CN105434379A - Five flower tea dropping pill and preparation method thereof - Google Patents
Five flower tea dropping pill and preparation method thereof Download PDFInfo
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- CN105434379A CN105434379A CN201510903650.1A CN201510903650A CN105434379A CN 105434379 A CN105434379 A CN 105434379A CN 201510903650 A CN201510903650 A CN 201510903650A CN 105434379 A CN105434379 A CN 105434379A
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Abstract
The invention discloses a five flower tea dropping pill. The five flower tea dropping pill is prepared from, by mass, 1-4 parts of floral herbal tea extracting concentrated liquid, 13-35 parts of polyethylene glycol 6000 and 0.1-0.4 part of polysorbate 80. The invention further discloses a preparation method of the five flower tea dropping pill. According to the five flower tea dropping pill and the preparation method thereof, traditional Chinese herbal tea is prepared into dropping pills which are convenient to produce and carry, capable of being drunk after being brewed and suitable for the old and the young, the problems that the using process of the traditional Chinese herbal tea consumes time and is cumbersome are solved, and the utility value of the herbal tea is greatly improved. The obtained five flower tea dropping pill has a certain anti-tumor effect.
Description
Technical field
The invention belongs to Chinese herbal medicine preparation technology field, be specifically related to a kind of five-flower tea drop pill, the invention still further relates to a kind of preparation method of five-flower tea drop pill.
Background technology
Five-flower tea is a kind of folks of china tradition beverage, and one of herbal tea that Cantonese often drinks, is made up of Flos Lonicerae, Flos Plumeriae Acutifoliae, Flos Bombacis Malabarici, Flos Sophorae and Flos puerariae lobatae; Flos Lonicerae heat-clearing and toxic substances removing, wind-heat dissipating in side; Flos Plumeriae Acutifoliae clearing away summer-heat, bowel relieving antidiarrheal, relieving cough and resolving phlegm; Flos Bombacis Malabarici clearing away heat-damp and promoting diuresis, expelling wind and removing dampness, promoting blood circulation and detumescence, removing obstruction for relieving pain; Flos Sophorae cooling blood for hemostasis, purging liver-fire; Flos puerariae lobatae heat-clearing and toxic substances removing, promoting digestion, protecting liver; Radix Glycyrrhizae coordinating the actions of various ingredients in a prescription, thus heat clearing away is played, removing heat from blood, effect of removing toxic substances altogether by full side; There is heat clearing away, detoxify, relieve summer heat and dry, lower the intestines and stomach thorn heat, diuresis, removing heat from blood, prevention anemopyretic cold in summer and grippal effect, drink during especially applicable summer.
At present, the use for five-flower tea generally still rests on traditional herbal tea and decocts, and use procedure is consuming time, loaded down with trivial details, owing to decocting for a long time, the medicinal efficacy of Flos Lonicerae is obviously reduced simultaneously, greatly hinders the promotion and application of five-flower tea.Therefore, at present in the urgent need to providing a kind of five-flower tea health beverage of conveniently drinking, to adapt to the demand of consumers in general, significantly promoted the quality of life of people.
Drop pill has the following feature: 1, equipment simple, easy to operate, be beneficial to labor protection, process cycle is short, productivity ratio is high; 2, process conditions are easy to control, steady quality, and dosage is accurate, and heated time is short, after the volatile medicine of oxidizable and tool is dissolved in substrate, can increase its stability; 3, substrate holds liquid drug amount greatly, therefore liquid drug can be made to solidify; 4, have the advantages that absorption is rapid, bioavailability is high with drop pill prepared by solid dispersion technology.Clathrate has the following advantages: cover bad stink, reduces zest; Increase drug dissolution and bioavailability; Improve medicine stability.
Herbal tea is as Chinese tradition beverage, and the herbal tea paving big and small in In Guangdong Province is seen everywhere, and pouplarity has some idea of.But traditional herb tea decocts to waste time and energy, the rhythm of life of urbanite is but more and more faster now, and younger generation few people are ready to buy specially a clay pot and spend several hours and go decoction one to take herbal tea.Meanwhile, in herbal tea, there is the oxidizable and volatile medicine of tool, be not easy to preserve; Herbal tea bitter in the mouth, is not easy to be accepted by people especially the younger generation.
Summary of the invention
The object of this invention is to provide a kind of five-flower tea drop pill, solve the cost existed in prior art high, extraction ratio is low, problem that active ingredient is not fully suggested.
Another object of the present invention is to provide the preparation method of five-flower tea drop pill.
First technical scheme of the present invention is, a kind of five-flower tea drop pill, comprises following component according to mass parts: five-flower tea extracts concentrated solution 1 part-4 parts, polyethylene glycol 6000 13 parts-35 parts, polyoxyethylene sorbitan monoleate 0.1 part-0.4 part.
Further, five-flower tea extraction concentrated solution prepares by the following method:
Step 1.1, Flos Lonicerae, Flos Plumeriae Acutifoliae close and carry, and be that 2:1 is pulverized and mixed, add water Flos Lonicerae, Flos Plumeriae Acutifoliae according to mass ratio, adjust pH to 8-10, join CO
2in supercritical extraction device, ethanol is as entrainer, and the percent by volume that entrainer accounts for total extractant is 8-10%, extracting pressure 45-60MPa, temperature 30-50 DEG C, CO
2flow 1-3m1/g crude drug .min, extraction time 4-8h, obtains supercritical extract, add the alcoholic solution of 95%, soak 20h-28h, reflux 2h-3h, then filter under normal temperature and pressure, obtain leaching liquid, concentrating under reduced pressure is carried out to leaching liquid and obtains blackish green extractum, be alcohol extraction liquid, concentrated, be added on LSA-900C macroporous adsorptive resins, 50% ethanol elution, collects 5 times amount column volume eluents, decompression recycling ethanol, concentrated and dry, obtain Flos Lonicerae and Flos Plumeriae Acutifoliae extract;
After step 1.2, Flos Magnoliae, Flos Sophorae and Flos puerariae lobatae singly being carried respectively, dried by Flos Magnoliae, pulverizing, the dosage through x ray irradiation x is 24-30kGy's
60co-gamma-ray irradiation, obtains Flos Magnoliae powder; Use 60-95% ethanol percolation, residue volatilizes ethanol, adds 4-8 times of water gaging reflux, extract, 1-3 time, and each 4 hours-8 hours, reflux temperature was 45 DEG C-75 DEG C, filters, by filtrate simmer down to extractum; To extractum water dissolution, filter, column purification on filtrate, QFF is as ion exchange column, and 10mMTris-HCl, pH8.0 Gradient elution, obtains Flos Magnoliae extract; Adopt said method to extract Flos Sophorae and Flos puerariae lobatae respectively, obtain Flos Sophorae and Flos puerariae lobatae extract respectively;
Step 1.3, weigh following component according to mass parts: Flos Lonicerae and Flos Plumeriae Acutifoliae extract 42 parts-58 parts, Flos Magnoliae extract 12 parts-15 parts, Flos Sophorae extract 12 parts-15 parts and Flos puerariae lobatae extract 12 parts-15 parts; Load weighted each extract is merged, namely obtains five-flower tea and extract concentrated solution.
