese paris rhizome total saponin.It is mainly distributed on the ground such as Yunnan Province of China, Guangxi, Sichuan.Xiao Mei virtue et al. has inquired into chonglou saponin I in vitro
To influence and the related mechanism of SMMC-7721 cell line proliferation and apoptosis.Studies have shown that chonglou saponin I can the time and
The proliferation of the inhibition SMMC-7721 liver cancer cells of concentration dependent, it may be possible to the growth that chonglou saponin I passes through blocks tumor cells
And the mechanism such as induce cell apoptosis, to inhibit the proliferation of liver cancer cells.(the increasing of Xiao Meifang etc., chonglou saponin I to liver cancer cells
It grows and the influence life science .2011 of apoptosis, 15 (6): 519) 50 μm of ol/L chonglou saponin Ⅱ solution can press down in vitro
Lupus nephritis local immunity reaction processed, it may be possible to by the expression quantity for improving TGF-β albumen and IL-10 albumen in lymphocyte
Th1/Th2 is unbalance adjusting, and then improves the immunosuppressive action of CD4+CD25+Treg (Wang Juan etc., pariphyllin II is to lupus
Property nephritis patient peripheral blood CD4+CD25+T adjust cell expression cell factor influence .2010,10 (1): 50).
Chonglou saponin XI (23S, 25S) -3 β, 23,27-trihydroxyspirost-5en-3O- β-D-
Glucopyranosyl- (1 → 6)-β-D-glucopyranoside is main in a kind of important steroid saponin and Paris polyphylla
One of functional component, medical value with higher, it is also famous Chinese patent drug Yunnan Baiyao, Ji Desheng snake medicine and Gong Xue Ning
The main composition drug of capsule etc..TNF- in multiple trauma model Wistar rat blood serum can be significantly reduced in Chinese paris rhizome total saponin
The content of α, IL-1 β and IL-6 cell factor, so that (the Paris polyphylla such as Ling Li is total for the damage for mitigating its lung and local inflammation reaction
Influence of the saponin(e to multiple trauma rat blood serum cytokine levels, 2009,11 (6): 241).But currently, to chonglou saponin
The report of XI is less, and especially applying it to is even more to be rarely reported in the drug for the treatment of tonsillitis.In mentioning for chonglou saponin
Take aspect at present mostly based on the extraction of Chinese paris rhizome total saponin or several saponin mixtures, functional component is uncertain, and exists and extract
The problems such as technology is loaded down with trivial details, low efficiency and not high purity.
Seedling medicine Paris polyphylla and anaesthetic fohum aconiti kusnezoffii, black cloud incense have a significant effect in treatment tonsillitis, by itself and other
Chinese medicine compounding, Chinese medicine composition obtained have good curative effect in treatment antiadoncus, hyperemia, tonsillitis.Its
In, Paris polyphylla anti-inflammatory goes to swell, the clearing heat and detoxicating analgesic of elecampane fohum aconiti kusnezoffii, black cloud incense collaboration anti-inflammatory analgetic, with other a few herbs materials
Compound is with medicine is combined, and effect is more preferably.
Summary of the invention
In order to solve the above technical problems, the present invention provides the preparation method of a kind of chonglou saponin XI and its flat treating
Application in peach body inflammation is extracted, ultrasonic wave is auxiliary it is intended that providing the preparation method of chonglou saponin XI a kind of by high pressure
Mixed enzyme is helped to extract, multiple silica gel column purification, obtained chonglou saponin XI is (can reach 98% or more) with high purity, yield height (92-
95%), and method is easy, does not need harsh experiment condition, at low cost, it is easy to accomplish industrial applications.
