CN100389791C - Eye drops and preparation method thereof - Google Patents
Eye drops and preparation method thereof Download PDFInfo
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- CN100389791C CN100389791C CNB2007101439088A CN200710143908A CN100389791C CN 100389791 C CN100389791 C CN 100389791C CN B2007101439088 A CNB2007101439088 A CN B2007101439088A CN 200710143908 A CN200710143908 A CN 200710143908A CN 100389791 C CN100389791 C CN 100389791C
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Abstract
The invention relates to a health liquid using plant materials as the main raw materials and its preparing process, wherein the liquid is prepared from butterflybush flower, cassia seed, wild chrysanthemum flower, Tribulus terrestris, Epuisetum hiemale, notopterygium root, bile of vertebrates, boneol, boracic acid, Ethylparabenum, borax, propylparaben and sodium chloride through steps of extracting, concentrating, alcohol depositing, water precipitating, decolorizing, diluting and filtering.
Description
(1) technical field
The present invention relates to a kind of is the eye drop and the method for making of raw material with the vegetable material mainly, especially a kind of sanitary hygienic liquid of eyes and method for making.
(2) background technology
Eyes are one of vitals of people, people's life,, study, work at every moment all be unable to do without eyes, blind understand cause great misery to people.But the disease of eye is a lot of again, so treat oculopathy and the health care of eyes is caused the scientist's of this technical field great concern.Disclosing this art document both at home and abroad has a lot.
Chinese patent literature, the applying date is December in 1999 1 day, application number 99122579.1, notification number CN1084625C discloses the medicament for the treatment of cataract, the white abnormal pigmentary deposit on the skin of cornea, and this medicament is made by Radix Angelicae Sinensis, Olibanum, Calamina, Spica Prunellae, Endoconcha Sepiae, Moschus, Cinnabaris, Flos Chrysanthemi, Borneolum Syntheticum, Radix Gentianae, Concha Haliotidis, Semen Astragali Complanati, Semen Cassiae, Periostracum Serpentis, Faeces Vespertilionis, hydrogen powder, Plumbum preparatium 13 flavor herbal raw materials.
Chinese patent literature, the applying date is on May 17th, 2000, application number 00110423.3, notification number CN1137699C also disclose the cataractous eye drop of a kind of treatment.
Chinese patent literature, the applying date is August 17 nineteen ninety-five, application number 95111932.X, publication number CN1129127A discloses a kind of eyesight improving liquid, its main recipe ingredient based on Folium Mori, Flos Chrysanthemi, Semen Cassiae,, be equipped with assistant medicament, it has antiinflammatory, pain relieving, the vision of subsiding a swelling, make eye bright, keep healthy, the beauty treatment eyelashes effect.But lose the effect that improves vision is arranged.
Growing along with science and technology, TV, computer have entered in the daily life of family, see TV for a long time, use computer, cause damage for people's vision, cause the vision fatiguability, and the situation that vision weakens takes place.
(3) summary of the invention
Purpose of the present invention just is to develop a kind of eye drop of the eyes that keep healthy.
Another object of the present invention is the preparation method that works out the eye drop of this health care eyes.
A kind of eye drop of the present invention wherein medicinal raw material medicated bag is drawn together Flos Buddlejae 1.025～12.3 weight portions, Semen Cassiae 0.825～9.9 weight portion, Flos Chrysanthemi 0.825～9.9 weight portion, Fructus Tribuli 0.825～9.9 weight portion, Herba Equiseti Hiemalis's 0.825～9.9 weight portion, Rhizoma Et Radix Notopterygii 0.575～6.90 weight portion, the above-mentioned raw materials Chinese crude drug is through extracting, concentrate, precipitate with ethanol, water precipitating, rarely joining, filter, a kind of eye drop that forms.
For the care treatment effect that makes a kind of eye drop of the present invention better, the vertebrate gallbladder that also contains except that the people is bile 0.1～1.2 weight portion, Borneolum Syntheticum 0.025～0.3 weight portion, at the vertebrate bile that adds behind the water precipitating except that the people, decolour again, rare joining, add Borneolum Syntheticum in rare timing.
In order to make the stable pH value of maintaining of a kind of eye drop of the present invention and antibacterial, boric acid 0.6～7.2 weight portion, ethyl hydroxybenzoate 0.00675～0.081 weight portion, Borax 0.0285～0.342 weight portion, propylparaben 0.00675～0.081 weight portion, sodium chloride 0.11～1.32 weight portion have been added for better.Said weight portion can be unit of weights such as gram, jin, kilogram, ton.
Said except that the people vertebrate gallbladder be that bile can be wherein a kind of of bile such as Fel Ursi, Fel Bovis seu Bubali, horse bile, sheep bile, Fel Sus domestica, Fel Canitis juice, Fel Gallus domesticus, fish bile, Fel Serpentis, with the Fel Ursi is best, and other bile has the Fel Ursi similar effects.
Flos Chrysanthemi used among the present invention is turbination, flattens slightly sometimes to be fan-shaped, diameter 1.5～3.0cm is discrete.Involucre dish shape; 3～4 layers of phyllarys, avette or oval, herbaceous stem, yellow green or breen, the outside is by pubescence, and the edge is membranous, holder hemispherical, no supporting spring or holder hair.Ligulate flower number layer, female, be positioned at the periphery, off-white color, neck is straight, and last act is vertically foldable, scattered golden yellow gland point; The tubular flower majority, both sexes.Be positioned at central authorities, by ligulate flower is hidden, yellow, top 5 fissures.The achene aplasia, no pappus.Body is light, and matter is soft and moist, and is crisp when doing.Gas delicate fragrance, sweet in the mouth, little hardship.The white immortal free from admixture of body dry color.
Differentiate: do the thin layer chromatography experiment, compare, should on the relevant position, show the speckle of same color with chlorogenic acid.
Flos Buddlejae: this product mostly is the close poly-inflorescence branchlet of alabastrum, is irregular coniform, long 1.5～3cm.Surface lark or pale brown color, close by fine hair.Alabastrum is corynebacterium, and the upper end is bigger, long 0.3～1cm, diameter 0.1～0.2cm; Calyx mitriform, tip 4 fissures, the corolla tubular, isometric or long slightly with calyx, tip 4 splits, and sliver is avette; Stamen 4 and is given birth at corolla pipe middle part.The matter softness.Feeble QI perfume (or spice), mildly bitter flavor, suffering.
Fructus Tribuli: this product is made up of 5 mericarps, is radial arrangement, diameter 7～12mm.Often split and be single mericarp, mericarp is the axe shape, long 3～6mm; The back yellow green, protuberance has vertical rib and most spinule, and has symmetric lunge and weak point to sting each 1 pair, and two sides are coarse, and reticulate pattern is arranged, canescence.Matter is hard.Odorless, bitter in the mouth, suffering.
The Herba Equiseti Hiemalis: this product is elongated tubular, and branch is not grown 40～60mm, diameter 0.2～0.7cm.Surface celadon or yellow green have 18～30 vertical ribs, and the verruca of most tiny lights is arranged on the rib; Joint obviously, the long 2.5～9cm of internode, on the joint life tubular unicorn leaf, leaf sheath base and sheath tooth are dark brown, the middle part light brown yellow.Body is light, and matter is crisp, frangibility, and section hollow, periphery has most circular areolas.Feeble QI, slightly sweet flavor, little puckery, that chews has a grains of sand sense.
Rhizoma Et Radix Notopterygii: be the crooked rhizome of cylindric summary, long 4～13cm, diameter 0.6～2.5cm, top tool stem trace.The surface sepia is to pitchy, and crust comes off and locates to be yellow.Internode shortens, and is the ring-type of tight protuberance, and the likeness in form silkworm is practised title " silkworm Qiang ": elongation of internode, and shape such as ring shape, habit claims " RHIZOMA SEU RADIX NOTOPTERYGII ".Root trace and brown broken scale that most point-like or strumae are arranged on the joint.Body is light, and matter is crisp, frangibility, and the section out-of-flatness has most slight cracks, and skin zone's yellowish-brown is to burgundy, and is glossy, and brown oil drop is arranged, the woody part yellow-white, ray is obvious, and the marrow yellow is to yellowish-brown.Gas perfume (or spice), mildly bitter flavor and suffering.