Second technical scheme of the present invention is, a kind of preparation method of five-flower tea drop pill, comprises the following steps:
Step 1, prepare five-flower tea extract concentrated solution:
Step 2, weighing, weigh following component according to weight portion: five-flower tea extracts concentrated solution 1 part-4 parts, polyethylene glycol 6000 13 parts-35 parts, polyoxyethylene sorbitan monoleate 0.1 part-0.4 part;
Step 3, above-mentioned load weighted five-flower tea extracted concentrated solution, polyethylene glycol 6000 and polyoxyethylene sorbitan monoleate and be placed in heating container and heat while stirring, until the fused solution obtained containing five-flower tea extraction concentrated solution and substrate is for subsequent use; The temperature control system of adjustment pill dripping machine, makes the water dropper of pill dripping machine heat and maintains the temperature at 65 DEG C ~ 75 DEG C, adopts liquid paraffin liquid coolant carry out condensation and maintain the temperature at 40 DEG C ~-5 DEG C; When pill dripping machine water dropper and condensing agent reach described state of temperature respectively, by the fused solution containing described extract and substrate, be placed in the water dropper tank of pill dripping machine, shrink molding in instillation condensing agent, to obtain final product.
Further, prepare five-flower tea extraction concentrated solution in step 1 to be specially:
Step 1.1, Flos Lonicerae, Flos Plumeriae Acutifoliae close and carry, and be that 2:1 is pulverized and mixed, add water Flos Lonicerae, Flos Plumeriae Acutifoliae according to mass ratio, adjust pH to 8-10, join CO
2in supercritical extraction device, ethanol is as entrainer, and ethanol, as entrainer, extracts, obtain supercritical extract, add the alcoholic solution of 95%, soak, reflux, then filters under normal temperature and pressure, obtains leaching liquid, concentrating under reduced pressure is carried out to leaching liquid and obtains blackish green extractum, be alcohol extraction liquid, concentrated, be added on macroporous adsorptive resins, 50% ethanol elution, collect 5 times amount column volume eluents, decompression recycling ethanol, concentrated and dry, obtain Flos Lonicerae and Flos Plumeriae Acutifoliae extract;
After step 1.2, Flos Magnoliae, Flos Sophorae and Flos puerariae lobatae singly being carried respectively, Flos Magnoliae is dried, pulverizing, warp
60co-gamma-ray irradiation, obtains Flos Magnoliae powder; With ethanol percolation, residue volatilizes ethanol, and add water reflux, extract, filters, by filtrate simmer down to extractum; To extractum water dissolution, filter, column purification eluting on filtrate, obtains Flos Magnoliae extract; Adopt said method to extract Flos Sophorae and Flos puerariae lobatae respectively, obtain Flos Sophorae and Flos puerariae lobatae extract respectively;
Step 1.3, weigh following component according to mass parts: Flos Lonicerae and Flos Plumeriae Acutifoliae extract 42 parts-58 parts, Flos Magnoliae extract 12 parts-15 parts, Flos Sophorae extract 12 parts-15 parts and Flos puerariae lobatae extract 12 parts-15 parts; Load weighted each extract is merged, namely obtains five-flower tea and extract concentrated solution.
Further, the percent by volume that in step 1.1, entrainer accounts for total extractant is 8-10%; Extracting pressure 45-60MPa, temperature 30-50 DEG C, CO
2flow 1-3m1/g crude drug .min, extraction time 4-8h.
Further, be 20h-28h to the soak time of supercritical extract in step 1.1; The reflux time is 2h-3h; Elution requirement is: adopt LSA-900C macroporous adsorptive resins.
Further, in step 1.2, the dosage of 60Co-gamma-ray irradiation is 24-30kGy; Counterflow condition is for use 60-95% ethanol percolation, and residue volatilizes ethanol, and add 4-8 times of water gaging reflux, extract, 1-3 time, each 4h-8h, reflux temperature is 45 DEG C-75 DEG C.
Further, in step 1.2, filtrate upper prop elution requirement is: QFF as ion exchange column, 10mMTris-HCl, pH8.0 Gradient elution.
The invention has the beneficial effects as follows: five-flower tea drop pill of the present invention has easy to use; Its stability is increased after the volatile medicine of oxidizable and tool in herbal tea is dissolved in substrate; Mask the taste of herbal tea simultaneously, be more suitable for child, old man and working clan use.
The present invention makes drop pill traditional herb tea, be convenient to produce and carry, namely rush namely with, old and young suitable, solve the problem that traditional herb tea is in use consuming time, loaded down with trivial details, improve the value of herbal tea greatly.The five-flower tea drop pill that the present invention prepares has certain antineoplastic action.
Detailed description of the invention
Below in conjunction with detailed description of the invention, the present invention is described in detail.
The invention provides a kind of five-flower tea drop pill, comprise following component according to mass parts: five-flower tea extracts concentrated solution 1 part-4 parts, polyethylene glycol 6000 13 parts-35 parts, polyoxyethylene sorbitan monoleate 0.1 part-0.4 part.