The present invention provides the preparation method of chonglou saponin XI a kind of, prepares in accordance with the following methods:
Step 1: weighing Paris polyphylla coarse powder, the buffer solution of certain volume is added, is placed in the heating extraction of autoclave mesohigh,
After extraction, be cooled to 50 DEG C, be added a certain amount of cellulase and amylase, ultrasonic wave assisted extraction after a certain period of time,
High temperature fire extinguishing 5min, three times with the extraction of ethyl acetate-light petrol mixed solution, filtering, merging filtrate, vacuum rotary steam concentration, with
Silica gel mixing, obtains Paris polyphylla silica white；
Step 2: by step 1 preparation Paris polyphylla silica white on silicagel column, with the mixed liquor of chloroform and methanol to product into
Row elution, obtains eluted product, obtained eluted product is carried out thin-layer chromatography, under ultraviolet light observation colour developing, with Paris polyphylla soap
The standard specimen of glycosides XI compares, and finds out and extract the study containing chonglou saponin XI, and merging is mutually same, obtains chonglou saponin XI study, subtracts
Pressure concentration obtains chonglou saponin XI concentration study；
Step 3: reverse phase silica gel column on the chonglou saponin XI concentration study that step 3 is obtained, with methanol solution to described
Study elution is concentrated in chonglou saponin XI, continues thin-layer chromatography, under ultraviolet light observation colour developing, the standard specimen with chonglou saponin XI
Comparison, merges without the sample of other impurities by spot identical with the standard specimen of chonglou saponin XI and in observed under fluorescent light, must contain
The methanol solution of the purified product of the chonglou saponin XI, after the solution petroleum ether degreasing, ethyl acetate-acetone extraction subtracts
Pressure concentration removes solvent to get chonglou saponin XI.
As further improvement of the invention, the purity of chonglou saponin XI is 98% or more, the chonglou saponin XI
Rate is 92%-98%.
As further improvement of the invention, buffer solution described in step 1 is the Na of pH=4.62HPO4Citric acid is slow
Rush solution；The grain of the Paris polyphylla coarse powder is through number between 24-60 mesh；The solid-to-liquid ratio of the Paris polyphylla coarse powder and buffer solution is 1:
(15-25)。
As further improvement of the invention, high pressure described in step 1 is 1.5-2 atmospheric pressure, and temperature is 70-90 DEG C,
Extraction time is 60-90min.
As further improvement of the invention, extraction time described in step 1 is 120-180min；The ultrasonic power
For 600-800W；The cellulase dosage is (30-50) U/g substrate, and starch enzyme dosage is (10-15) U/g substrate.
As further improvement of the invention, silica gel described in step 1 is 100-200 mesh；The ethyl acetate-pet
The volume ratio of ether mixed solution is (1-5): 2.
As further improvement of the invention, silica gel described in step 2 is 200-300 mesh；The elution is washed for gradient
It is de-；The proportion of the chloroform and methanol is followed successively by 100:1,30:1,20:1,10:1,1:1.
As further improvement of the invention, elution described in step 3 is gradient elution；The quality of the methanol solution
Score is followed successively by 80%, 85% and 100%, and the volume ratio of the ethyl acetate-acetone is 1:(1-7).
As further improvement of the invention, ultraviolet light described in step 2 and step 3 is 254nm.
The present invention further protects a kind of above-mentioned Chinese medicine composition for treating tonsillitis, and the composition is by including following
The raw material of parts by weight is prepared: 25 parts of chonglou saponin XI；22 parts of schizonepeta；20 parts of Radix Mussaendae；20 parts of radix glycyrrhizae preparata；Honey 17
Part；15 parts of rhizoma anemarrhenae；15 parts of the root of Dahurain angelica；12 parts of fritillaria thunbergii；10 parts of fohum aconiti kusnezoffii；10 parts of black cloud incense；7 parts of FLOS CHRYSANTHEMI ALBA from Haizhou of China；5 parts of peppermint.
The present invention further protects a kind of preparation method of above-mentioned Chinese medicine composition for treating tonsillitis, according to following step
Rapid preparation:
Step 1: take schizonepeta, Radix Mussaendae, radix glycyrrhizae preparata, rhizoma anemarrhenae, the root of Dahurain angelica, fritillaria thunbergii, fohum aconiti kusnezoffii, black cloud incense, FLOS CHRYSANTHEMI ALBA from Haizhou of China,
Peppermint dries, crush after mix, 8-10 times of volume of water is added, impregnates 60-120min, decocts 120-180min, is filtered under diminished pressure, filters
Liquid is spare；
Step 2: decocting 60-90min by 5-7 times of volume of water is added in the dregs of a decoction obtained by step 1, being filtered under diminished pressure, filtrate is standby
With；
Step 3: filtrate obtained by step 1 and step 2 is merged, 400 meshes are crossed, honey and chonglou saponin XI is added, are mixed
It closes uniformly, concentration filtrate to relative density is 1.3-1.7, adds auxiliary material, is prepared into regular dosage form.