Semen Cassiae: slightly be the square or short cylindrical shape of Pedicellus et Pericarpium Trapae, two ends parallel oblique, long 3～7mm.Wide 2～4mm.The green brown or burgundy in surface, smoothly glossy.One end is more smooth, and end is tiltedly sharp in addition, and dorsal ventral side respectively has the crest line of a projection, and respectively there is 1 oblique symmetry the crest line both sides and the more shallow linear dimpled grain of color.Matter is hard, is difficult for broken.It is thin to plant skin, cotyledon 2, yellow: be serpentine warpage and overlapping.Feeble QI, mildly bitter flavor.Seed becomes real full free from admixture.
Used Borneolum Syntheticum contains Borneolum Syntheticum (C10H18O) and is no less than 55.0% non-volatile part≤0.035%, heavy metal 0.0005%, and potassium salt≤0.0002% is good.
Said vertebrate bile can be wherein a kind of of bile such as Fel Ursi, Fel Bovis seu Bubali, horse bile, sheep bile, Fel Sus domestica, Fel Canitis juice, Fel Gallus domesticus, fish bile, Fel Serpentis, be again best with the Fel Ursi, other bile has the Fel Ursi similar effects.
The preparation method of a kind of eye drop of the present invention comprises following processing step:
(1) gets the raw materials ready by Flos Buddlejae 1.025～12.3 weight portions, Semen Cassiae 0.825～9.9 weight portion, Flos Chrysanthemi 0.825～9.9 weight portion, Fructus Tribuli 0.825～9.9 weight portion, Herba Equiseti Hiemalis's 0.825～9.9 weight portion, Rhizoma Et Radix Notopterygii 0.575～6.90 weight portion.
(2) the above-mentioned Chinese crude drug raw material of getting ready is placed extractor, add and extract solvent, said extraction solvent is a water, the weight of extracting for the first time the extraction aqueous solvent that adds is Flos Buddlejae, Semen Cassiae, Flos Chrysanthemi, Fructus Tribuli, Herba Equiseti Hiemalis, Rhizoma Et Radix Notopterygii gross weight 4～12 times, heated and boiled, kept under the state 1～4 hour boiling, draw and obtain the medicinal liquid that extracts for the first time; The weight of extracting for the second time the extraction aqueous solvent that adds is Flos Buddlejae, Semen Cassiae, Flos Chrysanthemi, Fructus Tribuli, Herba Equiseti Hiemalis, Rhizoma Et Radix Notopterygii gross weight 3～5 times, and heated and boiled kept under the state 0.5～2 hour boiling, and obtained the medicinal liquid that extracts for the second time.
(3) with the medicinal liquid mix homogeneously of extracted twice, heat concentratedly, be concentrated to concentrated solution proportion 1.10～1.12 (60 ℃).
(4) under stirring, in concentrated solution, add ethanol to concentration of ethanol and reach 60～85% percetages by weight, leave standstill and carried out precipitate with ethanol in 12～48 hours, leave standstill the back and extract its supernatant, reclaim ethanol.
(5) 2～8 times injection water of medicinal liquid gross weight left standstill and carried out water precipitating in 65～110 hours after ethanol was reclaimed in adding in the medicinal liquid after reclaiming ethanol through precipitate with ethanol.
(6) with the supernatant behind the water precipitating with aqueous slkali for example sodium hydroxide solution regulate PH to 6.0～7.0 and add water for injection and carry out rare joining to being adjusted to supernatant to PH6.0～7.0 again, it is Flos Buddlejae, Semen Cassiae, Flos Chrysanthemi, Fructus Tribuli, Herba Equiseti Hiemalis, Rhizoma Et Radix Notopterygii gross weight 8～51.6 times that the water for injection that is added makes the gross weight of medicinal liquid, rare dosing.
(7) medicinal liquid after rare joining is filtered, and obtain eye drop of the present invention.
In preparation during eye drop of the present invention, at first the centering medicinal raw material carries out pick and picks out non-medicinal part of Chinese crude drug and impurity foreign body etc.Get the raw materials ready in a quantity as required, again the Chinese crude drug raw material behind the pick is carried out pretreatment for well, twice of clear water (for example tap water, well water, distilled water, with distilled water for well) rinsing used in said pretreatment exactly, each rinsing 3-5 minute, the Chinese crude drug raw material after the rinsing is poured on the net drained then.
The Chinese crude drug raw material that rinsing is drained is for example put in the extraction vessel in the extraction pot, wooden Chinese crude drug raw material is put into the bottom of extraction pot in reinforced process, add kind of subclass and stem and leaf class draft Chinese crude drug then, can be convenient to extract the sucking-off of medicinal liquid like this, after having thrown the Chinese crude drug raw material, cleaning jar mouth, build cover, add and extract aqueous solvent (for example tap water, distilled water, ion exchange water), heat, for example can be heated to and boil, extract with the water vapour of steam pressure 0.1～0.15Mpa.The 4-12 that adds the addition of extracting aqueous solvent when extracting for the first time and be Flos Buddlejae, Semen Cassiae, Flos Chrysanthemi, Fructus Tribuli, Herba Equiseti Hiemalis, Rhizoma Et Radix Notopterygii gross weight doubly, heated and boiled kept 1-4 hour boiling under the state, drew the medicinal liquid that extracts for the first time that obtain; When carrying out extracting the second time, add the addition of extracting aqueous solvent be Flos Buddlejae, Semen Cassiae, Flos Chrysanthemi, Fructus Tribuli, Herba Equiseti Hiemalis, Rhizoma Et Radix Notopterygii gross weight 3-5 doubly, heated and boiled kept 0.5-2 hour under the state boiling, and drew and extracted medicinal liquid the second time that obtains.
Merge the medicinal liquid of extracted twice, it is concentrated to place concentrate container to heat, but carrying out vacuum concentration at the combination concentrator for well, and its vacuum degree control is concentrated into concentrated solution ratio 1.10～1.12 (60 ℃) that weigh at 0.05～0.09Mpa during vacuum concentration.
The concentrated solution that will be concentrated into proportion 1.10～1.12 (60 ℃) carries out precipitate with ethanol.The method of its said precipitate with ethanol is under the state that stirs, the ethanol that slowly adds 0.5～1.5 times 80% percetage by weight of concentrated solution weight, stir, carry active ingredient in the medicinal liquid secretly in order to avoid form big pellet, under the state that stirs, slowly add dense ethanol then, make ethanol concentration of alcohol in the alcohol deposit fluid of integral body reach 60～85% percetages by weight, left standstill 12～48 hours.
Reclaiming alcoholic acid method is, with the alcohol deposit fluid that leaves standstill 12～48 hours, extract supernatant, then 70～85% the ethanol of sedimentary bits with 1.5～2.5 times of amounts of bits is washed 1～3 time, by filtering equipment extruding bits, the clear liquid and the cleaning mixture of extruding bits gained are incorporated in the supernatant that extracts behind the precipitate with ethanol,, carried out alcoholic acid recovery with the method that those skilled in the art all know.
To reclaimed the water for injection that adds 2～8 times of amount of liquid medicine in the alcoholic acid medicinal liquid through precipitate with ethanol, leave standstill and carried out water precipitating in 65～110 hours.
The aqueous solution that adds dissolved vertebrate bile 0.1～1.2 weight portion in the supernatant behind water precipitating, with the alkali of 7～20% percetages by weight for example sodium hydroxide regulate PH6.0～7.0,1～3% medical activated carbon of the amount of liquid medicine of PH to 6.0～7.0 is regulated in adding through alkali, boiled 20～60 minutes, decolour, be that filter membrane sucking filtration to the medicinal liquid of 0.45mm is clarified with four metafiltration paper and one deck specification successively, obtain clarifying medicinal liquid, standby.