The present invention also provides a kind of preparation method of five-flower tea drop pill, comprises the following steps:
Step 1, prepare five-flower tea extract concentrated solution:
Step 1.1, Flos Lonicerae, Flos Plumeriae Acutifoliae close and carry, and be that 2:1 is pulverized and mixed, add water Flos Lonicerae, Flos Plumeriae Acutifoliae according to mass ratio, adjust pH to 8-10, join CO
2in supercritical extraction device, ethanol is as entrainer, and the percent by volume that entrainer accounts for total extractant is 8-10%, extracting pressure 45-60MPa, temperature 30-50 DEG C, CO
2flow 1-3m1/g crude drug .min, extraction time 4-8h, obtains supercritical extract, add the alcoholic solution of 95%, soak 20h-28h, reflux 2h-3h, then filter under normal temperature and pressure, obtain leaching liquid, concentrating under reduced pressure is carried out to leaching liquid and obtains blackish green extractum, be alcohol extraction liquid, concentrated, be added on LSA-900C macroporous adsorptive resins, 50% ethanol elution, collects 5 times amount column volume eluents, decompression recycling ethanol, concentrated and dry, obtain Flos Lonicerae and Flos Plumeriae Acutifoliae extract;
After step 1.2, Flos Magnoliae, Flos Sophorae and Flos puerariae lobatae singly being carried respectively, dried by Flos Magnoliae, pulverizing, the dosage through x ray irradiation x is 24-30kGy's
60co-gamma-ray irradiation, obtains Flos Magnoliae powder; Use 60-95% ethanol percolation, residue volatilizes ethanol, adds 4-8 times of water gaging reflux, extract, 1-3 time, and each 4 hours-8 hours, reflux temperature was 45 DEG C-75 DEG C, filters, by filtrate simmer down to extractum; To extractum water dissolution, filter, column purification on filtrate, QFF is as ion exchange column, and 10mMTris-HCl, pH8.0 Gradient elution, obtains Flos Magnoliae extract; Adopt said method to extract Flos Sophorae and Flos puerariae lobatae respectively, obtain Flos Sophorae and Flos puerariae lobatae extract respectively;
Step 1.3, weigh following component according to mass parts: Flos Lonicerae and Flos Plumeriae Acutifoliae extract 42 parts-58 parts, Flos Magnoliae extract 12 parts-15 parts, Flos Sophorae extract 12 parts-15 parts and Flos puerariae lobatae extract 12 parts-15 parts; Load weighted each extract is merged, namely obtains five-flower tea and extract concentrated solution.
Step 2, weighing, weigh following component according to weight portion: five-flower tea extracts concentrated solution 1 part-4 parts, polyethylene glycol 6000 13 parts-35 parts, polyoxyethylene sorbitan monoleate 0.1 part-0.4 part;
Step 3, above-mentioned load weighted five-flower tea extracted concentrated solution, polyethylene glycol 6000 and polyoxyethylene sorbitan monoleate and be placed in heating container and heat while stirring, until the fused solution obtained containing five-flower tea extraction concentrated solution and substrate is for subsequent use; The temperature control system of adjustment pill dripping machine, makes the water dropper of pill dripping machine heat and maintains the temperature at 65 DEG C ~ 75 DEG C, adopts liquid paraffin liquid coolant carry out condensation and maintain the temperature at 40 DEG C ~-5 DEG C; When pill dripping machine water dropper and condensing agent reach described state of temperature respectively, by the fused solution containing described extract and substrate, be placed in the water dropper tank of pill dripping machine, shrink molding in instillation condensing agent, to obtain final product.
Embodiment 1
A preparation method for five-flower tea drop pill, comprises the following steps: Flos Lonicerae, Flos Plumeriae Acutifoliae are closed and carry, and be that 2:1 is pulverized and mixed, add water Flos Lonicerae, Flos Plumeriae Acutifoliae according to mass ratio, adjusts pH to 9, joins CO
2in supercritical extraction device, ethanol is as entrainer, and the percent by volume that entrainer accounts for total extractant is 9%, extracting pressure 50MPa, temperature 40 DEG C, CO
2flow 2m1/g crude drug .min, extraction time 6h, obtains supercritical extract, add the alcoholic solution of 95%, soak 24h, reflux 2.5h, then filter under normal temperature and pressure, obtain leaching liquid, concentrating under reduced pressure is carried out to leaching liquid and obtains blackish green extractum, be alcohol extraction liquid, concentrated, be added on LSA-900C macroporous adsorptive resins, 50% ethanol elution, collects 5 times amount column volume eluents, decompression recycling ethanol, concentrated and dry, obtain Flos Lonicerae and Flos Plumeriae Acutifoliae extract; Flos Magnoliae, Flos Sophorae and Flos puerariae lobatae are singly carried respectively, after Flos Magnoliae oven dry, pulverizing, the dosage through x ray irradiation x is 27kGy's
60co-gamma-ray irradiation, obtains Flos Magnoliae powder; Use 75% ethanol percolation, residue volatilizes ethanol, adds 6 times of water gaging reflux, extract, 2 times, each 6 hours, and reflux temperature is 60 DEG C, filters, by filtrate simmer down to extractum; To extractum water dissolution, filter, column purification on filtrate, QFF is as ion exchange column, and 10mMTris-HCl, pH8.0 Gradient elution, obtains Flos Magnoliae extract; Adopt said method to extract Flos Sophorae and Flos puerariae lobatae respectively, obtain Flos Sophorae and Flos puerariae lobatae extract respectively; Following component is weighed: Flos Lonicerae and Flos Plumeriae Acutifoliae extract 50 parts, Flos Magnoliae extract 13.5 parts, Flos Sophorae extract 13.5 parts and Flos puerariae lobatae extract 13.5 parts according to mass parts; Load weighted each extract is merged, namely obtains five-flower tea and extract concentrated solution; Following component is weighed: five-flower tea extracts concentrated solution 2.5 parts, polyethylene glycol 6000 24 parts, polyoxyethylene sorbitan monoleate 0.25 part according to weight portion; Above-mentioned load weighted five-flower tea extraction concentrated solution, polyethylene glycol 6000 and polyoxyethylene sorbitan monoleate are placed in heating container and heat while stirring, until the fused solution obtaining extracting containing five-flower tea concentrated solution and substrate is for subsequent use; The temperature control system of adjustment pill dripping machine, makes the water dropper of pill dripping machine heat and maintains the temperature at 70 DEG C, adopts liquid paraffin liquid coolant carry out condensation and maintain the temperature at 20 DEG C; When pill dripping machine water dropper and condensing agent reach described state of temperature respectively, by the fused solution containing described extract and substrate, be placed in the water dropper tank of pill dripping machine, shrink molding in instillation condensing agent, to obtain final product.