Improved as of the invention further, auxiliary material be selected from maltodextrin, starch, starch slurry, mannitol, calcium monohydrogen phosphate,
Silica, magnesium stearate, microcrystalline cellulose, sodium carboxymethylcellulose, talcum powder, Macrogol 4000, Macrogol 6000,
One or more of ethyl alcohol, superfine silica gel powder.
As further improvement of the invention, regular dosage form includes pulvis, granule, pill, tablet and capsule.
The invention has the following beneficial effects:
1. the chonglou saponin XI that the present invention is prepared is (can reach 98% or more) with high purity, yield is high, and method is easy,
Harsh experiment condition is not needed, it is at low cost, it is easy to accomplish industrial applications；
2. chonglou saponin XI has clear hemostasis and anti-inflammation and treats the activity of tonsillitis, can heat toxin sore carbuncle, throat it is swollen
Bitterly, clearing heat and promoting diuresis, removing toxicity for detumescence, with schizonepeta, Radix Mussaendae, radix glycyrrhizae preparata, rhizoma anemarrhenae, the root of Dahurain angelica, fritillaria thunbergii, fohum aconiti kusnezoffii, black cloud incense, Hangzhoupro
Feverfew, peppermint, honey compound prescription, can significantly mitigate throat antiadoncus, congestive symptom, so that patient temperature restores
Normally, pharyngalgia and purulent secretion disappear, and clinical symptoms completely disappear；
3. instant component is all made of natural Chinese medicine material, and preparation is easy, medicine source is wide, and treatment tonsillitis effect is aobvious
It writes, short treating period is at low cost, and has no toxic side effect.
Detailed description of the invention
Fig. 1 is the preparation technology figure of Paris polyphylla saponins X I；
Fig. 2 is the high-efficient liquid phase chromatogram of Paris polyphylla saponins X I.
Specific embodiment
Below in conjunction with the embodiment of the present invention, the technical scheme in the embodiment of the invention is clearly and completely described,
Obviously, the embodiment described is the embodiment of part of representative of the invention, rather than whole embodiments, this field are general
Other all embodiments obtained belong to protection of the invention to logical technical staff without making creative work
Range.
The preparation of 1 chonglou saponin XI of embodiment
It prepares in accordance with the following methods:
Step 1: weighing 24 mesh Paris polyphylla coarse powder, the Na of pH=4.6 is added2HPO4Citric acid solution (solid-to-liquid ratio 1:
15) 70 DEG C of extraction 60min of autoclave mesohigh (1.5 atmospheric pressure), are placed in, after extraction, 50 DEG C is cooled to, 30U/ is added
The cellulase of g substrate and the amylase of 10U/g substrate, after 600W ultrasonic wave assisted extraction 120min, high temperature is put out a fire 5min, is used
Ethyl acetate-light petrol (volume ratio 1:2) mixed solution extracts filtering three times, merging filtrate, vacuum rotary steam concentration, with 100-
The silica gel of 200 mesh mixes, and obtains Paris polyphylla silica white；
Step 2: by silicagel column on the Paris polyphylla silica white of step 1 preparation (silica gel is 200-300 mesh), with chloroform and methanol
Mixed liquor gradient elution is carried out to product, the proportion of chloroform and methanol is followed successively by 100:1,30:1,20:1,10:1,1:1, obtains
To eluted product, obtained eluted product is subjected to thin-layer chromatography, colour developing is observed at ultraviolet light (254nm), with chonglou saponin
The standard specimen of XI compares, and finds out and extract the study containing chonglou saponin XI, and merging is mutually same, obtains chonglou saponin XI study, depressurizes
Concentration obtains chonglou saponin XI concentration study；
Step 3: reverse phase silica gel column on the chonglou saponin XI concentration study that step 3 is obtained, with methanol solution to Paris polyphylla
Study gradient elution is concentrated in saponins X I, and the mass fraction of methanol solution is followed successively by 80%, 85% and 100%, continues thin layer
Chromatography observes colour developing at ultraviolet light (254nm), compares with the standard specimen of chonglou saponin XI, by the standard specimen phase with chonglou saponin XI
With spot and merge in observed under fluorescent light without the sample of other impurities, the methanol for obtaining the purified product containing chonglou saponin XI is molten
Liquid, after the solution petroleum ether degreasing, ethyl acetate-acetone (volume ratio 1:1) extraction is concentrated under reduced pressure and removes solvent to get weight
Building saponins X I, yield 98%.