Clarifying medicinal liquid after the decolouring is carried out rare joining.Said rare joining is at first with the boric acid of 0.6～7.2 weight portion, 0.00675 the ethyl hydroxybenzoate of～0.081 weight portion, 0.0285 the Borax of～0.342 weight portion, 0.00675 the propylparaben of～0.081 weight portion, 0.11 the sodium chloride of～1.32 weight portions is made aqueous solution with the water for injection dissolving, the Borneolum Syntheticum of reuse anhydrous alcohol solution 0.025～0.3 weight portion, become its alcoholic solution, the weight of the dehydrated alcohol that the dissolving Borneolum Syntheticum is used is 1.0 times～8 times of Borneolum Syntheticum weight, with clarifying medicinal liquid and boric acid, Borax, sodium chloride, ethyl hydroxybenzoate, the aqueous solution of propylparaben and the alcoholic solution of Borneolum Syntheticum mix, behind the mix homogeneously, join with water for injection is rare, making the medicinal liquid gross weight after rare joining is Flos Buddlejae, Semen Cassiae, Flos Chrysanthemi, Fructus Tribuli, the Herba Equiseti Hiemalis, Rhizoma Et Radix Notopterygii, vertebrate bile, Borneolum Syntheticum, boric acid, ethyl hydroxybenzoate, Borax, propylparaben, 8～51.6 times of sodium chloride gross weight, mix homogeneously.The rare dosing after rare joining.
To after rare joining rare dosing be filtered through the politef filter stick of 0.2um and the filter membrane of 0.2um successively, the pressure of control filter stick is to begin between 0.025～0.035Mpa to filter during filtration.Filtered liquid medicine is carried out fill, in the eye drop plastic bottle of packing into.Strict with aseptic craft sanitary requirement operation, hunt leak after the fill.
Said leak detection is that medicinal liquid is swung in the leak detection dish that adds a layer paperboard of trying to get to the heart of a matter, and puts into the vacuum leak hunting case, and the control vacuum pressure is 0.025～0.03Mpa, and the time is 5 minutes, hunts leak.
Carry out lamp inspection after the leak detection again, said lamp inspection, be with the qualified medicinal liquid of leak detection by the Zhi Jinhang lamp inspection, requiring lamp inspection illumination is 2000～3000LX, every time of inspecting be 15 seconds each hands hold 2～3, inspect by straight, horizontal, the rotation of falling the three-step approach.
Behind the lamp inspection, packing, warehouse-in.
The excellent results of product of the present invention and preparation method just is:
1 a kind of eye drop of the present invention (trade name is the Herba Senecionis Scandentis eye drop) has alleviating asthenopia, improves vision, prevents and treat the effect of myopia and pseudomyopia, (eye drop with the embodiment of the invention 1 in experiment is called the Herba Senecionis Scandentis eye drop again No. 1)
The advantage of the preparation method of 2 a kind of eye drops of the present invention is that applied Chinese crude drug raw material is simple, is easy to get, and the product cost of producing is low, and is easy to utilize.
Carry out eye drop of the present invention (No. 1, Herba Senecionis Scandentis eye drop) alleviating asthenopia for this reason, improved human trials such as vision.
1 material and method:
1.1 sample: No. 1, Herba Senecionis Scandentis eye drop, light brown liquid, specification is that 8mL/ props up.Provide (lot number: 20070119) by Herba Senecionis Scandentis Pharmaceutical group Siping City, Liaoning health product company limited.
1.2 study subject: select long-term with and be not less than about 6h with machine time every day, the fatigable adult of vision, get rid of among the experimenter and suffer from infectious ocular disease person, corneal nebula, inside and outside eye disease patients such as circle Phasiana cornea: get rid of and suffer from fundus oculi disease or be associated with cardiovascular, cerebrovascular, liver, kidney, the patient of diseases such as hemopoietic system: eliminating is taken in a short time and is tried the relevant article of function, have influence on judgement person: get rid of and take other relevant medicine for a long time or use other Therapeutic Method to the result, fail termination person: get rid of the standard of including in that do not meet, edible in accordance with regulations, or data is not congruent influences effect or safety judgement person:
1.3 taking dose and method: splash into ophthalmic, closed one's eyes 2～3 minutes, each 1～2, every day 3 times or use when needing.
1.4 EXPERIMENTAL DESIGN: according to " the health product function assessment assessment process and the method for inspection " (DB22-T397-2006) in function of relieving visual fatigue human feeding trial regulation, two kinds of contrast methods of contrast between own control and group before and after the experimenter adopts, requirement according to the random-blind method is divided into groups, consider again under influence factors' such as subject age, sex, work the prerequisite, examination of visual acuity situation and eye symptom by the experimenter are divided into experimental group and matched group at random, every group of experimenter is 15 examples, and carries out the harmony check.Test group is used given the test agent, and matched group is as blank, and the useful life is 7d.To the pairing t-check of test group data before and after experimentizing, two groups of means are relatively adopted t-check in groups.When P＜0.05, think that difference has significance.
1.5 key instrument: bright is that persistence is measured with " product " word figure, interrupted Chronograph.
1.6 detection index
1.6.1 ophthalmologic examination, ophthalmalgia, expand, photophobia, blurred vision, asthenopia symptom such as dry and astringent.Decision method sees Table 1
Table 1 asthenopia symptom decision method (sxemiquantitative integration method)
Annotate: " random thoughts " are meant 1-2 time/2d: " time have " is meant 1-3 time/d: " often " is meant＞3 times/d
1.6.2 the mensuration of duration of photopic vision
Duration of photopic vision=(photopic vision time/watch attentively total time) * 100%
Local lighting 100-150LX, minute are 2min.
1.7 adopting SPSS10.0 software adds up with the t check.
2 results:
2.1 asthenopia symptom integral result before and after test group and the matched group test
Asthenopia symptom integral before and after table 2 test group and the matched group test
2.2 asthenopia symptom integral and pairing t-assay before and after the test group test
Asthenopia symptom integral and pairing t-check before and after the test of table 3 test group
2.3 test group and matched group test backsight fatigue symptom integration reach t-assay in groups
Table 4 test group and matched group test backsight fatigue symptom integration and t-check in groups
3 brief summaries:
Screening 30 examples are long-term with eye and be not less than about 6h with machine time every day, the fatigable volunteer of vision, and 15 examples are used No. 1, the Herba Senecionis Scandentis eye drop of Herba Senecionis Scandentis Pharmaceutical group Siping City, Liaoning health product company limited production on request, and 15 examples are as blank.After 7 days, self compare the symptom total mark before and after the test group and descend 4.73, duration of photopic vision raises 10.72%; Test group and matched group relatively symptom total mark descend 5.93, and duration of photopic vision raises 31.05%, and total effective rate obviously improves.Three indexs reach effective criterion and by self pairing t-check and in groups the t-check relatively have significant difference (P＜0.05): the experimenter does not see all not obviously changes of cornea, iris, conjunctiva irritation and other symptom before and after the test.Judge according to " the health product function assessment assessment process and the method for inspection " criterion in (DB22-T397-2006): the Herba Senecionis Scandentis eye drop has function of relieving visual fatigue No. 1.(following blank)
The harmonious comparison of table 5 liang group (x ± S)
2 result of the tests
2.1 " No. 1, Herba Senecionis Scandentis eye drop " subjective symptom on probation changes
After the experimenter used " No. 1, Herba Senecionis Scandentis eye drop ", subjective symptoms such as test group asthenopia obviously alleviated or disappear, and compared x with matched group
2=48.40, P＜0.005, the difference highly significant does not see that the trier has untoward reaction.