Embodiment 2
A preparation method for five-flower tea drop pill, comprises the following steps: Flos Lonicerae, Flos Plumeriae Acutifoliae are closed and carry, and be that 2:1 is pulverized and mixed, add water Flos Lonicerae, Flos Plumeriae Acutifoliae according to mass ratio, adjusts pH to 8, joins CO
2in supercritical extraction device, ethanol is as entrainer, and the percent by volume that entrainer accounts for total extractant is 8%, extracting pressure 45MPa, temperature 30 DEG C, CO
2flow 1m1/g crude drug .min, extraction time 4h, obtains supercritical extract, add the alcoholic solution of 95%, soak 20h, reflux 3h, then filter under normal temperature and pressure, obtain leaching liquid, concentrating under reduced pressure is carried out to leaching liquid and obtains blackish green extractum, be alcohol extraction liquid, concentrated, be added on LSA-900C macroporous adsorptive resins, 50% ethanol elution, collects 5 times amount column volume eluents, decompression recycling ethanol, concentrated and dry, obtain Flos Lonicerae and Flos Plumeriae Acutifoliae extract; Flos Magnoliae, Flos Sophorae and Flos puerariae lobatae are singly carried respectively, after Flos Magnoliae oven dry, pulverizing, the dosage through x ray irradiation x is 24kGy's
60co-gamma-ray irradiation, obtains Flos Magnoliae powder; Use 60% ethanol percolation, residue volatilizes ethanol, adds 4 times of water gaging reflux, extract, 1 time, each 4 hours, and reflux temperature is 45 DEG C, filters, by filtrate simmer down to extractum; To extractum water dissolution, filter, column purification on filtrate, QFF is as ion exchange column, and 10mMTris-HCl, pH8.0 Gradient elution, obtains Flos Magnoliae extract; Adopt said method to extract Flos Sophorae and Flos puerariae lobatae respectively, obtain Flos Sophorae and Flos puerariae lobatae extract respectively; Following component is weighed: Flos Lonicerae and Flos Plumeriae Acutifoliae extract 42 parts, Flos Magnoliae extract 12 parts, Flos Sophorae extract 12 parts and Flos puerariae lobatae extract 12 parts according to mass parts; Load weighted each extract is merged, namely obtains five-flower tea and extract concentrated solution; Following component is weighed: five-flower tea extracts concentrated solution 1 part, polyethylene glycol 6000 13 parts, polyoxyethylene sorbitan monoleate 0.4 part according to weight portion; Above-mentioned load weighted five-flower tea extraction concentrated solution, polyethylene glycol 6000 and polyoxyethylene sorbitan monoleate are placed in heating container and heat while stirring, until the fused solution obtaining extracting containing five-flower tea concentrated solution and substrate is for subsequent use; The temperature control system of adjustment pill dripping machine, makes the water dropper of pill dripping machine heat and maintains the temperature at 65 DEG C, adopts liquid paraffin liquid coolant carry out condensation and maintain the temperature at 40 DEG C; When pill dripping machine water dropper and condensing agent reach described state of temperature respectively, by the fused solution containing described extract and substrate, be placed in the water dropper tank of pill dripping machine, shrink molding in instillation condensing agent, to obtain final product.
Embodiment 3
A preparation method for five-flower tea drop pill, comprises the following steps: Flos Lonicerae, Flos Plumeriae Acutifoliae are closed and carry, and be that 2:1 is pulverized and mixed, add water Flos Lonicerae, Flos Plumeriae Acutifoliae according to mass ratio, adjusts pH to 10, joins CO
2in supercritical extraction device, ethanol is as entrainer, and the percent by volume that entrainer accounts for total extractant is 10%, extracting pressure 60MPa, temperature 50 C, CO
2flow 3m1/g crude drug .min, extraction time 8h, obtains supercritical extract, add the alcoholic solution of 95%, soak 28h, reflux 2h, then filter under normal temperature and pressure, obtain leaching liquid, concentrating under reduced pressure is carried out to leaching liquid and obtains blackish green extractum, be alcohol extraction liquid, concentrated, be added on LSA-900C macroporous adsorptive resins, 50% ethanol elution, collects 5 times amount column volume eluents, decompression recycling ethanol, concentrated and dry, obtain Flos Lonicerae and Flos Plumeriae Acutifoliae extract; Flos Magnoliae, Flos Sophorae and Flos puerariae lobatae are singly carried respectively, after Flos Magnoliae oven dry, pulverizing, the dosage through x ray irradiation x is 30kGy's
60co-gamma-ray irradiation, obtains Flos Magnoliae powder; Use 95% ethanol percolation, residue volatilizes ethanol, adds 8 times of water gaging reflux, extract, 3 times, each 8 hours, and reflux temperature is 75 DEG C, filters, by filtrate simmer down to extractum; To extractum water dissolution, filter, column purification on filtrate, QFF is as ion exchange column, and 10mMTris-HCl, pH8.0 Gradient elution, obtains Flos Magnoliae extract; Adopt said method to extract Flos Sophorae and Flos puerariae lobatae respectively, obtain Flos Sophorae and Flos puerariae lobatae extract respectively; Following component is weighed: Flos Lonicerae and Flos Plumeriae Acutifoliae extract 58 parts, Flos Magnoliae extract 15 parts, Flos Sophorae extract 15 parts and Flos puerariae lobatae extract 15 parts according to mass parts; Load weighted each extract is merged, namely obtains five-flower tea and extract concentrated solution; Following component is weighed: five-flower tea extracts concentrated solution 4 parts, polyethylene glycol 6000 35 parts, polyoxyethylene sorbitan monoleate 0.4 part according to weight portion; Above-mentioned load weighted five-flower tea extraction concentrated solution, polyethylene glycol 6000 and polyoxyethylene sorbitan monoleate are placed in heating container and heat while stirring, until the fused solution obtaining extracting containing five-flower tea concentrated solution and substrate is for subsequent use; The temperature control system of adjustment pill dripping machine, makes the water dropper of pill dripping machine heat and maintains the temperature at 75 DEG C, adopts liquid paraffin liquid coolant carry out condensation and maintain the temperature at-5 DEG C; When pill dripping machine water dropper and condensing agent reach described state of temperature respectively, by the fused solution containing described extract and substrate, be placed in the water dropper tank of pill dripping machine, shrink molding in instillation condensing agent, to obtain final product.