The preparation of 2 chonglou saponin XI of embodiment
It prepares in accordance with the following methods:
Step 1: weighing 60 mesh Paris polyphylla coarse powder, the Na of pH=4.6 is added2HPO4Citric acid solution (solid-to-liquid ratio 1:
25) 90 DEG C of extraction 90min of autoclave mesohigh (2 atmospheric pressure), are placed in, after extraction, 50 DEG C is cooled to, 50U/g is added
The cellulase of substrate and the amylase of 15U/g substrate, after 800W ultrasonic wave assisted extraction 180min, high temperature is put out a fire 5min, is used
Ethyl acetate-light petrol (volume ratio 5:2) mixed solution extracts filtering three times, merging filtrate, vacuum rotary steam concentration, with 100-
The silica gel of 200 mesh mixes, and obtains Paris polyphylla silica white；
Step 2: by silicagel column on the Paris polyphylla silica white of step 1 preparation (silica gel is 200-300 mesh), with chloroform and methanol
Mixed liquor gradient elution is carried out to product, the proportion of chloroform and methanol is followed successively by 100:1,30:1,20:1,10:1,1:1, obtains
To eluted product, obtained eluted product is subjected to thin-layer chromatography, colour developing is observed at ultraviolet light (254nm), with chonglou saponin
The standard specimen of XI compares, and finds out and extract the study containing chonglou saponin XI, and merging is mutually same, obtains chonglou saponin XI study, depressurizes
Concentration obtains chonglou saponin XI concentration study；
Step 3: reverse phase silica gel column on the chonglou saponin XI concentration study that step 3 is obtained, with methanol solution to Paris polyphylla
Study gradient elution is concentrated in saponins X I, and the mass fraction of methanol solution is followed successively by 80%, 85% and 100%, continues thin layer
Chromatography observes colour developing at ultraviolet light (254nm), compares with the standard specimen of chonglou saponin XI, by the standard specimen phase with chonglou saponin XI
With spot and merge in observed under fluorescent light without the sample of other impurities, the methanol for obtaining the purified product containing chonglou saponin XI is molten
Liquid, after the solution petroleum ether degreasing, ethyl acetate-acetone (volume ratio 1:7) extraction is concentrated under reduced pressure and removes solvent to get weight
Building saponins X I, yield 92%.
The preparation of 3 chonglou saponin XI of embodiment
It prepares in accordance with the following methods:
Step 1: weighing 24 mesh Paris polyphylla coarse powder, the Na of pH=4.6 is added2HPO4Citric acid solution (solid-to-liquid ratio 1:
20) 80 DEG C of extraction 80min of autoclave mesohigh (2 atmospheric pressure), are placed in, after extraction, 50 DEG C is cooled to, 40U/g is added
The cellulase of substrate and the amylase of 12U/g substrate, after 700W ultrasonic wave assisted extraction 150min, high temperature is put out a fire 5min, is used
Ethyl acetate-light petrol (volume ratio 3:2) mixed solution extracts filtering three times, merging filtrate, vacuum rotary steam concentration, with 100-
The silica gel of 200 mesh mixes, and obtains Paris polyphylla silica white；
Step 2: by silicagel column on the Paris polyphylla silica white of step 1 preparation (silica gel is 200-300 mesh), with chloroform and methanol
Mixed liquor gradient elution is carried out to product, the proportion of chloroform and methanol is followed successively by 100:1,30:1,20:1,10:1,1:1, obtains
To eluted product, obtained eluted product is subjected to thin-layer chromatography, colour developing is observed at ultraviolet light (254nm), with chonglou saponin
The standard specimen of XI compares, and finds out and extract the study containing chonglou saponin XI, and merging is mutually same, obtains chonglou saponin XI study, depressurizes
Concentration obtains chonglou saponin XI concentration study；
Step 3: reverse phase silica gel column on the chonglou saponin XI concentration study that step 3 is obtained, with methanol solution to Paris polyphylla
Study gradient elution is concentrated in saponins X I, and the mass fraction of methanol solution is followed successively by 80%, 85% and 100%, continues thin layer
Chromatography observes colour developing at ultraviolet light (254nm), compares with the standard specimen of chonglou saponin XI, by the standard specimen phase with chonglou saponin XI
With spot and merge in observed under fluorescent light without the sample of other impurities, the methanol for obtaining the purified product containing chonglou saponin XI is molten
Liquid, after the solution petroleum ether degreasing, ethyl acetate-acetone (volume ratio 1:5) extraction is concentrated under reduced pressure and removes solvent to get weight
Building saponins X I, yield 95%.