Table 6 test group and matched group test back subjective symptom are relatively
x
2＝48.40，P＜0.005
2.2 " No. 1, Herba Senecionis Scandentis eye drop " is to visual acuity affected
Show that from table 3,4 use " No. 1, Herba Senecionis Scandentis eye drop " back test group vision obviously to improve, there were significant differences to compare (P＜0.01) with matched group.
Vision changes before and after the table 7 liang group test
Table 8 " No. 1, Herba Senecionis Scandentis eye drop " back on probation eyesight improving situation
2.3 " No. 1, Herba Senecionis Scandentis eye drop " refraction of eye degree on probation reduces situation
From table 5,6,7 as seen, test back test group detects the diopter result through computerized optometry, skiametry and inserted sheet method and shows, the eye number average of diopter reduction-0.25D is more than 60%, with matched group comparison diopter obvious reduction is arranged.
Table 9 computer optometry detects diopter to be changed
Table 10 skiametry detects diopter to be changed
Table 11 inserted sheet method detects diopter and changes
3 conclusions
" No. 1, Herba Senecionis Scandentis eye drop " has obvious elimination asthenopia, improves vision, the health-care effect of pre-myopia prevention.
(4) specific embodiment
Below with embodiment the present invention is described in detail, will help the present invention is further understood, embodiment does not limit protection scope of the present invention, protection scope of the present invention is decided by claims.
Embodiment 1
The eye drop of present embodiment (being the Herba Senecionis Scandentis eye drop again No. 1), raw material is that 1.025 kilograms of Flos Buddlejaes, 0.825 kilogram of Semen Cassiae, 0.825 kilogram of Flos Chrysanthemi, 1.65 kilograms of Fructus Tribulis, 1.65 kilograms of Herba Equiseties Hiemalis, 1.15 kilograms of Rhizoma Et Radix Notopterygiis, 0.1 kilogram of Fel Ursi, 0.025 kilogram of Borneolum Syntheticum, 0.6 kilogram of boric acid, 0.00675 kilogram of ethyl hydroxybenzoate, 0.0285 kilogram of Borax, 0.00675 kilogram of propylparaben, sodium chloride are raw material for 0.11 kilogram, with above-mentioned Chinese crude drug raw material through extracting, concentrate, precipitate with ethanol, water precipitating, decolouring, rarely joining, filter a kind of eye drop that forms.
Its preparation method is:
(1) gets the raw materials ready by above-mentioned prescription
(2) Flos Buddlejae, Semen Cassiae, Flos Chrysanthemi, Fructus Tribuli, Herba Equiseti Hiemalis, Rhizoma Et Radix Notopterygii raw material of Chinese medicine are placed extraction vessel (if specific productivity is one ton, can use TQM-VI type extraction pot), add and extract aqueous solvent, the weight of the extraction aqueous solvent that is added is Flos Buddlejae, Semen Cassiae, Flos Chrysanthemi, Fructus Tribuli, Herba Equiseti Hiemalis, Rhizoma Et Radix Notopterygii gross weight 4 times, with water vapor pressure is that being steam heated to of 0.1Mpa boiled, under the state that boils, kept 2 hours, carry out the first time and extract, draw and extract medicinal liquid the first time that obtains.Add to extract aqueous solvent again, it is Flos Buddlejae, Semen Cassiae, Flos Chrysanthemi, Fructus Tribuli, Herba Equiseti Hiemalis, Rhizoma Et Radix Notopterygii gross weight 3 times that institute adds the weight of extracting aqueous solvent, and heated and boiled kept 0.5 hour under the state that boils, the medicinal liquid of the absorption extraction second time.
(3) medicinal liquid of merging extracted twice carries out vacuum concentration, and its vacuum degree control is at 0.08Mpa, and it is 1.10 (60 ℃) that the extraction medicinal liquid that merges is concentrated to concentrated solution proportion.
If production capacity can be used ZWW-500 type group and concentration tank for 500 kilograms/hour).
(4) concentrated solution that will be concentrated into proportion 1.10 (60 ℃) carries out precipitate with ethanol.When carrying out precipitate with ethanol the ethanol that under agitation slowly adds 80% percetage by weight of 1 times of concentrated solution weight, stir, under the state that stirs, slowly add ethanol again, make ethanol concentration of ethanol in the alcohol deposit fluid of integral body reach 80% percetage by weight, left standstill 24 hours, with the alcohol deposit fluid that leaves standstill 24 hours, extract supernatant, sedimentary bits are washed 2 times with the ethanol that bits weigh 80% percetage by weight of 2 times of amounts, filter pressing extruding bits are incorporated the clear liquid and the cleaning mixture of extruding bits gained in the supernatant that extracts behind the precipitate with ethanol into, carry out alcoholic acid recovery with the method that those skilled in the art all know.(if specific productivity is 200 kilograms/batches, can adopt V-200 type alcohol feel jar during precipitate with ethanol).
(5) water for injection of 2 times of amounts of adding amount of liquid medicine in the medicinal liquid after passing through precipitate with ethanol and reclaiming ethanol left standstill 72 hours, carried out water precipitating.
(6) add the aqueous solution of 0.1 kilogram of dissolving Fel Ursi in the supernatant behind water precipitating, regulate PH to 6.0, add 1% medical activated carbon, boiled 20 minutes, decolour through the amount of liquid medicine of sodium hydroxide adjusting PH to 6.0 with 10% sodium hydrate aqueous solution.Be that filter membrane sucking filtration to the medicinal liquid of 0.45mm is clarified with four metafiltration paper and one deck specification successively, obtain the clear liquor of medicinal liquid.
(7) the clarifying medicinal liquid after the decolouring is carried out rare joining, said rare joining is boric acid with 0.6 kilogram, 0.00675 the ethyl hydroxybenzoate of kilogram, 0.0285 the Borax of kilogram, 0.00675 the propylparaben of kilogram, 0.11 the sodium chloride water of kilogram is made their aqueous solution, 0.025 kilogram of Borneolum Syntheticum of reuse anhydrous alcohol solution is made the alcoholic solution of Borneolum Syntheticum, the weight of dissolving Borneolum Syntheticum used dehydrated alcohol is heavy 1.0 times of Borneolum Syntheticum, at last with clarifying medicinal liquid and boric acid, Borax, sodium chloride, ethyl hydroxybenzoate, propylparaben, aqueous solution and the alcoholic solution mix homogeneously of Borneolum Syntheticum, join with water for injection is rare, making the medicinal liquid gross weight after rare joining is Flos Buddlejae, Semen Cassiae, Flos Chrysanthemi, Fructus Tribuli, the Herba Equiseti Hiemalis, Rhizoma Et Radix Notopterygii, Fel Ursi, Borneolum Syntheticum, boric acid, Borax, sodium chloride, ethyl hydroxybenzoate, 8 times of propylparaben gross weight, mix homogeneously obtains the rare dosing after rare joining.
(8) rare dosing is filtered through the politef filter stick of 0.2um and the filter membrane of 0.2um successively, the pressure of control filter stick is 0.03Mpa during filtration.Make eye drop of the present invention.
Can carry out the fill of medicinal liquid with PY-II type medicament automatic filling machine,, hunt leak,, put in storage again with the automatic lot number printer prints of GP200D type lot number with JL-I type leak hunting box.
Embodiment 2
Its preparation method and used equipment are substantially with embodiment 1, and only different is 2.05 kilograms of Flos Buddlejaes, 1.65 kilograms of Semen Cassiaes, 1.65 kilograms of Flos Chrysanthemis, 0.825 kilogram of Fructus Tribuli, 0.825 kilogram of Herba Equiseti Hiemalis, 0.575 kilogram of Rhizoma Et Radix Notopterygii, 0.2 kilogram of Fel Ursi, Borneolum Syntheticum 0.05 kilogram, 1.2 kilograms of boric acid, 0.0135 kilogram of ethyl hydroxybenzoate, 0.057 kilogram of Borax, 0.0135 kilogram of propylparaben, 0.22 kilogram in sodium chloride.
