CN104922187B - A kind of honeysuckle oral liquid and preparation method thereof - Google Patents
A kind of honeysuckle oral liquid and preparation method thereof Download PDFInfo
- Publication number
- CN104922187B CN104922187B CN201510283985.8A CN201510283985A CN104922187B CN 104922187 B CN104922187 B CN 104922187B CN 201510283985 A CN201510283985 A CN 201510283985A CN 104922187 B CN104922187 B CN 104922187B
- Authority
- CN
- China
- Prior art keywords
- oral liquid
- flos lonicerae
- water
- preparation
- filtrate
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- 239000007788 liquid Substances 0.000 title claims abstract description 44
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- 241000205585 Aquilegia canadensis Species 0.000 title claims abstract 3
- 241000628997 Flos Species 0.000 claims abstract description 41
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 36
- 239000000706 filtrate Substances 0.000 claims abstract description 17
- 238000002156 mixing Methods 0.000 claims abstract description 16
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 claims abstract description 15
- 229930006000 Sucrose Natural products 0.000 claims abstract description 15
- WXMKPNITSTVMEF-UHFFFAOYSA-M sodium benzoate Chemical compound [Na+].[O-]C(=O)C1=CC=CC=C1 WXMKPNITSTVMEF-UHFFFAOYSA-M 0.000 claims abstract description 15
- 235000010234 sodium benzoate Nutrition 0.000 claims abstract description 15
- 239000004299 sodium benzoate Substances 0.000 claims abstract description 15
- 230000001954 sterilising effect Effects 0.000 claims abstract description 15
- 239000005720 sucrose Substances 0.000 claims abstract description 15
- 238000001256 steam distillation Methods 0.000 claims abstract description 10
- 239000012467 final product Substances 0.000 claims abstract description 7
- 238000003756 stirring Methods 0.000 claims abstract description 6
- 239000006228 supernatant Substances 0.000 claims abstract description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical class [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 29
- 238000000034 method Methods 0.000 claims description 22
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 20
- 239000003814 drug Substances 0.000 claims description 11
- 229940079593 drug Drugs 0.000 claims description 5
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 3
- 238000007254 oxidation reaction Methods 0.000 claims description 3
- 229910052708 sodium Inorganic materials 0.000 claims description 3
- 239000011734 sodium Substances 0.000 claims description 3
- 230000001186 cumulative effect Effects 0.000 claims description 2
- 238000004659 sterilization and disinfection Methods 0.000 claims description 2
- 240000000111 Saccharum officinarum Species 0.000 claims 1
- 235000007201 Saccharum officinarum Nutrition 0.000 claims 1
- 238000001914 filtration Methods 0.000 abstract description 4
- 239000004615 ingredient Substances 0.000 description 28
- 239000000284 extract Substances 0.000 description 19
- 238000000605 extraction Methods 0.000 description 19
- 235000001368 chlorogenic acid Nutrition 0.000 description 18
- CWVRJTMFETXNAD-FWCWNIRPSA-N 3-O-Caffeoylquinic acid Natural products O[C@H]1[C@@H](O)C[C@@](O)(C(O)=O)C[C@H]1OC(=O)\C=C\C1=CC=C(O)C(O)=C1 CWVRJTMFETXNAD-FWCWNIRPSA-N 0.000 description 17
- PZIRUHCJZBGLDY-UHFFFAOYSA-N Caffeoylquinic acid Natural products CC(CCC(=O)C(C)C1C(=O)CC2C3CC(O)C4CC(O)CCC4(C)C3CCC12C)C(=O)O PZIRUHCJZBGLDY-UHFFFAOYSA-N 0.000 description 17
- CWVRJTMFETXNAD-KLZCAUPSSA-N Neochlorogenin-saeure Natural products O[C@H]1C[C@@](O)(C[C@@H](OC(=O)C=Cc2ccc(O)c(O)c2)[C@@H]1O)C(=O)O CWVRJTMFETXNAD-KLZCAUPSSA-N 0.000 description 17
- CWVRJTMFETXNAD-JUHZACGLSA-N chlorogenic acid Chemical compound O[C@@H]1[C@H](O)C[C@@](O)(C(O)=O)C[C@H]1OC(=O)\C=C\C1=CC=C(O)C(O)=C1 CWVRJTMFETXNAD-JUHZACGLSA-N 0.000 description 17
- 229940074393 chlorogenic acid Drugs 0.000 description 17
- FFQSDFBBSXGVKF-KHSQJDLVSA-N chlorogenic acid Natural products O[C@@H]1C[C@](O)(C[C@@H](CC(=O)C=Cc2ccc(O)c(O)c2)[C@@H]1O)C(=O)O FFQSDFBBSXGVKF-KHSQJDLVSA-N 0.000 description 17
- BMRSEYFENKXDIS-KLZCAUPSSA-N cis-3-O-p-coumaroylquinic acid Natural products O[C@H]1C[C@@](O)(C[C@@H](OC(=O)C=Cc2ccc(O)cc2)[C@@H]1O)C(=O)O BMRSEYFENKXDIS-KLZCAUPSSA-N 0.000 description 17
- 241001570521 Lonicera periclymenum Species 0.000 description 13
- 238000012360 testing method Methods 0.000 description 13