A kind of preparation for the Chinese medicine composition for treating tonsillitis of embodiment 4
Raw material composition: 25 parts of chonglou saponin XI；22 parts of schizonepeta；20 parts of Radix Mussaendae；20 parts of radix glycyrrhizae preparata；17 parts of honey；Know
It is 15 parts female；15 parts of the root of Dahurain angelica；12 parts of fritillaria thunbergii；10 parts of fohum aconiti kusnezoffii；10 parts of black cloud incense；7 parts of FLOS CHRYSANTHEMI ALBA from Haizhou of China；5 parts of peppermint.
Preparation method:
Step 1: take schizonepeta, Radix Mussaendae, radix glycyrrhizae preparata, rhizoma anemarrhenae, the root of Dahurain angelica, fritillaria thunbergii, fohum aconiti kusnezoffii, black cloud incense, FLOS CHRYSANTHEMI ALBA from Haizhou of China,
Peppermint dries, crush after mix, 8 times of volume of water are added, impregnate 60min, decocts 120min, is filtered under diminished pressure, filtrate is spare；
Step 2: decocting 60min by 5 times of volume of water are added in the dregs of a decoction obtained by step 1, being filtered under diminished pressure, filtrate is spare；
Step 3: filtrate obtained by step 1 and step 2 is merged, 400 meshes are crossed, honey and chonglou saponin XI is added, are mixed
It closes uniformly, concentration filtrate to relative density is 1.3, adds auxiliary material maltodextrin, and spray drying obtains solid medicinal powder.
A kind of preparation of the Chinese medicine composition of the treatment tonsillitis without chonglou saponin XI of embodiment 6
Raw material composition: 22 parts of schizonepeta；20 parts of Radix Mussaendae；20 parts of radix glycyrrhizae preparata；17 parts of honey；15 parts of rhizoma anemarrhenae；15 parts of the root of Dahurain angelica；
12 parts of fritillaria thunbergii；10 parts of fohum aconiti kusnezoffii；10 parts of black cloud incense；7 parts of FLOS CHRYSANTHEMI ALBA from Haizhou of China；5 parts of peppermint.
Preparation method:
Step 1: take schizonepeta, Radix Mussaendae, radix glycyrrhizae preparata, rhizoma anemarrhenae, the root of Dahurain angelica, fritillaria thunbergii, fohum aconiti kusnezoffii, black cloud incense, FLOS CHRYSANTHEMI ALBA from Haizhou of China,
Peppermint dries, crush after mix, 10 times of volume of water are added, impregnate 120min, decocts 180min, is filtered under diminished pressure, filtrate is spare；
Step 2: decocting 90min by 7 times of volume of water are added in the dregs of a decoction obtained by step 1, being filtered under diminished pressure, filtrate is spare；
Step 3: filtrate obtained by step 1 and step 2 is merged, 400 meshes are crossed, honey is added, are uniformly mixed, concentration
Filtrate to relative density is 1.7, adds auxiliary material maltodextrin, and spray drying obtains the solid medicinal powder without chonglou saponin XI.
The identification of 1 chonglou saponin XI of test case
The extract chonglou saponin XI that embodiment 1 obtains is placed in progress nuclear magnetic resonance pop detection in deuterated chloroform,
As a result are as follows: ESI-MS provides quasi-molecular ion peak m/z:869 [M-XI]-；Releasing its molecular formula in conjunction with 1XI NMR, 13C NMR is
C39XI62O15。
The result is shown in tables 1.