Embodiment 4
A preparation method for five-flower tea drop pill, comprises the following steps: Flos Lonicerae, Flos Plumeriae Acutifoliae are closed and carry, and be that 2:1 is pulverized and mixed, add water Flos Lonicerae, Flos Plumeriae Acutifoliae according to mass ratio, adjusts pH to 8.5, joins CO
2in supercritical extraction device, ethanol is as entrainer, and the percent by volume that entrainer accounts for total extractant is 8.5%, extracting pressure 48MPa, temperature 38 DEG C, CO
2flow 1.5m1/g crude drug .min, extraction time 5h, obtains supercritical extract, add the alcoholic solution of 95%, soak 22h, reflux 2.2h, then filter under normal temperature and pressure, obtain leaching liquid, concentrating under reduced pressure is carried out to leaching liquid and obtains blackish green extractum, be alcohol extraction liquid, concentrated, be added on LSA-900C macroporous adsorptive resins, 50% ethanol elution, collects 5 times amount column volume eluents, decompression recycling ethanol, concentrated and dry, obtain Flos Lonicerae and Flos Plumeriae Acutifoliae extract; Flos Magnoliae, Flos Sophorae and Flos puerariae lobatae are singly carried respectively, after Flos Magnoliae oven dry, pulverizing, the dosage through x ray irradiation x is 26kGy's
60co-gamma-ray irradiation, obtains Flos Magnoliae powder; Use 65% ethanol percolation, residue volatilizes ethanol, adds 4-8 times of water gaging reflux, extract, 2 times, each 5 hours, and reflux temperature is 55 DEG C, filters, by filtrate simmer down to extractum; To extractum water dissolution, filter, column purification on filtrate, QFF is as ion exchange column, and 10mMTris-HCl, pH8.0 Gradient elution, obtains Flos Magnoliae extract; Adopt said method to extract Flos Sophorae and Flos puerariae lobatae respectively, obtain Flos Sophorae and Flos puerariae lobatae extract respectively; Following component is weighed: Flos Lonicerae and Flos Plumeriae Acutifoliae extract 46 parts, Flos Magnoliae extract 12.5 parts, Flos Sophorae extract 12.5 parts and Flos puerariae lobatae extract 12.5 parts according to mass parts; Load weighted each extract is merged, namely obtains five-flower tea and extract concentrated solution; Following component is weighed: five-flower tea extracts concentrated solution 1.5 parts, polyethylene glycol 6000 20 parts, polyoxyethylene sorbitan monoleate 0.2 part according to weight portion; Above-mentioned load weighted five-flower tea extraction concentrated solution, polyethylene glycol 6000 and polyoxyethylene sorbitan monoleate are placed in heating container and heat while stirring, until the fused solution obtaining extracting containing five-flower tea concentrated solution and substrate is for subsequent use; The temperature control system of adjustment pill dripping machine, makes the water dropper of pill dripping machine heat and maintains the temperature at 68 DEG C, adopts liquid paraffin liquid coolant carry out condensation and maintain the temperature at 20 DEG C; When pill dripping machine water dropper and condensing agent reach described state of temperature respectively, by the fused solution containing described extract and substrate, be placed in the water dropper tank of pill dripping machine, shrink molding in instillation condensing agent, to obtain final product.
Embodiment 5
A preparation method for five-flower tea drop pill, comprises the following steps: Flos Lonicerae, Flos Plumeriae Acutifoliae are closed and carry, and be that 2:1 is pulverized and mixed, add water Flos Lonicerae, Flos Plumeriae Acutifoliae according to mass ratio, adjusts pH to 9.5, joins CO
2in supercritical extraction device, ethanol is as entrainer, and the percent by volume that entrainer accounts for total extractant is 9.5%, extracting pressure 56MPa, temperature 42 DEG C, CO
2flow 2.5m1/g crude drug .min, extraction time 7h, obtains supercritical extract, add the alcoholic solution of 95%, soak 26h, reflux 2.8h, then filter under normal temperature and pressure, obtain leaching liquid, concentrating under reduced pressure is carried out to leaching liquid and obtains blackish green extractum, be alcohol extraction liquid, concentrated, be added on LSA-900C macroporous adsorptive resins, 50% ethanol elution, collects 5 times amount column volume eluents, decompression recycling ethanol, concentrated and dry, obtain Flos Lonicerae and Flos Plumeriae Acutifoliae extract; Flos Magnoliae, Flos Sophorae and Flos puerariae lobatae are singly carried respectively, after Flos Magnoliae oven dry, pulverizing, the dosage through x ray irradiation x is 28kGy's
60co-gamma-ray irradiation, obtains Flos Magnoliae powder; Use 85% ethanol percolation, residue volatilizes ethanol, adds 6 times of water gaging reflux, extract, 2 times, each 7 hours, and reflux temperature is 65 DEG C, filters, by filtrate simmer down to extractum; To extractum water dissolution, filter, column purification on filtrate, QFF is as ion exchange column, and 10mMTris-HCl, pH8.0 Gradient elution, obtains Flos Magnoliae extract; Adopt said method to extract Flos Sophorae and Flos puerariae lobatae respectively, obtain Flos Sophorae and Flos puerariae lobatae extract respectively; Following component is weighed: Flos Lonicerae and Flos Plumeriae Acutifoliae extract 54 parts, Flos Magnoliae extract 14.5 parts, Flos Sophorae extract 14.5 parts and Flos puerariae lobatae extract 14.5 parts according to mass parts; Load weighted each extract is merged, namely obtains five-flower tea and extract concentrated solution; Following component is weighed: five-flower tea extracts concentrated solution 1.5, polyethylene glycol 6000 13.35 parts, polyoxyethylene sorbitan monoleate 0.15 part according to weight portion; Above-mentioned load weighted five-flower tea extraction concentrated solution, polyethylene glycol 6000 and polyoxyethylene sorbitan monoleate are placed in heating container and heat while stirring, until the fused solution obtaining extracting containing five-flower tea concentrated solution and substrate is for subsequent use; The temperature control system of adjustment pill dripping machine, makes the water dropper of pill dripping machine heat and maintains the temperature at 72 DEG C, adopts liquid paraffin liquid coolant carry out condensation and maintain the temperature at 0 DEG C; When pill dripping machine water dropper and condensing agent reach described state of temperature respectively, by the fused solution containing described extract and substrate, be placed in the water dropper tank of pill dripping machine, shrink molding in instillation condensing agent, to obtain final product.