- 239000004744 fabric Substances 0.000 description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 8
- 238000002474 experimental method Methods 0.000 description 8
- 238000011068 loading method Methods 0.000 description 7
- 230000006378 damage Effects 0.000 description 6
- 230000000694 effects Effects 0.000 description 6
- 239000012535 impurity Substances 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 239000000047 product Substances 0.000 description 5
- 238000010923 batch production Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 238000012216 screening Methods 0.000 description 4
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 3
- 239000004480 active ingredient Substances 0.000 description 3
- 238000004821 distillation Methods 0.000 description 3
- 239000003205 fragrance Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000003921 oil Substances 0.000 description 3
- KWGRBVOPPLSCSI-WPRPVWTQSA-N (-)-ephedrine Chemical compound CN[C@@H](C)[C@H](O)C1=CC=CC=C1 KWGRBVOPPLSCSI-WPRPVWTQSA-N 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 235000009508 confectionery Nutrition 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- PQTCMBYFWMFIGM-UHFFFAOYSA-N gold silver Chemical compound [Ag].[Au] PQTCMBYFWMFIGM-UHFFFAOYSA-N 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 210000003097 mucus Anatomy 0.000 description 2
- 150000007524 organic acids Chemical class 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 239000000341 volatile oil Substances 0.000 description 2
- 102000009027 Albumins Human genes 0.000 description 1
- 108010088751 Albumins Proteins 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 239000000039 congener Substances 0.000 description 1
- 238000007596 consolidation process Methods 0.000 description 1
- KWGRBVOPPLSCSI-UHFFFAOYSA-N d-ephedrine Natural products CNC(C)C(O)C1=CC=CC=C1 KWGRBVOPPLSCSI-UHFFFAOYSA-N 0.000 description 1
- 238000006298 dechlorination reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000007850 degeneration Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 230000006806 disease prevention Effects 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000857 drug effect Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 229960002179 ephedrine Drugs 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 229930003935 flavonoid Natural products 0.000 description 1
- 150000002215 flavonoids Chemical class 0.000 description 1
- 235000017173 flavonoids Nutrition 0.000 description 1
- 239000000796 flavoring agent Substances 0.000 description 1
- 235000019634 flavors Nutrition 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 238000005213 imbibition Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 239000008194 pharmaceutical composition Substances 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000003908 quality control method Methods 0.000 description 1
- 239000013558 reference substance Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- KKCBUQHMOMHUOY-UHFFFAOYSA-N sodium oxide Chemical compound [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 description 1
- 229910001948 sodium oxide Inorganic materials 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 238000013112 stability test Methods 0.000 description 1
- 210000002784 stomach Anatomy 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000003440 toxic substance Substances 0.000 description 1
- 235000013619 trace mineral Nutrition 0.000 description 1
- 239000011573 trace mineral Substances 0.000 description 1
- 229930182493 triterpene saponin Natural products 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
Landscapes
- Acyclic And Carbocyclic Compounds In Medicinal Compositions (AREA)
- Medicinal Preparation (AREA)
Abstract
The invention provides a kind of honeysuckle oral liquid, this oral liquid of 1000ml is made up of 90g Flos Lonicerae, 190 210g sucrose and 1 3g sodium benzoate；Present invention also offers the preparation method of this oral liquid, Flos Lonicerae is extracted with steam distillation, collects distillate and decocting liquid, and the filtrate of decocting liquid adjusts pH value to 34, and centrifugal, after supernatant liquid filtering, tune pH value is to 45, concentrating under reduced pressure；Concentrated solution, with sucrose and sodium benzoate, stirring and dissolving, mixing, filters, and filtrate mixes with step distillate (1), adds water to enough, mixing, sterilizing, and subpackage to obtain final product.