1 chonglou saponin XI of table is in tritium for the data of hydrogen in chloroform and carbon
The purity test of 2 chonglou saponin XI of test case
The chonglou saponin XI that Example 1 obtains, is added in high performance liquid chromatography, and wherein chromatographic condition is Inertsil
ODS-3C18Chromatographic column (150mm × 4.6mm, 5 μm)；Mobile phase is acetonitrile-water (45: 55)；Detection wavelength is 210nm；Flow velocity is
1.0mL·min-1；Column temperature is 35 DEG C；Sample volume is 20.0 μ L.The purity of long chonglou saponin XI is calculated using area normalization method
Greater than 98.0%, the results are shown in attached figure 2.The present invention provides new thinking for chonglou saponin XI in Paris polyphylla.
3 human trial of test case
1, group is tested.It is divided into 3 groups of experimental group, 1 group of control, 2 groups of control and control.
2, experimental method.
(1) case selection.Choose what the first affiliated hospital of Guangxi province university of TCM accepted for medical treatment 2 months in Mays, -2018 in 2016
Acute festering type tonsillotome infant 120 excludes hepatic and kidney function obstacle, disease in the blood system and gastrointestinal disease patient.By 120
Infant is randomly divided into four groups, every group 30.In experimental group, male 12, female 18, the age 5~12 years old, average age (7.20 ±
1.21) year, 1~5d of the course of disease, average (3.70 ± 0.29) d, infant have heating paresthesia, 37.93~39.90 DEG C of body temperature, average
(38.45 ± 0.42) DEG C, white blood cell count(WBC) (10.5-12.6) × 109g/L；It compares in 1 group, male 18, female 12, the age 5~
10 years old, average age (6.90 ± 1.12) year, 1~5d of the course of disease, average (2.57 ± 0.46) d, infant has heating paresthesia, body temperature
38.22~39.56 DEG C, average (38.27 ± 0.86) DEG C, white blood cell count(WBC) (10.9-12.4) × 109g/L；It compares in 2 groups, male
15, female 15, the age 4~10 years old, average age (6.52 ± 1.72) year, 1~4d of the course of disease, average (2.66 ± 0.55) d suffer from
Youngster has heating paresthesia, 37.98~39.51 DEG C of body temperature, is averaged (38.31 ± 0.70) DEG C, and white blood cell count(WBC) (10.9-12.4) ×
109g/L.Compare in 3 groups, male 17, female 12, the age 5~9 years old, average age (7.02 ± 1.75) year, 1~4d of the course of disease, put down
(2.76 ± 0.95) d, infant have heating paresthesia, and 37.78~39.71 DEG C of body temperature, average (38.62 ± 0.75) DEG C are white thin
Born of the same parents count (10.8-12.5) × 109g/L.Four groups of infants are compared in basic conditions such as age, gender, the course of disease and the degree of heat
Compared with, it is not statistically significant, it is comparable.
(2) experimental method.It compares 1 group of infant and gives injection Clindamycin Hydrochloride, take this product 1, add 0.9% chlorination
Intravenous drip after sodium injection is dissolved and diluted, dosage are 5~8mg/kg, injection 3 times daily, successive administration 7d；Compare 2 groups
Infant gives injection Clindamycin Hydrochloride, and method takes macrolide antibiotics with 1 group of infant of control daily, often
It 2 times, each 20g, hot water is taken after reconstituting；It compares 3 groups of infants and gives injection Clindamycin Hydrochloride, while taking reality daily
The solid medicinal powder without chonglou saponin XI of the preparation of example 5 is applied, 2 times a day, each 20g, hot water is taken after reconstituting；Experimental group infant
Injection Clindamycin Hydrochloride is given, method takes the solid medicinal powder of the preparation of embodiment 4 with 1 group of infant of control daily, often
It 2 times, each 20g, hot water is taken after reconstituting.Four groups of infant reasonable diets, take a good rest.