Its preparation method is:
(1) gets the raw materials ready by above-mentioned prescription
When (2) extracting for the first time, the weight of the extraction aqueous solvent that is added is Flos Buddlejae, Semen Cassiae, Flos Chrysanthemi, puncturevine caltrop fruit, Herba Equiseti Hiemalis, Rhizoma Et Radix Notopterygii gross weight 6 times, keeps 1 hour under the state that boils; When extracting for the second time, add that to extract aqueous solvent be Flos Buddlejae, Semen Cassiae, Flos Chrysanthemi, Fructus Tribuli, Herba Equiseti Hiemalis, Rhizoma Et Radix Notopterygii gross weight 4 times, under the state that boils, kept 1 hour.
(3) concentrate, be vacuum concentration, when carrying out vacuum concentration, vacuum degree control is at 0.05Mpa, and the proportion that is concentrated to concentrated solution is 1.12 (60 ℃).
When (4) carrying out precipitate with ethanol, add the ethanol of 80% percetage by weight of 0.5 times of concentrated solution weight, add ethanol again and make ethanol in the alcohol deposit fluid of integral body, concentration of alcohol reaches 60% percetage by weight, leaves standstill 48 hours.
(5) during water precipitating, add the water for injection of 3 times of amount of liquid medicine, left standstill 65 hours, carry out water precipitating.
(6) add the aqueous solution of 0.2 kilogram of dissolved Fel Ursi in the supernatant behind water precipitating, the sodium hydrate aqueous solution with 7% is regulated PH6.3, and adding through sodium hydroxide adjusting PH is 1% medicinal carbon of 6.3 amount of liquid medicine, boils 30 minutes, decolours.
(7) carry out rare joining.Rare joining is with 1.2 kilograms of boric acid, 0.0135 the ethyl hydroxybenzoate of kilogram, 0.057 kilogram Borax, 0.0135 kilogram propylparaben, 0.22 the sodium chloride of kilogram is made their aqueous solution, with 0.05 kilogram of Borneolum Syntheticum of anhydrous alcohol solution, the weight of the used dehydrated alcohol of dissolving Borneolum Syntheticum is clarification medicinal liquid and the above-mentioned two kinds of solution mix homogeneously after 2 times of Borneolum Syntheticum weight will decolour, join with water for injection is rare, making the medicinal liquid gross weight after rare joining is Flos Buddlejae, Semen Cassiae, Flos Chrysanthemi, Fructus Tribuli, the Herba Equiseti Hiemalis, Rhizoma Et Radix Notopterygii, Fel Ursi, Borneolum Syntheticum, boric acid, Borax, sodium chloride, ethyl hydroxybenzoate, 15 times of propylparaben gross weight.
(8) filter, the pressure of control filter stick is 0.025Mpa during filtration.
Embodiment 3
Its preparation method and used equipment are substantially with embodiment 1, and only different is 4.10 kilograms of Flos Buddlejaes, 3.30 kilograms of Semen Cassiaes, 3.30 kilograms of Flos Chrysanthemis, 4.95 kilograms of Fructus Tribulis, 4.95 kilograms of Herba Equiseties Hiemalis, 3.45 kilograms of Rhizoma Et Radix Notopterygiis, 0.4 kilogram of Fel Sus domestica, 0.1 kilogram of Borneolum Syntheticum, 2.4 kilograms of boric acid, 0.027 kilogram of ethyl hydroxybenzoate, 0.114 kilogram of Borax, 0.027 kilogram of propylparaben, 0.44 kilogram in sodium chloride.
(1) gets the raw materials ready by above-mentioned prescription.
(2 first time are when extracting, the weight of the extraction aqueous solvent that is added is Flos Buddlejae, Semen Cassiae, Flos Chrysanthemi, Fructus Tribuli, Herba Equiseti Hiemalis, Rhizoma Et Radix Notopterygii gross weight 8 times, under the state that boils, kept 3 hours, when extracting for the second time, add to extract aqueous solvent and be Flos Buddlejae, Semen Cassiae, Flos Chrysanthemi, Fructus Tribuli, Herba Equiseti Hiemalis, Rhizoma Et Radix Notopterygii gross weight 5 times, under the state that boils, kept 2 hours.
(3) concentrate, be vacuum concentration, when carrying out vacuum concentration, vacuum degree control is 1.11 (60 ℃) at the proportion that 0.07Mpa is concentrated to concentrated solution.
When (4) carrying out precipitate with ethanol, the ethanol of 80% percetage by weight of 1.5 times of amounts of adding concentrated solution weight makes ethanol again in the alcohol deposit fluid of integral body, and concentration of ethanol reaches 70% percetage by weight, leaves standstill 12 hours, carries out precipitate with ethanol.
(5) during water precipitating, add the water for injection of 4 times of amount of liquid medicine, left standstill 80 hours, carry out water precipitating.
(6) add the aqueous solution of 0.4 kilogram of dissolving Fel Sus domestica in the supernatant behind water precipitating, it is 7.0 that the sodium hydroxide with 20% is regulated PH, and adding through sodium hydroxide adjusting PH is 3% medicinal carbon of 7.0 amount of liquid medicine, boils 60 minutes, decolours.
(7) carry out rare joining.Rare timing is with 2.4 kilograms of boric acid, 0.027 the ethyl hydroxybenzoate of kilogram, 0.114 kilogram Borax, 0.027 kilogram propylparaben, 0.44 the sodium chloride of kilogram is made their aqueous solution, Borneolum Syntheticum with 0.1 kilogram of anhydrous alcohol solution, the weight of the dehydrated alcohol that the dissolving Borneolum Syntheticum is used is 1.5 times of Borneolum Syntheticum weight, clarification medicinal liquid and above-mentioned two kinds of solution mix homogeneously will decolour, join with water for injection is rare, making the medicinal liquid gross weight after rare joining is Flos Buddlejae, Semen Cassiae, Flos Chrysanthemi, Fructus Tribuli, the Herba Equiseti Hiemalis, Rhizoma Et Radix Notopterygii, Fel Sus domestica, Borneolum Syntheticum, boric acid, Borax, sodium chloride, ethyl hydroxybenzoate, 20 times of propylparaben gross weight.
(8) filter, the pressure of control filter stick is 0.035Mpa during filtration.
Embodiment 4
Its preparation method and used equipment are substantially with embodiment 1, and only different is 8.20 kilograms of Flos Buddlejaes, 6.60 kilograms of Semen Cassiaes, 6.60 kilograms of Flos Chrysanthemis, 3.30 kilograms of Fructus Tribulis, 3.30 kilograms of Herba Equiseties Hiemalis, 2.30 kilograms of Rhizoma Et Radix Notopterygiis, 0.8 kilogram of horse bile, 0.2 kilogram of Borneolum Syntheticum, 4.8 kilograms of boric acid, 0.054 kilogram of ethyl hydroxybenzoate, 0.228 kilogram of Borax, 0.054 kilogram of propylparaben, 0.88 kilogram in sodium chloride.
Its preparation method is:
(1) gets the raw materials ready by above-mentioned prescription.
When (2) extracting for the first time, the weight of the extraction aqueous solvent that is added is Flos Buddlejae, Semen Cassiae, Flos Chrysanthemi, Fructus Tribuli, Herba Equiseti Hiemalis, Rhizoma Et Radix Notopterygii gross weight 10 times, keeps 4 hours under the state that boils; When extracting for the second time, add that to extract aqueous solvent be Flos Buddlejae, Semen Cassiae, Flos Chrysanthemi, Fructus Tribuli, Herba Equiseti Hiemalis, Rhizoma Et Radix Notopterygii gross weight 5 times, under the state that boils, kept 2 hours.
(3) concentrate, be vacuum concentration, when carrying out vacuum concentration, vacuum degree control is 1.11 (60 ℃) at the proportion that 0.09Mpa is concentrated to concentrated solution.