Description
Technical field
The present invention relates to the pharmaceutical formulation of field of medicaments, specifically a kind of honeysuckle oral liquid and preparation method thereof.
Background technology
Flos Lonicerae, for the flower opened at the beginning of Caprifoliaceae woodbine Radix Ophiopogonis and congener dry flower or band.Its property is sweet cold
Gas fragrance, clearing away heat with drugs sweet in flavor and cold in nature and do not injure one's stomach, fragrance thoroughly reaches and can be eliminating evil, is the good medicine of heat-clearing and toxic substances removing.
The effect that traditional Chinese medicine disease prevention is cured the disease has direct relation with the accuracy of institute's effective component extracting and the number of content thereof.If
If processing unreasonable, not science, destruction and the loss of effective ingredient certainly will be caused, thus affect the quality of preparation, curative effect.Gold silver
The active ingredient of flower includes organic acid, flavonoid, triterpene saponin, volatile oil and trace element etc., wherein with chlorogenic acid
It is main with volatile oil component.The character of this two parts principle active component determines, if expecting superior in quality Flos Lonicerae system
Agent its preparation technology must be carried out science careful grope research.
Chinese medicine preparation effective ingredient is complicated, often with the lower limit of its principle active component content for controlling during quality control
Index, therefore, a lot of herbal species just do not continue to put into financial resource and material resource after reaching basic standard to be continued to optimize technique, enters one
Step improves product quality.It is on the low side, follow-up broken to there is extraction ratio in existing Flos Lonicerae preparation, the particularly preparation technology of single preparations of ephedrine
Bad, loss, than the deficiency such as more serious, has had a strong impact on product quality.In order to preferably play the medical value of Flos Lonicerae, urgent need
A kind of extracts active ingredients is more complete, content higher Flos Lonicerae preparation.
Summary of the invention
It is an object of the invention to provide a kind of extracts active ingredients more completely, content higher Flos Lonicerae preparation, particularly
Easily facilitating the honeysuckle oral liquid taken, this honeysuckle oral liquid further increases the content of the effective ingredient such as chlorogenic acid,
Lay a good foundation for preferably playing the medical value of Flos Lonicerae.
The invention provides a kind of honeysuckle oral liquid, this oral liquid of 1000ml is by 90g Flos Lonicerae, 190-210g sucrose
And 1-3g sodium benzoate makes.Preferably it is made up of 90g Flos Lonicerae, 200g sucrose and 3g sodium benzoate.
Honeysuckle oral liquid of the present invention, formula is very simple, and sucrose therein is conventional food materials, without the medicine of drug effect
Considerably less with supplementary product consumption, i.e. reduce the simplification of the absorption of nonessential composition, the most beneficially preparation technology.
The preparation method of above-mentioned oral liquid, comprises the following steps:
(1) take recipe quantity Flos Lonicerae to decoct a drug wrapped, use steam distillation to extract 2 times, 8 times of water first, 1 hour, for the second time 6
Times water, 0.5 hour, collects distillate；Decocting liquid filters after being cooled to room temperature in 10-30 minute；
Step (1) filtrate add hydrochloric acid adjust pH value to 3-4, centrifugal, take supernatant, filter；
(3) step (2) filtrate hydro-oxidation sodium adjusts pH value to 4-5, concentrating under reduced pressure；
(4) in step concentrated solution (3), add sucrose and sodium benzoate, stirring and dissolving, mixing, filter, filtrate and step
(1) distillate mixing, adds water to enough, mixing, sterilizing, and subpackage to obtain final product.