(3) observation caliber.Observe and record that four groups of infants are brought down a fever, pharyngalgia, the clinical symptoms such as tonsillotome hyperemia enlargement improve
Time and total white blood cells restore normal time, compare the clinical efficacy of two groups of patients.
(4) curative effect judging standard.Recovery from illness: tonsillotome is without purulent secretion, and no constitutional symptom, laboratory, which checks, restores just
Often；It is effective: to there are 2 to restore normal in tonsillotome, constitutional symptom and laboratory inspection；It is effective: tonsillotome, constitutional symptom and experiment
Room has 1 to restore normal in checking；Invalid: for patient after treating, symptom is without improvement, or even has the tendency that exacerbation.Always effective=
Recovery from illness+effective+effectively.
Experimental result is referring to table 2 and table 3.
Curative effect compares after 2 four groups of infant treatments of table
3 four groups of infant clinical symptoms improvement times of table compare
As seen from the above table, four groups of infants by comparing, illustrate that the Chinese medicine solid medicinal powder that joined chonglou saponin XI has obviously
The effect for treating tonsillitis.Relative to the specific drug macrolide antibiotics for the treatment of tonsillitis, chonglou saponin joined
The Chinese medicine solid medicinal powder of XI has higher drug effect, shortens the time of infant clinical symptoms improvement, and therapeutic effect reaches 100%.
Meanwhile being compared in the embodiment 5 without chonglou saponin XI, the solid medicinal powder for the chonglou saponin XI being added to, which has, more preferably treats
Effect.Therefore illustrate, chonglou saponin XI has apparent therapeutic effect to tonsillitis, is the medical value of Paris polyphylla saponins X I
Exploitation specifies direction.
Those skilled in the art is not under conditions of departing from the spirit and scope of the present invention that claims determine, also
Various modifications can be carried out to the above content.Therefore the scope of the present invention is not limited in above explanation, but by
The range of claims determines.
Claims (13)
1. a kind of preparation method of chonglou saponin XI, which is characterized in that prepare in accordance with the following methods:
Step 1: weighing Paris polyphylla coarse powder, the buffer solution of certain volume is added, is placed in the heating extraction of autoclave mesohigh, extracts
After, be cooled to 50 DEG C, be added a certain amount of cellulase and amylase, ultrasonic wave assisted extraction after a certain period of time, high temperature
Put out a fire 5min, three times with the extraction of ethyl acetate-light petrol mixed solution, filtering, merging filtrate, vacuum rotary steam concentration, with silica gel
Mixing, obtains Paris polyphylla silica white；
Step 2: silicagel column on the Paris polyphylla silica white of step 1 preparation washes product with the mixed liquor of chloroform and methanol
It is de-, eluted product is obtained, obtained eluted product is subjected to thin-layer chromatography, under ultraviolet light observation colour developing, with chonglou saponin XI
Standard specimen comparison, find out and extract the study containing chonglou saponin XI, merge mutually same, obtain chonglou saponin XI study, decompression is dense
Contracting obtains chonglou saponin XI concentration study；
Step 3: reverse phase silica gel column on the chonglou saponin XI concentration study that step 3 is obtained, with methanol solution to the Paris polyphylla
Study elution is concentrated in saponins X I, continues thin-layer chromatography, under ultraviolet light observation colour developing, the standard specimen pair with chonglou saponin XI
Than merging by spot identical with the standard specimen of chonglou saponin XI and in observed under fluorescent light without the sample of other impurities, obtaining containing
The methanol solution of the purified product of chonglou saponin XI is stated, after the solution petroleum ether degreasing, ethyl acetate-acetone extraction, decompression
Concentration removes solvent to get chonglou saponin XI.
2. a kind of preparation method of chonglou saponin XI according to claim 1, which is characterized in that the chonglou saponin XI's
Purity is 98% or more, and the yield of the chonglou saponin XI is 92%-98%.
3. a kind of preparation method of chonglou saponin XI according to claim 1, which is characterized in that buffered described in step 1
Solution is the Na of pH=4.62HPO4Citric acid solution；The grain of the Paris polyphylla coarse powder is through number between 24-60 mesh；It is described heavy
The solid-to-liquid ratio of building coarse powder and buffer solution is 1:(15-25).