Embodiment 6
A preparation method for five-flower tea drop pill, comprises the following steps: Flos Lonicerae, Flos Plumeriae Acutifoliae are closed and carry, and be that 2:1 is pulverized and mixed, add water Flos Lonicerae, Flos Plumeriae Acutifoliae according to mass ratio, adjust pH to 8-10, join CO
2in supercritical extraction device, ethanol is as entrainer, and the percent by volume that entrainer accounts for total extractant is 8.5%, extracting pressure 55MPa, temperature 48 DEG C, CO
2flow 2.8m1/g crude drug .min, extraction time 7h, obtains supercritical extract, add the alcoholic solution of 95%, soak 27h, reflux 2.8h, then filter under normal temperature and pressure, obtain leaching liquid, concentrating under reduced pressure is carried out to leaching liquid and obtains blackish green extractum, be alcohol extraction liquid, concentrated, be added on LSA-900C macroporous adsorptive resins, 50% ethanol elution, collects 5 times amount column volume eluents, decompression recycling ethanol, concentrated and dry, obtain Flos Lonicerae and Flos Plumeriae Acutifoliae extract; Flos Magnoliae, Flos Sophorae and Flos puerariae lobatae are singly carried respectively, after Flos Magnoliae oven dry, pulverizing, the dosage through x ray irradiation x is 28kGy's
60co-gamma-ray irradiation, obtains Flos Magnoliae powder; Use 80% ethanol percolation, residue volatilizes ethanol, adds 7 times of water gaging reflux, extract, 3 times, each 5 hours, and reflux temperature is 50 DEG C, filters, by filtrate simmer down to extractum; To extractum water dissolution, filter, column purification on filtrate, QFF is as ion exchange column, and 10mMTris-HCl, pH8.0 Gradient elution, obtains Flos Magnoliae extract; Adopt said method to extract Flos Sophorae and Flos puerariae lobatae respectively, obtain Flos Sophorae and Flos puerariae lobatae extract respectively; Following component is weighed: Flos Lonicerae and Flos Plumeriae Acutifoliae extract 56 parts, Flos Magnoliae extract 13 parts, Flos Sophorae extract 13 parts and Flos puerariae lobatae extract 13 parts according to mass parts; Load weighted each extract is merged, namely obtains five-flower tea and extract concentrated solution; Following component is weighed: five-flower tea extracts concentrated solution 3.75 parts, polyethylene glycol 6000 33.375 parts, polyoxyethylene sorbitan monoleate 0.375 part according to weight portion; Above-mentioned load weighted five-flower tea extraction concentrated solution, polyethylene glycol 6000 and polyoxyethylene sorbitan monoleate are placed in heating container and heat while stirring, until the fused solution obtaining extracting containing five-flower tea concentrated solution and substrate is for subsequent use; The temperature control system of adjustment pill dripping machine, the water dropper of pill dripping machine is heated and maintains the temperature at 66 DEG C, liquid paraffin liquid coolant is adopted to carry out condensation and maintain the temperature at 10 DEG C when pill dripping machine water dropper and condensing agent reach described state of temperature respectively, by the fused solution containing described extract and substrate, be placed in the water dropper tank of pill dripping machine, shrink molding in instillation condensing agent, to obtain final product.
Comparative example:
The drop pill that common process prepares.
Below in conjunction with dissolving time limit, subjective appreciation, hardness, outward appearance and drug effect evaluate beneficial effect of the present invention:
1, the test of pesticide effectiveness
1.1, the routine patient of clinical observation 60, treatment group 30 example, matched group 30 example.Whole case history all meets case selection standard, man 36 example, female 24 example, age 35-48 year, the course of disease is the shortest 2 days, the longest 2 weeks, takes five-flower tea drop pill one week.
Diagnosis basis: disconnected standard is based on the standard of anemopyretic cold card relevant in " disease of tcm Standardization of diagnosis and curative effect ", and 1. heating, micro evil wind are trembled with fear, have a stuffy nose watery nasal discharge, sneeze, headache, general malaise.2. light red tongue or limit point red, platform book is yellow, floating and rapid pulse.3. unusual weather conditions or daily life cause accidentally, sudden onset.
Symptom and sign ranking criterion: according to correlation intergal standard in " traditional Chinese medical science Clinical Researches of New Drugs guideline ", the disappearance of headache, general pain, watery nasal discharge, pharyngalgia, pharyngeal congestion, cough, slight, moderate, severe long-pending 0,1,2,3 point respectively.
Inclusive criteria: meet the diagnostic criteria of traditional Chinese medical science anemopyretic cold card, body temperature is no more than 39 DEG C of persons, and the course of disease is person within 48h, and the age is between 18 ~ 65 years old.