Flos Lonicerae is dry flower or the first flower opened of band, very easy rotten through decocting, and thickness is difficult to filter, it is easier to
It is burned.Decoct to this end, inventor is loaded into cloth bag (such as gauze), i.e. decoct a drug wrapped, determine subpackage cloth bag according to inventory
Quantity, and, during subpackage, Flos Lonicerae not can exceed that the 2/5 of cloth bag volume.It is certain to it is known that Flos Lonicerae packs excessively consolidation
Affect the dissolution of its composition, but how many concrete dresses properly has no way of learning.This loading amount has been also carried out investigating by inventor, and result is sent out
Existing, when Flos Lonicerae loading amount is within the 1/4 of cloth bag volume, the extraction of effective ingredient is had little to no effect by loading amount, more than 1/4
After, along with the increase of loading amount, the extraction of effective ingredient is affected increasingly stronger, particularly exceedes cloth bag when Flos Lonicerae loading amount by loading amount
Volume 2/5 time, this impact is significantly raised.Therefore, present invention determine that loading amount when Flos Lonicerae is decocted a drug wrapped is less than cloth bag volume
2/5, in order to still have sufficient space after Flos Lonicerae imbibition by solvent flow, it is to avoid the reasons such as local concentration is high or blocked are led
Cause effective ingredient dissolution limited, thus affect the extraction efficiency of effective ingredient.
Steam distillation can extract volatile ingredient and the water soluble ingredient of Flos Lonicerae simultaneously, but existing technique mostly is one
Secondary extraction, the time is many at about 1.5 hours, exist water soluble ingredient extraction efficiency low and destroy than more serious defect.Experiment
Showing, during steam distillation 45 minutes, volatile ingredient major part is extracted；Steam distillation 1 is little constantly, and volatile ingredient is
Basic collection is completely.Therefore, the time below is mainly used in decocting water soluble ingredient, and the efficiency of the extraction of this time is the lowest,
Relative to the continuous heating destruction to effective ingredient, lose more than gain.Extraction is divided into twice by the present invention, within 1 hour first, completes
The extraction of volatile ingredient, in distillator, decocting liquid filters, and medicinal residues carry out second extraction, test result indicate that, although water consumption phase
Suitable with, extraction time, but the content of extracting solution Content of Chlorogenic Acid than existing methods that this extracting method obtains improves about 5%.
(2) step adds hydrochloric acid and adjusts pH value the impurity (e.g., albumin glue, mucus, pollen etc.) extracted can be made in acid to 3-4
Property environment under degeneration precipitation, follow-up centrifugal remove impurity.
Because of the particularity of Flos Lonicerae quality, causing extracting solution to filter extremely difficult problem, centrifugal method is effectively improved
This problem, but effective ingredient is caused bigger loss.The long-time heating and the medicinal liquid that concentrate link are lost the most also
It it is the main cause of effective ingredient total rate of transform reduction.But above loss is all difficult to avoid that.Effective for reduction chlorogenic acid as far as possible etc.
The loss of composition, inventor, through great many of experiments, finds that following several respects can reach good effect.
On the one hand, the opportunity that Flos Lonicerae feeds intake is changed.The quality of Flos Lonicerae is unlike ratio of rhizome medicinal material, it is not necessary to soak for a long time
Bubble, in order to avoid the inefficient extraction period destruction to effective ingredient as far as possible, when described step is extracted first, first heats water
It is then placed in Flos Lonicerae to 70-80 DEG C.Alleviate the difficulty of filtration the most to a certain extent, improve again extraction effect.
On the other hand, described step decocting liquid (1) was cooled to room temperature in 15-20 minute, existed with minimizing effective ingredient as far as possible
Time in hot environment.Inventor compares through overtesting, finds that the temperature after the ratio cooling of cooling spent time is to effective ingredient
Impact bigger.The selection of time of 15-20 minute, has taken into account the protection of effective ingredient and the resource energy consumption of this link.
Further, inventor has investigated sodium hydroxide and the concentration of hydrochloric acid used by regulation pH.Find when the hydrogen using 1mol/L
During sodium oxide, owing to the alkali concentration higher destruction to organic acid effective ingredient such as chlorogenic acids in local is obvious, and 0.5mol/L
And destructiveness can reduce about 10% during following concentration.Although the impact of effective ingredient is not so good as above-mentioned by different concentration of hydrochloric acid
Alkali is notable, but also has identical trend.In view of dosing volume and the operating efficiency of this link, determine step (2) and (3) salt used
The concentration of acid and sodium hydroxide is 0.5mol/L.