4. a kind of preparation method of chonglou saponin XI according to claim 1, which is characterized in that high pressure described in step 1
For 1.5-2 atmospheric pressure, temperature is 70-90 DEG C, extraction time 60-90min.
5. a kind of preparation method of chonglou saponin XI according to claim 1, which is characterized in that extracted described in step 1
Time is 120-180min；The ultrasonic power is 600-800W；The cellulase dosage is (30-50) U/g substrate, starch
Enzyme dosage is (10-15) U/g substrate.
6. a kind of preparation method of chonglou saponin XI according to claim 1, which is characterized in that silica gel described in step 1
For 100-200 mesh；The volume ratio of the ethyl acetate-light petrol mixed solution is (1-5): 2.
7. a kind of preparation method of chonglou saponin XI according to claim 1, which is characterized in that silica gel described in step 2
For 200-300 mesh；The elution is gradient elution；The proportion of the chloroform and methanol is followed successively by 100:1,30:1,20:1,10:
1、1:1。
8. a kind of preparation method of chonglou saponin XI according to claim 1, which is characterized in that eluted described in step 3
For gradient elution；The mass fraction of the methanol solution is followed successively by 80%, 85% and 100%, the body of the ethyl acetate-acetone
Product is than being 1:(1-7).
9. a kind of preparation method of chonglou saponin XI according to claim 1, which is characterized in that in step 2 and step 3
The ultraviolet light is 254nm.
10. a kind of Chinese medicine composition for treating tonsillitis, which is characterized in that the composition is by the original including following parts by weight
Material is prepared: 25 parts of chonglou saponin XI；22 parts of schizonepeta；20 parts of Radix Mussaendae；20 parts of radix glycyrrhizae preparata；17 parts of honey；Rhizoma anemarrhenae 15
Part；15 parts of the root of Dahurain angelica；12 parts of fritillaria thunbergii；10 parts of fohum aconiti kusnezoffii；10 parts of black cloud incense；7 parts of FLOS CHRYSANTHEMI ALBA from Haizhou of China；5 parts of peppermint.
11. a kind of preparation method for the Chinese medicine composition for treating tonsillitis according to claim 10, which is characterized in that press
It is prepared according to following steps:
Step 1: taking schizonepeta, Radix Mussaendae, radix glycyrrhizae preparata, rhizoma anemarrhenae, the root of Dahurain angelica, fritillaria thunbergii, fohum aconiti kusnezoffii, black cloud incense, FLOS CHRYSANTHEMI ALBA from Haizhou of China, peppermint
Dry, crush after mix, be added 8-10 times of volume of water, impregnate 60-120min, decoct 120-180min, be filtered under diminished pressure, filtrate is standby
With；
Step 2: decocting 60-90min by 5-7 times of volume of water is added in the dregs of a decoction obtained by step 1, being filtered under diminished pressure, filtrate is spare；
Step 3: filtrate obtained by step 1 and step 2 is merged, 400 meshes are crossed, honey and chonglou saponin XI is added, mixing is equal
Even, concentration filtrate to relative density is 1.3-1.7, adds auxiliary material, is prepared into regular dosage form.
12. treating the preparation method of the Chinese medicine composition of tonsillitis according to claim 11, which is characterized in that described auxiliary
Material is selected from maltodextrin, starch, starch slurry, mannitol, calcium monohydrogen phosphate, silica, magnesium stearate, microcrystalline cellulose, carboxylic first
One or more of base sodium cellulosate, talcum powder, Macrogol 4000, Macrogol 6000, ethyl alcohol, superfine silica gel powder.
13. treating the preparation method of tonsillitis Chinese medicine composition according to claim 11, which is characterized in that the routine
Dosage form includes pulvis, granule, pill, tablet and capsule.
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| CN101601798A (en) * | 2009-07-01 | 2009-12-16 | 南京泽朗医药科技有限公司 | A kind of preparation method of paris polyphylla saponin |
| CN108186764A (en) * | 2018-03-03 | 2018-06-22 | 广西中医药大学 | Radix Mussaendae extract and its preparation and the application for treating tonsillitis |
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| CN101601798A (en) * | 2009-07-01 | 2009-12-16 | 南京泽朗医药科技有限公司 | A kind of preparation method of paris polyphylla saponin |
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