When (4) carrying out precipitate with ethanol, the ethanol of 80% percetage by weight of 1.5 times of amounts of adding concentrated solution weight adds ethanol again and makes ethanol in the alcohol deposit fluid of integral body, and concentration of ethanol reaches 85% percetage by weight, leaves standstill 36 hours, carries out precipitate with ethanol.
(5) during water precipitating, add the water for injection of 6 times of amount of liquid medicine, left standstill 90 hours, carry out water precipitating.
(6) add dissolved horse bile 0.8 kg of water solution in the supernatant behind water precipitating, it is 6.7 that the sodium hydroxide with 10% is regulated PH, and adding through sodium hydroxide adjusting PH is 1% medicinal carbon of 6.7 amount of liquid medicine, boils 40 minutes, decolours.
(7) carry out rare joining.Rare timing is with 4.8 kilograms of boric acid, 0.054 the ethyl hydroxybenzoate of kilogram, 0.228 kilogram Borax, 0.054 kilogram propylparaben, 0.88 the sodium chloride of kilogram is made their aqueous solution, Borneolum Syntheticum with 0.2 kilogram of anhydrous alcohol solution, the weight of the dehydrated alcohol that the dissolving Borneolum Syntheticum is used is 4 times of Borneolum Syntheticum weight, clarification medicinal liquid and above-mentioned two kinds of solution mix homogeneously will decolour, join with water for injection is rare, making the medicinal liquid gross weight after rare joining is Flos Buddlejae, Semen Cassiae, Flos Chrysanthemi, Fructus Tribuli, the Herba Equiseti Hiemalis, Rhizoma Et Radix Notopterygii, horse bile, Borneolum Syntheticum, boric acid, Borax, sodium chloride, ethyl hydroxybenzoate, 30 times of propylparaben gross weight.
(8) filter, the pressure of control filter stick is 0.03Mpa during filtration.
Embodiment 5
Its preparation method and used equipment are substantially with embodiment 1, and only different is with 1.0 kilograms of sheep biles
Embodiment 6
Its preparation method and used equipment are substantially with embodiment 1, and only different is with 1.2 kilograms of Fel Gallus domesticuss
Embodiment 7
Its preparation method and used equipment are substantially with embodiment 1, and only different is 10.25 kilograms of Flos Buddlejaes, 8.25 kilograms of Semen Cassiaes, 8.25 kilograms of Flos Chrysanthemis, 6.60 kilograms of Fructus Tribulis, 6.60 kilograms of Herba Equiseties Hiemalis, 4.60 kilograms of Rhizoma Et Radix Notopterygiis, 1.0 kilograms of Fel Bovis seu Bubali, 0.25 kilogram of Borneolum Syntheticum, 6.0 kilograms of boric acid, 0.0675 kilogram of ethyl hydroxybenzoate, 0.305 kilogram of Borax, 0.0675 kilogram of propylparaben, 1.1 kilograms in sodium chloride.
Its preparation method is:
(1) gets the raw materials ready by above-mentioned prescription
When (2) extracting for the first time, the weight of the extraction aqueous solvent that is added is Flos Buddlejae, Semen Cassiae, Flos Chrysanthemi, Fructus Tribuli, Herba Equiseti Hiemalis, Rhizoma Et Radix Notopterygii gross weight 12 times, keeps 4 hours under the state that boils; When extracting for the second time, add that to extract aqueous solvent be Flos Buddlejae, Semen Cassiae, Flos Chrysanthemi, Fructus Tribuli, Herba Equiseti Hiemalis, Rhizoma Et Radix Notopterygii gross weight 5 times, under the state that boils, kept 2 hours.
(3) concentrate, be vacuum concentration, when carrying out vacuum concentration, vacuum degree control is at 0.06Mpa, and the proportion that is concentrated to concentrated solution is 1.11 (60 ℃).
When (4) carrying out precipitate with ethanol, add the ethanol of 80% percetage by weight of 0.8 times of concentrated solution weight, add ethanol again and make ethanol in the alcohol deposit fluid of integral body, concentration of alcohol reaches 80% percetage by weight, leaves standstill 24 hours.
(5) during water precipitating, add the water for injection of 8 times of amount of liquid medicine, left standstill 110 hours, carry out water precipitating.
(6) add the aqueous solution of 1.0 kilograms of dissolved Fel Bovis seu Bubali in the supernatant behind water precipitating, the sodium hydrate aqueous solution with 15% is regulated PH6.5, and adding through sodium hydroxide adjusting PH is 1.5% medicinal carbon of 6.5 amount of liquid medicine, boils 25 minutes, decolours.
(7) carry out rare joining.Rare joining is with 6.0 kilograms of boric acid, 0.0675 the ethyl hydroxybenzoate of kilogram, 0.305 kilogram Borax, 0.0675 kilogram propylparaben, 1.1 the sodium chloride of kilogram is made their aqueous solution, with 0.25 kilogram of Borneolum Syntheticum of anhydrous alcohol solution, the weight of the used dehydrated alcohol of dissolving Borneolum Syntheticum is 8 times of Borneolum Syntheticum weight, with clarification medicinal liquid and the above-mentioned two kinds of solution mix homogeneously after the decolouring, join with water for injection is rare, making the medicinal liquid gross weight after rare joining is Flos Buddlejae, Semen Cassiae, Flos Chrysanthemi, Fructus Tribuli, the Herba Equiseti Hiemalis, Rhizoma Et Radix Notopterygii, Fel Bovis seu Bubali, Borneolum Syntheticum, boric acid, Borax, sodium chloride, ethyl hydroxybenzoate, 40 times of propylparaben gross weight.
(8) filter, the pressure of control filter stick is 0.030Mpa during filtration.
Embodiment 8
Its preparation method and used equipment are substantially with embodiment 1, and only different is 12.30 kilograms of Flos Buddlejaes, 9.9 kilograms of Semen Cassiaes, 9.9 kilograms of Flos Chrysanthemis, 8.25 kilograms of Fructus Tribulis, 6.60 kilograms of Herba Equiseties Hiemalis, 5.75 kilograms of Rhizoma Et Radix Notopterygiis, 1.2 kilograms of bile of cyprinoid fish, 0.3 kilogram of Borneolum Syntheticum, 7.2 kilograms of boric acid, 0.081 kilogram of ethyl hydroxybenzoate, 0.342 kilogram of Borax, 0.081 kilogram of propylparaben, 1.32 kilograms in sodium chloride.
Its preparation method is:
(1) gets the raw materials ready by above-mentioned prescription.
When (2) extracting for the first time, the weight of the extraction aqueous solvent that is added is Flos Buddlejae, Semen Cassiae, Flos Chrysanthemi, Fructus Tribuli, Herba Equiseti Hiemalis, Rhizoma Et Radix Notopterygii gross weight 12 times, keeps 3 hours under the state that boils; When extracting for the second time, add that to extract aqueous solvent be Flos Buddlejae, Semen Cassiae, Flos Chrysanthemi, Fructus Tribuli, Herba Equiseti Hiemalis, Rhizoma Et Radix Notopterygii gross weight 4 times, under the state that boils, kept 1.5 hours.
(3) concentrate, be vacuum concentration, when carrying out vacuum concentration, vacuum degree control is 1.11 (60 ℃) at the proportion that 0.08Mpa is concentrated to concentrated solution.
When (4) carrying out precipitate with ethanol, the ethanol of 80% percetage by weight of 1 times of amount of adding concentrated solution weight adds ethanol again and makes ethanol in the alcohol deposit fluid of integral body, and concentration of ethanol reaches 80% percetage by weight, leaves standstill 24 hours, carries out precipitate with ethanol.
(5) during water precipitating, add the water for injection of 7 times of amount of liquid medicine, left standstill 72 hours, carry out water precipitating.
(6) add dissolved bile of cyprinoid fish 1.2 kg of water solution in the supernatant behind water precipitating, it is 6.4 that the sodium hydroxide with 10% is regulated PH, and adding through sodium hydroxide adjusting PH is 1% medicinal carbon of 6.4 amount of liquid medicine, boils 30 minutes, decolours.