Additionally, present invention eliminates the centrifugal front step adding activated carbon.Can inhale due to its porous when activated carbon filters
Fine material in attached various liquid, is usually used in decolouring, deodorize, dechlorination, organics removal and the heavy metal during water processes, antibacterial
Deng material.And the reason of filtration difficulty of the present invention, on the one hand it is the impurity such as the mucus, the pollen that extract, is on the other hand gold silver
Fiber substance etc. after perianth is well-done, these are not particularly suited for the mode remove impurity of activated carbon adsorption.Activated carbon in existing technique
Filtering and impurity removing is not only the most substantially helped by the step of absorption, but also needs to take up to the time of repose of 12 hours, more has
Effective ingredient can be caused adsorption losses, therefore, after optimization of the present invention, this step is cancelled by technique.
Described step (2) in centrifugal, its rotating speed is 10000-20000 rev/min, it is contemplated that when industrialization produces, height turns
The safety issue of speed, preferably rotating speed is 12000-15000 rev/min, and required time is true according to medicine liquid volume and selected rotating speed
Fixed, general centrifugation time controlled within 30 minutes.
Described step sterilizing methods (4) is inspissation.At present technique used 100 DEG C 20-30 minute
Sterilizing methods, makes being seriously damaged of chlorogenic acid, and loss up to 20%, after the present invention changes sterilizing methods, effectively by this damage
Within mistake is down to 8%.
The pressure of described step (2) concentrating under reduced pressure is 0.04-0.06MPa, and temperature is 60-80 DEG C, is concentrated into cumulative volume
55-65%.
Inventor, through a large amount of scientific experimentss, obtains the preparation method of honeysuckle oral liquid of the present invention, this preparation side
Method is an organic whole, reaches the content of its chlorogenic acid in product and is not less than the final effect of 19mg/20ml, and this result is more existing
Preparation method improves nearly 20%.
Inventor has also carried out stability test to oral liquid of the present invention, within accelerated 6 months, investigates, has good stability.
Inventor investigates different process step and parameter to the shadow of effective ingredient in honeysuckle oral liquid by tests below
Ring.
Reiterate: tests below is the test of the illustrative in numerous tests in development process of the present invention, is not covered by
Be exhausted all experiments that the inventor present invention is done, purpose is only in that and illustrates honeysuckle oral liquid by those data
The partial routine of preparation method screening and optimizing and result.
One, extraction process screening experiment
1, test sample: weigh Flos Lonicerae 5 parts, every part of 50g.
2, experimental technique: according to following packet, extracts with steam distillation respectively.Wherein, decocting liquid mensuration chlorogenic acid contains
Amount (is converted into theoretical finished product to calculate)；Collect follow-up distillate cold preservation (after follow-up distillate, i.e. regulation extraction time terminate, to continue
The continuous distillate extracted), whether its surface of visual observations has oil droplet.Completeness is extracted as index with chlorogenic acid and fragrance ingredient
Screening Extraction technique.
Group 1:14 times amount water, extracts 1 time, 30 minutes time；
Group 2:14 times amount water, extracts 1 time, 45 minutes time；
Group 3:14 times amount water, extracts 1 time, 1 hour time；
Group 4:14 times amount water, extracts 1 time, 1.5 hours time；
Group 5: totally 14 times amount water, extracts 2 times；1st 8 times of water, 1 hour, the 2nd 6 times of water, 0.5 hour.
Chlorogenic acid content detection chromatographic condition:
Chromatographic column:ods-3,5μm 4.6*250mm
Flowing phase: acetonitrile 0.4% phosphoric acid (6:94)
Detection wavelength: 327nm flow velocity: 1.0ml/min
Column temperature: 25 sample sizes: 10 μ l
Sample treatment:
After extracting solution filters, precision measures 5ml respectively, puts 50ml brown and holds in bottle, adds water to scale, with microporous filter membrane
(0.45 μm) filters, and to obtain final product.Configuration chlorogenic acid reference substance solution about 50 μ g/ml.
3, experimental result: experimental data shows, 1. extracts 1 hour, and volatile ingredient extracts completely substantially, it is contemplated that produce
Efficiency, remainder can be ignored；2. in the case of not increasing total extraction time and water consumption, the reasonable distribution water yield and time
Extract at twice, the extraction ratio of Chlorogenic Acid of Flos Lonicerae can be significantly improved.Refer to table 1.
Table 1 extraction process screening test result
Note: "+" indicate oil droplet, " ± " represent that range estimation is substantially without oil droplet.
Two, naoh concentration examination
1, test sample: test the Flos Lonicerae extractive solution of a group 5.