Excluded cases standard: used medicine person as antibiotic, hormone or other cold medicines person or the person that do not bring down a fever; Merge other primary disease persons of pulmonary, as pulmonary tuberculosis, lung swelling and pain person; Merge serious cardiovascular, liver, kidney and disease of hematopoietic system person; Age is under-18s or over-65s person or be trimester of pregnancy, women breast-feeding their children, and body constitution allergy sufferers.
Matched group: comparative example drop pill, 3 times/d, 7d were 1 course for the treatment of.
Criterion of therapeutical effect: cardinal symptom sign curative effect determinate standard more than temperature decline 0.5C is onset, dropping to 37.4C is that temperature recovery is normal.Other symptom and sign integrations reduce by 1 and are divided into onset, and 0 is divided into disappearance.Comprehensive therapeutic effect criterion is fully recovered: within treatment 3d, temperature recovery is normal, and sings and symptoms all disappears, or symptom, somatic feature score decline more than 90% person; Effective: within treatment 3d, body temperature is normal, and most of sings and symptoms disappears, or symptom, somatic feature score decline more than 75% person; Effective: treatment 3d within body temperature reduce than before, cardinal symptom and sign partial disappearance, or symptom, somatic feature score decline more than 50% person; Invalid: within treatment 3d, body temperature does not fall or raises, cardinal symptom and sign are without improvement or improve <50%.Therapeutic outcome: in table 2.
Contrast with embodiments of the invention 1-5 and comparative example, draw the following conclusions.
Table 1 comparing result
| Dissolve scattered time limit (min) | Formability | Roundness | Fineness | Hardness | |
| Embodiment 1 | 14 | Be shaped | Good | Good | Good |
| Embodiment 2 | 13 | Be shaped | Better | Good | Slightly soft |
| Embodiment 3 | 15 | Be shaped | Better | Good | Slightly soft |
| Embodiment 4 | 13 | Be shaped | Good | Good | Good |
| Embodiment 5 | 16 | Be shaped | Good | Good | Good |
| Comparative example | 25 | Shapeless | Difference | Difference | Too soft |
The observation of curative effect of this drop pill of table 2 treatment anemopyretic cold patient
As shown in Table 2, illustrate that the active ingredient ratio in drop pill of the present invention is easier to extract, drop pill treatment anemopyretic cold effect of the present invention is higher than existing five-flower tea drop pill.
1.2, get the Lewis lung cancer solid tumor of interior generation ten times under aseptic condition, in tumor block (g): the ratio that normal saline (ml) is 1:3 makes single cell suspension, get 0.2ml (containing oncocyte 2 × 10
6) to be inoculated in the right axillary fossa of C57BL/6J mice subcutaneous.Inoculate next day, the antineoplastic extract being divided into model control group, positive controls and the embodiment of the present invention 5 to prepare at random is low, high dose group, often organizes 10.Antineoplastic extract that the other lumbar injection the present embodiment of dosage component prepares (5 and 20mg/kg), positive controls intraperitoneal injection of cyclophosphamide (20mg/kg), model control group intraperitoneal injection of saline.Volume injected is 0.2ml (10gbw)
-1, every day 1 time, continuous 21d.Experimental session mice freely drinks water and takes food.Inoculate beginning in the 10th day, use major diameter and the minor axis of vernier caliper measurement tumor every three days, calculate gross tumor volume.After the administration of mice last, water 12h is can't help in fasting, and pluck eyeball and get blood, separation of serum is for subsequent use.De-cervical vertebra is put to death, and carefully peeling off tumor in situ, weighs, in getting 0.1g tumor tissues, putting in liquid nitrogen frozen for subsequent use on ice.Get bilateral pulmonary, liquid-solid fixed with Bouin ' s.As shown in table 3, the tumor weight of model control group mice reaches 3.23 ± 0.88g, after the antineoplastic extract that lumbar injection the present embodiment prepares, the antineoplastic extract that low, high dose the present embodiment prepares all can suppress the growth of mice lewis tumor in situ, its tumour inhibiting rate is respectively 25.9% and 39.4%, has obvious dose-effect relationship.The effect of the antineoplastic extract high dose group prepared with the present invention is better.
The tumour inhibiting rate of the antineoplastic extract that table 3 the present embodiment prepares
| Group | Tumor weight (g) | Tumour inhibiting rate (%) |
| Model control group | 3.43±0.88 | 0 |
| Positive controls | 1.09±0.33** | 68.2％ |
| Antineoplastic extract low dosage of the present invention | 2.54±0.99* | 25.9％ |
| Antineoplastic extract high dose of the present invention | 2.08±1.01** | 39.4％ |
* P<0.05**P<0.01 compares with model control group
Wherein, tumour inhibiting rate=(the average tumor weight of 1-dosage group average tumor weight/model control group) × 100%.
Claims (8)
1. a five-flower tea drop pill, is characterized in that, comprises following component according to mass parts: five-flower tea extracts concentrated solution 1 part-4 parts, polyethylene glycol 6000 13 parts-35 parts, polyoxyethylene sorbitan monoleate 0.1 part-0.4 part.