(7) carry out rare joining.Rare timing is with 7.2 kilograms of boric acid, 0.081 the ethyl hydroxybenzoate of kilogram, 0.342 kilogram Borax, 0.081 kilogram propylparaben, 1.32 the sodium chloride of kilogram is made their aqueous solution, Borneolum Syntheticum with 0.3 kilogram of anhydrous alcohol solution, the weight of the dehydrated alcohol that the dissolving Borneolum Syntheticum is used is 6 times of Borneolum Syntheticum weight, clarification medicinal liquid and above-mentioned two kinds of solution mix homogeneously will decolour, join with water for injection is rare, making the medicinal liquid gross weight after rare joining is Flos Buddlejae, Semen Cassiae, Flos Chrysanthemi, Fructus Tribuli, the Herba Equiseti Hiemalis, Rhizoma Et Radix Notopterygii, bile of cyprinoid fish, Borneolum Syntheticum, boric acid, Borax, sodium chloride, ethyl hydroxybenzoate, 51.6 times of propylparaben gross weight.
(8) filter, the pressure of control filter stick is 0.030Mpa during filtration.
Embodiment 9
(1) gets the raw materials ready by above-mentioned prescription.
When (2) extracting for the first time, the weight of the extraction aqueous solvent that is added is Flos Buddlejae, Semen Cassiae, Flos Chrysanthemi, Fructus Tribuli, Herba Equiseti Hiemalis, Rhizoma Et Radix Notopterygii gross weight 6 times, keeps 2 hours under the state that boils; When extracting for the second time, add that to extract aqueous solvent be Flos Buddlejae, Semen Cassiae, Flos Chrysanthemi, Fructus Tribuli, Herba Equiseti Hiemalis, Rhizoma Et Radix Notopterygii gross weight 4 times, under the state that boils, kept 1 hour.
(3 concentrate, and heat concentratedly, and the proportion that is concentrated to concentrated solution is 1.11 (60 ℃).
(4) precipitate with ethanol adds ethanol when carrying out precipitate with ethanol in concentrated solution under the state that stirs, reach 80% percetage by weight to concentration of ethanol, leaves standstill 24 hours, carries out precipitate with ethanol, after leaving standstill, extracts its supernatant, reclaims ethanol.
(5) during water precipitating, will reclaim medicinal liquid behind the ethanol, add the water for injection that reclaims the 4 times of amounts of medicinal liquid gross weight behind the ethanol, leave standstill 72 hours, carry out water precipitating through precipitate with ethanol.
(6) save the decoloration process step.
(7) supernatant behind the water precipitating being regulated PH with 10% sodium hydroxide solution is 6.4, to be adjusted to PH again and be in 6.4 the supernatant and add water for injection, carry out rare joining, it is Flos Buddlejae, Semen Cassiae, Flos Chrysanthemi, Fructus Tribuli, Herba Equiseti Hiemalis, Rhizoma Et Radix Notopterygii gross weight 12 times that the amount of the water for injection that is added makes the medicinal liquid gross weight, rare dosing.
(medicinal liquid after 8 pairs of rare the joining filters.Four metafiltration paper sucking filtration for example.
Embodiment 10
Its preparation method and used equipment are substantially with embodiment 1, only different is 10.25 kilograms of Flos Buddlejaes, 8.25 kilograms of Semen Cassiaes, 8.25 kilograms of Flos Chrysanthemis, 9.9 kilograms of Fructus Tribulis, 9.9 kilograms of Herba Equiseties Hiemalis, 6.90 kilograms of Rhizoma Et Radix Notopterygiis, 6.0 kilograms of boric acid, 0.0675 kilogram of ethyl hydroxybenzoate, 3.05 kilograms of Boraxs, 0.0675 kilogram of propylparaben, 1.1 kilograms in sodium chloride, with above-mentioned Chinese crude drug raw material through extracting, concentrate, precipitate with ethanol, water precipitating, rarely joining, filter a kind of eye drop that forms.
Its preparation method is:
Processing step (1), (2), (3), (4), (5), (6) are fully with embodiment 9.
(7) carry out rare joining.Rare timing is with 6.0 kilograms of boric acid, 0.0675 the ethyl hydroxybenzoate of kilogram, 3.05 kilogram Borax, 0.0675 kilogram propylparaben, 1.1 the sodium chloride of kilogram is made their aqueous solution, with regulating PH with 10% sodium hydroxide behind the water precipitating is 6.5 supernatant and boric acid, ethyl hydroxybenzoate, Borax, propylparaben, behind the sodium chloride solution mix homogeneously, join with water for injection is rare, it is Flos Buddlejae that rare timing makes the medicinal liquid gross weight after rare joining, Semen Cassiae, Flos Chrysanthemi, Fructus Tribuli, the Herba Equiseti Hiemalis, Rhizoma Et Radix Notopterygii, boric acid, Borax, sodium chloride, ethyl hydroxybenzoate, 10 times of propylparaben gross weight.
(8) with the filter method of embodiment 9.
Embodiment 11
Its prescription and preparation method and used equipment is substantially with embodiment 1, the bile that only different is with Dinodon rufozonatum (Cantor).
Embodiment 12
Its preparation method and used equipment are substantially with embodiment 1, only different is 2.05 kilograms of Flos Buddlejaes, 1.65 kilograms of Semen Cassiaes, 1.65 kilograms of Flos Chrysanthemis, 0.825 kilogram of Fructus Tribuli, 0.825 kilogram of Herba Equiseti Hiemalis, 0.575 kilogram of Rhizoma Et Radix Notopterygii, 0.2 kilogram of Fel Ursi, Borneolum Syntheticum are raw material for 0.05 kilogram, with above-mentioned Chinese crude drug raw material through extracting, concentrate, water precipitating, decolouring, rarely joining, filter a kind of eye drop that forms.
Its preparation method is:
Processing step (1), (2), (3), (4), (5) are fully with embodiment 1.
(6) supernatant behind water precipitating adds the aqueous solution of 0.2 kilogram of dissolved Fel Ursi, and regulating PH with 10% sodium hydroxide solution is 6.5, adds through sodium hydroxide to regulate the medicinal carbon that PH is 6.5 amount of liquid medicine 1%, boils and decolours in 30 minutes.
(7) carry out rare joining.Rare timing 0.05 kilogram of Borneolum Syntheticum of anhydrous alcohol solution, the weight of the used dehydrated alcohol of dissolving Borneolum Syntheticum is 1.5 times of Borneolum Syntheticums.With the clear liquor after the decolouring and the alcoholic solution mix homogeneously of Borneolum Syntheticum, join with water for injection is rare, making medicinal liquid gross weight after rare joining is Flos Buddlejae, Semen Cassiae, Flos Chrysanthemi, Fructus Tribuli, Herba Equiseti Hiemalis, Rhizoma Et Radix Notopterygii, Fel Ursi, Borneolum Syntheticum gross weight 9 times.
(8) filter, during filtration rare dosing is filtered through the politef filter stick of 0.2um and the filter membrane of 0.2um successively, the pressure of control filter stick is 0.03Mpa during filtration.
Claims (10)
1. eye drop, it is characterized in that, the Chinese crude drug raw material comprises Flos Buddlejae 1.025～12.3 weight portions, Semen Cassiae, 0.825～9.9 weight portion, Flos Chrysanthemi, 0.825～9.9 weight portion, Fructus Tribuli 0.825～9.9 weight portion, Herba Equiseti Hiemalis's 0.825～9.9 weight portion, Rhizoma Et Radix Notopterygii 0.575～6.90 weight portion, and above-mentioned raw materials is through extracting, concentrate, precipitate with ethanol, water precipitating, rarely joining, filter a kind of eye drop that forms.