2, experimental technique: dripping the hydrochloric acid of 0.5mol/L in extracting solution, regulation pH value is to 3.5, centrifugal, takes supernatant,
Adding variable concentrations sodium hydroxide respectively adjusts pH value to 4.5, measures the content of solution Content of Chlorogenic Acid before and after hydro-oxidation sodium.
3, experimental result: experimental data shows, when the sodium hydroxide of 0.5～1mol/L uses as pH value regulator, its
Difference to solution Content of Chlorogenic Acid destructiveness is significant, and 0.3mol/L Yu 0.5mol/L no significant difference.Refer to table 2.
Table 2 naoh concentration examination result of the test
Three, sterilizing methods compares
1, test sample: test the sample after two 0.5mol/L sodium hydroxide regulation pH value.
2, experimental technique: be respectively adopted 100 DEG C 30 minutes (methods one), and low temperature batch process (method two) carries out sterilizing,
Each parallel 3 parts.
3, experimental result: experimental data shows, sterilization link is very serious to the destruction of chlorogenic acid, commonly uses the most at present
Method one, the adjustment that the present invention makes makes this link substantially reduce the destructiveness of effective ingredient.Refer to table 3.
Table 3 sterilizing methods comparative test result
Specific embodiments
Embodiment 1
1000ml prescription:
Flos Lonicerae 90g
Sucrose 200g
Sodium benzoate 3g
Preparation method: take recipe quantity Flos Lonicerae and load cloth bag, uses steam distillation to extract 2 times, adds 8 times amount first
Water, puts into Flos Lonicerae when water is heated to about 75 DEG C, extracts 1 hour；6 times of water for the second time, extracts 30 minutes, collects distillation
Liquid；Decocting liquid filters after being cooled to room temperature in 20 minutes；
Filtrate add 0.5mol/L hydrochloric acid adjust pH value to 3.5, centrifugal (rotating speed 15000 revs/min, the time is 20 minutes), take
Supernatant, filters；Filtrate add 0.5mol/L sodium hydroxide adjust pH value to 4.5, concentrating under reduced pressure (pressure 0.04-0.06MPa, temperature
It is about 70 DEG C), it is concentrated into 600ml；
In concentrated solution, add sucrose and the sodium benzoate of recipe quantity, stirring and dissolving, mixing, filter, filtrate and distillate
Mixing, adds water to enough, mixing, low temperature batch process sterilizing, and subpackage to obtain final product.After measured, gained honeysuckle oral liquid Content of Chlorogenic Acid
Content be 20.15mg/ml.
Embodiment 2
1000ml prescription:
Flos Lonicerae 90g
Sucrose 190g
Sodium benzoate 2g
Preparation method: with embodiment 1.
Embodiment 3
1000ml prescription:
Flos Lonicerae 90g
Sucrose 210g
Sodium benzoate 1g
Preparation method: take recipe quantity Flos Lonicerae and load cloth bag, uses steam distillation to extract 2 times, adds 8 times amount first
Water, puts into Flos Lonicerae when water is heated to about 70 DEG C, extracts 1 hour；6 times of water for the second time, extracts 30 minutes, collects distillation
Liquid；Decocting liquid filters after being cooled to room temperature in 15 minutes；
Filtrate adds 1mol/L hydrochloric acid and adjusts pH value to 3.0, is centrifuged (rotating speed 13000 revs/min, the time is 30 minutes), takes
Clear liquid, filters；Filtrate adds 0.5mol/L sodium hydroxide and adjusts pH value to 5.0, and (pressure 0.04-0.06MPa, temperature is about for concentrating under reduced pressure
It is 60 DEG C), it is concentrated into 650ml；
In concentrated solution, add sucrose and the sodium benzoate of recipe quantity, stirring and dissolving, mixing, filter, filtrate and distillate
Mixing, adds water to enough, mixing, low temperature batch process sterilizing, and subpackage to obtain final product.After measured, gained honeysuckle oral liquid Content of Chlorogenic Acid
Content be 19.88mg/ml.