2. five-flower tea drop pill according to claim 1, is characterized in that, described five-flower tea extracts concentrated solution and prepares by the following method:
Step 1.1, Flos Lonicerae, Flos Plumeriae Acutifoliae close and carry, and be that 2:1 is pulverized and mixed, add water Flos Lonicerae, Flos Plumeriae Acutifoliae according to mass ratio, adjust pH to 8-10, join CO
2in supercritical extraction device, ethanol is as entrainer, and the percent by volume that entrainer accounts for total extractant is 8-10%, extracting pressure 45-60MPa, temperature 30-50 DEG C, CO
2flow 1-3m1/g crude drug .min, extraction time 4-8h, obtains supercritical extract, add the alcoholic solution of 95%, soak 20h-28h, reflux 2h-3h, then filter under normal temperature and pressure, obtain leaching liquid, concentrating under reduced pressure is carried out to leaching liquid and obtains blackish green extractum, be alcohol extraction liquid, concentrated, be added on LSA-900C macroporous adsorptive resins, 50% ethanol elution, collects 5 times amount column volume eluents, decompression recycling ethanol, concentrated and dry, obtain Flos Lonicerae and Flos Plumeriae Acutifoliae extract;
After step 1.2, Flos Magnoliae, Flos Sophorae and Flos puerariae lobatae singly being carried respectively, dried by Flos Magnoliae, pulverizing, the dosage through x ray irradiation x is 24-30kGy's
60co-gamma-ray irradiation, obtains Flos Magnoliae powder; Use 60-95% ethanol percolation, residue volatilizes ethanol, adds 4-8 times of water gaging reflux, extract, 1-3 time, and each 4 hours-8 hours, reflux temperature was 45 DEG C-75 DEG C, filters, by filtrate simmer down to extractum; To extractum water dissolution, filter, column purification on filtrate, QFF is as ion exchange column, and 10mMTris-HCl, pH8.0 Gradient elution, obtains Flos Magnoliae extract; Adopt said method to extract Flos Sophorae and Flos puerariae lobatae respectively, obtain Flos Sophorae and Flos puerariae lobatae extract respectively;
Step 1.3, weigh following component according to mass parts: Flos Lonicerae and Flos Plumeriae Acutifoliae extract 42 parts-58 parts, Flos Magnoliae extract 12 parts-15 parts, Flos Sophorae extract 12 parts-15 parts and Flos puerariae lobatae extract 12 parts-15 parts; Load weighted each extract is merged, namely obtains five-flower tea and extract concentrated solution.
3. a preparation method for five-flower tea drop pill, is characterized in that, comprises the following steps:
Step 1, prepare five-flower tea extract concentrated solution:
Step 2, weighing, weigh following component according to weight portion: five-flower tea extracts concentrated solution 1 part-4 parts, polyethylene glycol 6000 13 parts-35 parts, polyoxyethylene sorbitan monoleate 0.1 part-0.4 part;
Step 3, above-mentioned load weighted five-flower tea extracted concentrated solution, polyethylene glycol 6000 and polyoxyethylene sorbitan monoleate and be placed in heating container and heat while stirring, until the fused solution obtained containing five-flower tea extraction concentrated solution and substrate is for subsequent use; The temperature control system of adjustment pill dripping machine, makes the water dropper of pill dripping machine heat and maintains the temperature at 65 DEG C ~ 75 DEG C, adopts liquid paraffin liquid coolant carry out condensation and maintain the temperature at 40 DEG C ~-5 DEG C; When pill dripping machine water dropper and condensing agent reach described state of temperature respectively, by the fused solution containing described extract and substrate, be placed in the water dropper tank of pill dripping machine, shrink molding in instillation condensing agent, to obtain final product.
4. the preparation method of five-flower tea drop pill according to claim 3, is characterized in that, prepares five-flower tea extraction concentrated solution and be specially in described step 1:
Step 1.1, Flos Lonicerae, Flos Plumeriae Acutifoliae close and carry, and be that 2:1 is pulverized and mixed, add water Flos Lonicerae, Flos Plumeriae Acutifoliae according to mass ratio, adjust pH to 8-10, join CO
2in supercritical extraction device, ethanol is as entrainer, and ethanol, as entrainer, extracts, obtain supercritical extract, add the alcoholic solution of 95%, soak, reflux, then filters under normal temperature and pressure, obtains leaching liquid, concentrating under reduced pressure is carried out to leaching liquid and obtains blackish green extractum, be alcohol extraction liquid, concentrated, be added on macroporous adsorptive resins, 50% ethanol elution, collect 5 times amount column volume eluents, decompression recycling ethanol, concentrated and dry, obtain Flos Lonicerae and Flos Plumeriae Acutifoliae extract;
After step 1.2, Flos Magnoliae, Flos Sophorae and Flos puerariae lobatae singly being carried respectively, Flos Magnoliae is dried, pulverizing, warp
60co-gamma-ray irradiation, obtains Flos Magnoliae powder; With ethanol percolation, residue volatilizes ethanol, and add water reflux, extract, filters, by filtrate simmer down to extractum; To extractum water dissolution, filter, column purification eluting on filtrate, obtains Flos Magnoliae extract; Adopt said method to extract Flos Sophorae and Flos puerariae lobatae respectively, obtain Flos Sophorae and Flos puerariae lobatae extract respectively;
Step 1.3, weigh following component according to mass parts: Flos Lonicerae and Flos Plumeriae Acutifoliae extract 42 parts-58 parts, Flos Magnoliae extract 12 parts-15 parts, Flos Sophorae extract 12 parts-15 parts and Flos puerariae lobatae extract 12 parts-15 parts; Load weighted each extract is merged, namely obtains five-flower tea and extract concentrated solution.
5. the preparation method of five-flower tea drop pill according to claim 4, is characterized in that, in described step 1.1, entrainer accounts for the percent by volume of total extractant is 8-10%; Extracting pressure 45-60MPa, temperature 30-50 DEG C, CO
2flow 1-3m1/g crude drug .min, extraction time 4-8h.
6. the preparation method of five-flower tea drop pill according to claim 4, is characterized in that, is 20h-28h to the soak time of supercritical extract in described step 1.1; The reflux time is 2h-3h; Elution requirement is: adopt LSA-900C macroporous adsorptive resins.
7. the preparation method of five-flower tea drop pill according to claim 4, is characterized in that, in described step 1.2
60the dosage of Co-gamma-ray irradiation is 24-30kGy; Counterflow condition is for use 60-95% ethanol percolation, and residue volatilizes ethanol, and add 4-8 times of water gaging reflux, extract, 1-3 time, each 4h-8h, reflux temperature is 45 DEG C-75 DEG C.
8. the preparation method of five-flower tea drop pill according to claim 4, is characterized in that, in described step 1.2, filtrate upper prop elution requirement is: QFF as ion exchange column, 10mMTris-HCl, pH8.0 Gradient elution.
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| CN106107375A (en) * | 2016-07-01 | 2016-11-16 | 萧方道 | Folium Bambosae flavone extracts and prepares this Folium Bambosae flavone health promoting beverage and the method for beverage |
| CN111000105A (en) * | 2019-11-28 | 2020-04-14 | 邳州高新区生物医药研究院有限公司 | Liver-protecting beverage and preparation method thereof |
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