Embodiment 4
1000ml prescription:
Flos Lonicerae 90g
Sucrose 200g
Sodium benzoate 3g
Preparation method: take recipe quantity Flos Lonicerae and load cloth bag, uses steam distillation to extract 2 times, adds 8 times amount first
Water, puts into Flos Lonicerae when water is heated to about 80 DEG C, extracts 1 hour；6 times of water for the second time, extracts 30 minutes, collects distillation
Liquid；Decocting liquid filters after being cooled to room temperature in 20 minutes；
Filtrate adds 0.5mol/L hydrochloric acid and adjusts pH value to 3.0, is centrifuged (rotating speed 10000 revs/min, the time is 30 minutes), takes
Supernatant, filters；Filtrate add 0.5mol/L sodium hydroxide adjust pH value to 4.0, concentrating under reduced pressure (pressure 0.04-0.06MPa, temperature
It is about 60 DEG C), it is concentrated into 550ml；
In concentrated solution, add sucrose and the sodium benzoate of recipe quantity, stirring and dissolving, mixing, filter, filtrate and distillate
Mixing, adds water to enough, mixing, low temperature batch process sterilizing, and subpackage to obtain final product.After measured, gained honeysuckle oral liquid Content of Chlorogenic Acid
Content be 21.47mg/ml.
More than it is intended to further illustrate the present invention, the scope of the present invention is not any limitation as.Those skilled in the art couple
Embodiment disclosed herein can be carried out without departing from scope and the improvement of spirit and change.
Claims (5)
1. a honeysuckle oral liquid, this oral liquid of 1000ml is by 90g Flos Lonicerae, 190-210g sucrose and 1-3g sodium benzoate
Make；
Preparation method comprises the following steps:
(1) take recipe quantity Flos Lonicerae to decoct a drug wrapped, use steam distillation to extract 2 times, 8 times of water first, 1 hour, 6 times of water for the second time,
0.5 hour, collect distillate；Decocting liquid filters after being cooled to room temperature in 15-20 minute；When extracting first, first heat water to 70-
80 DEG C are then placed in Flos Lonicerae；
Step (1) filtrate add hydrochloric acid adjust pH value to 3-4, centrifugal, take supernatant, filter；The concentration of this hydrochloric acid is 0.5mol/L；
(3) step (2) filtrate hydro-oxidation sodium adjusts pH value to 4-5, concentrating under reduced pressure；The concentration of this sodium hydroxide is 0.5mol/L；
(4) adding sucrose and sodium benzoate, stirring and dissolving, mixing in step concentrated solution (3), filter, filtrate and step are (1)
Distillate mixes, and adds water to enough, mixing, sterilizing, and subpackage to obtain final product.
2. oral liquid as claimed in claim 1, it is characterised in that the oral liquid of described 1000ml is by 90g Flos Lonicerae, 200g sugarcane
Sugar and 3g sodium benzoate are made.
3. oral liquid as claimed in claim 1, it is characterised in that the step in described preparation method (2) in centrifugal, its rotating speed is
10000-20000 rev/min.
4. oral liquid as claimed in claim 1, it is characterised in that the sterilizing methods (4) of the step in described preparation method is between low temperature
Have a rest sterilization.
5. oral liquid as claimed in claim 1, it is characterised in that the pressure of the (2) concentrating under reduced pressure of the step in described preparation method is
0.04-0.06MPa, temperature is 60-80 DEG C, is concentrated into the 55-65% of cumulative volume.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510283985.8A CN104922187B (en) | 2015-05-29 | 2015-05-29 | A kind of honeysuckle oral liquid and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510283985.8A CN104922187B (en) | 2015-05-29 | 2015-05-29 | A kind of honeysuckle oral liquid and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104922187A CN104922187A (en) | 2015-09-23 |
| CN104922187B true CN104922187B (en) | 2016-10-19 |
Family
ID=54109840
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510283985.8A Active CN104922187B (en) | 2015-05-29 | 2015-05-29 | A kind of honeysuckle oral liquid and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104922187B (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106511816A (en) * | 2016-12-19 | 2017-03-22 | 刘杰 | Poria cocos and honeysuckle oral liquid |
| CN110157544A (en) * | 2019-05-20 | 2019-08-23 | 山东省分析测试中心 | A kind of total preparation facilities and method of the distilled liquid of honeysuckle and water extract of flos lonicerae |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102764297A (en) * | 2011-04-30 | 2012-11-07 | 顾建光 | Flos ionicerae and radix scutellariae oral liquid and its preparation method |
| CN102441022A (en) * | 2011-11-30 | 2012-05-09 | 中山市中智药业集团有限公司 | Honeysuckle oral liquid |
-
2015
- 2015-05-29 CN CN201510283985.8A patent/CN104922187B/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| CN104922187A (en) | 2015-09-23 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| JP7309042B2 (en) | Plant extraction method | |
| CN101336987A (en) | Preparation method of total flavone of Hovenia dulcisThunb | |
| CN109833377B (en) | Camellia oleifera Abel extract and preparation method and application thereof | |
| CN103961381B (en) | Method for negative-pressure boiling extraction and preparation of low-acid ginkgo extract | |
| CN101167775B (en) | Method for extracting chrysanthemum total flavone | |
| CN105770207A (en) | Herba violae extract and application thereof | |
| CN102526315A (en) | Preparation method of extracts of effective fractions of lychee seeds | |
| CN104922187B (en) | A kind of honeysuckle oral liquid and preparation method thereof | |
| CN104306417A (en) | Low-toxicity acanthopanax injection and preparation method thereof | |
| CN104606276A (en) | Method for extracting micromolecular persimmon leaf flavones from persimmon leaves | |
| CN105535219A (en) | Xanthoceras sorbifolia bunge flavone extract as well as preparation method, quality detection method and application thereof | |
| WO2016110216A1 (en) | Method for extracting stilbene compounds | |
| CN104224952A (en) | Preparation method for total anthraquinones of rheum officinale with stable and uniform proportions of all components | |
| CN104547588B (en) | A kind of preparation method of stomach health drop pills | |
| CN113881503A (en) | Artemisia annua essential oil and white tea essential oil with anti-inflammatory effect, and their composition | |
| JP2005194256A (en) | Hepatic disease-treating medicinal composition and method for producing the same | |
| CN107281235B (en) | The purposes of wintersweet platymiscium resisiting influenza virus | |
| CN102258548B (en) | Method for preparing nardostachyos root and rhizome volatile oil beta-cyclodextrin inclusion compound | |
| CN104983789A (en) | Separating method for fine active dracocephalum heterophyllum component and application of fine active dracocephalum heterophyllum component | |
| CN104826088B (en) | A kind of preparation method of honeysuckle oral liquid | |
| CN105106254A (en) | Anti-influenza loosestrife extract | |
| RU2604141C2 (en) | Method for producing preparation of phenol nature from vegetal raw material | |
| CN109223739A (en) | A kind of composition and its preparation method and application | |
| CN110393774A (en) | A kind of extraction process of fresh bamboo sap | |
| CN103768494B (en) | One treats migrainous pharmaceutical composition and its preparation method and application |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C41 | Transfer of patent application or patent right or utility model | ||
| TA01 | Transfer of patent application right |
Effective date of registration: 20151119 Address after: 100077 Beijing, Fengtai District San Siro Park, building two, No. 23, 401 Applicant after: BEIJING BANGNIKANGDA MEDICAL TECHNOLOGY CO., LTD. Address before: 102204 No. 3 Chang flow road, Changping District Town, Beijing Applicant before: Beijing Kang Yuan pharmaceutical Co. Ltd |
|
| C41 | Transfer of patent application or patent right or utility model | ||
| TA01 | Transfer of patent application right |
Effective date of registration: 20160630 Address after: Bridge Street 437499 Hubei Tongcheng juanyong No. 9 Applicant after: Hubei Huaxin Pharmaceutical Co., Ltd. Address before: 100077 Beijing, Fengtai District San Siro Park, building two, No. 23, 401 Applicant before: BEIJING BANGNIKANGDA MEDICAL TECHNOLOGY CO., LTD. |
|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20181017 Address after: 430074 Xingning Road, biomedical industry park, Xian'an Economic Development Zone, Xianning, Hubei, 16 Patentee after: Real Austrian honeysuckle Pharmaceutical Co., Ltd. Address before: 437499 9 Xinqiao street, Juan Shui Town, Tongcheng County, Hubei Patentee before: Hubei Huaxin Pharmaceutical Co., Ltd. |
|
| TR01 | Transfer of patent right | ||
| PE01 | Entry into force of the registration of the contract for pledge of patent right |
Denomination of invention: Honeysuckle oral liquid and preparation method thereof Effective date of registration: 20220311 Granted publication date: 20161019 Pledgee: Bank of Hankou Limited by Share Ltd. Xianning branch Pledgor: Zhenao Honeysuckle Pharmaceutical Co.,Ltd. Registration number: Y2022990000142 |
|
| PE01 | Entry into force of the registration of the contract for pledge of patent right |