2. according to a kind of eye drop of claim 1, it is characterized in that the vertebrate gallbladder that also contains except that the people is bile 0.1～1.2 weight portion, Borneolum Syntheticum 0.025～0.3 weight portion.
3. according to one of them a kind of eye drop of claim 1.2, it is characterized in that, also contain boric acid 0.6～7.2 weight portion, ethyl hydroxybenzoate 0.00675～0.081 weight portion, Borax 0.0285～0.342 weight portion, propylparaben 0.00675～0.081 weight portion, sodium chloride 0.11～1.32 weight portion.
4. according to a kind of eye drop of claim 2, it is characterized in that said vertebrate gallbladder except that the people is that bile is wherein a kind of of Fel Ursi, Fel Bovis seu Bubali, horse bile, sheep bile, Fel Sus domestica, Fel Gallus domesticus, fish bile, Fel Serpentis.
5. the preparation method of an eye drop is characterized in that, comprises following processing step:
(1) get the raw materials ready by Flos Buddlejae 1.025～12.3 weight portions, Semen Cassiae 0.825～9.9 weight portion, Flos Chrysanthemi 0.825～9.9 weight portion, Fructus Tribuli 0.825～9.9 weight portion, Herba Equiseti Hiemalis's 0.825～9.9 weight portion, Rhizoma Et Radix Notopterygii 0.575～6.90 weight portion,
(2) the above-mentioned Chinese crude drug raw material of getting ready is placed extractor, add and extract solvent, said extraction solvent is a water, the weight of extracting for the first time the extraction aqueous solvent that adds is Flos Buddlejae, Semen Cassiae, Flos Chrysanthemi, Fructus Tribuli, Herba Equiseti Hiemalis, Rhizoma Et Radix Notopterygii gross weight 4～12 times, heated and boiled, kept under the state 1～4 hour boiling, draw and obtain the medicinal liquid that extracts for the first time; The weight of extracting for the second time the extraction aqueous solvent that adds is Flos Buddlejae, Semen Cassiae, Flos Chrysanthemi, Fructus Tribuli, Herba Equiseti Hiemalis, Rhizoma Et Radix Notopterygii gross weight 3～5 times, and heated and boiled kept under the state 0.5～2 hour boiling, and obtained the medicinal liquid that extracts for the second time;
(3) with the medicinal liquid mix homogeneously of extracted twice, heat concentratedly, the proportion that is concentrated to concentrated solution is 1.10～1.12,
(4) under stirring, in concentrated solution, add ethanol, reach the 60-85% percetage by weight to concentration of ethanol, leave standstill and carried out precipitate with ethanol in 12-48 hour, leave standstill the back and extract its supernatant, reclaim ethanol,
(5) in the medicinal liquid after reclaiming ethanol through precipitate with ethanol, the 2-8 water for injection doubly that the medicinal liquid gross weight behind the ethanol is reclaimed in adding leaves standstill and carried out water precipitating in 65-110 hour,
(6) supernatant behind the water precipitating is regulated PH6.0～7.0 with aqueous slkali, add water for injection at the supernatant after being adjusted to PH to 6.0～7.0 and carry out rare joining, the water for injection that is added, the gross weight that makes medicinal liquid is 8～51.6 of Flos Buddlejae, Semen Cassiae, Flos Chrysanthemi, Fructus Tribuli, Herba Equiseti Hiemalis, a Rhizoma Et Radix Notopterygii gross weight, get rare dosing
(7) medicinal liquid after rare joining is filtered.
6. according to the preparation method of a kind of eye drop of claim 5, it is characterized in that, said simmer down to vacuum concentration, its vacuum degree control is concentrated into the concentrated solution ratio 1.10-1.12 that weighs at 0.05-0.09Mpa when concentrating.
7. according to the preparation method of a kind of eye drop of claim 5, it is characterized in that, said precipitate with ethanol is under the state that stirs, the ethanol that slowly adds 0.5-1.5 80% percetage by weight doubly of concentrated solution weight, stir, under the state that stirs, slowly add dense ethanol again, make ethanol in the alcohol deposit fluid of integral body, concentration of alcohol reaches the 60-85% percetage by weight, leaves standstill 12～48 hours.
8. according to the preparation method of a kind of eye drop of claim 5, it is characterized in that, in the supernatant behind water precipitating, the aqueous solution that adds the vertebrate bile 0.1-1.2 weight portion of dissolving, regulating PH with the aqueous slkali of 7～20% percetages by weight is 6.0-7.0, adding is adjusted to the medical activated carbon of 1-3% of the medicinal liquid liquid measure of 6.0-7.0 through aqueous slkali, boiled 20-60 minute, decolouring, is that filter membrane sucking filtration to the medicinal liquid of 0.45mm is clarified with four metafiltration paper and one deck specification successively, clarifying medicinal liquid.
9. the preparation method of a kind of eye drop according to Claim 8, it is characterized in that, clarification medicinal liquid after the decolouring is carried out rare joining, said rare joining is at first with the boric acid of 0.6-7.2 weight portion, 0.00675-0.081 the ethyl hydroxybenzoate of weight portion, 0.0285-0.342 the Borax of weight portion, 0.00675-0.081 the propylparaben of weight portion, 0.11-1.32 weight portion sodium chloride is made aqueous solution with the water for injection dissolving, the Borneolum Syntheticum of reuse anhydrous alcohol solution 0.025-0.3 weight portion is made into alcoholic solution, the used alcoholic acid weight of dissolving Borneolum Syntheticum is 1.0 times～8 times of Borneolum Syntheticum weight, to clarify medicinal liquid and boric acid, Borax, sodium chloride, ethyl hydroxybenzoate, the aqueous solution of propylparaben and the alcoholic solution of Borneolum Syntheticum mix, behind the mix homogeneously, join with water for injection is rare, making the gross weight of the medicinal liquid after rare joining is Flos Buddlejae, Semen Cassiae, Flos Chrysanthemi, Fructus Tribuli, the Herba Equiseti Hiemalis, Rhizoma Et Radix Notopterygii, vertebrate bile, Borneolum Syntheticum, boric acid, ethyl hydroxybenzoate, Borax, propylparaben, the 8-51.6 of sodium chloride gross weight doubly, mix homogeneously, the rare dosing after rare joining.
10. according to the preparation method of a kind of eye drop of claim 9, it is characterized in that, rare dosing filtered through the politef filter stick of 0.2um and the filter membrane of 0.2um successively that the pressure of control filter stick is to begin between the 0.025-0.035Mpa to filter during filtration.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2007101439088A CN100389791C (en) | 2007-08-13 | 2007-08-13 | Eye drops and preparation method thereof |
Applications Claiming Priority (1)
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104547621A (en) * | 2015-01-21 | 2015-04-29 | 訾庆彬 | Eye protection traditional Chinese medicine |
| CN105878344A (en) * | 2016-05-10 | 2016-08-24 | 赫尔森江苏医药有限公司 | Eye drop and preparation method and application thereof |
| CN107184643A (en) * | 2017-05-24 | 2017-09-22 | 深圳市欧斯特尔实业有限公司 | A kind of eyesight-improving health care function liquid containing snake gall and preparation method thereof |
| CN107412552B (en) * | 2017-08-07 | 2020-10-02 | 秦皇岛康视生物科技有限公司 | Eye protection liquid capable of treating myopia of children and preparation method thereof |
| CN109381571A (en) * | 2018-11-26 | 2019-02-26 | 韩佳志 | A kind of Chinese medicine compound prescription eye drops for improving eyesight and preparation method |
| CN110693824A (en) * | 2019-11-01 | 2020-01-17 | 马跃宏 | Liquid preparation for relieving eye fatigue and preparation method thereof |
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| CN1085792A (en) * | 1993-07-30 | 1994-04-27 | 高峰 | Treat bathomorphic liniment and preparation method thereof |
| CN1037237C (en) * | 1994-08-11 | 1998-02-04 | 林继华 | "Qianliming" oculentum |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1085792A (en) * | 1993-07-30 | 1994-04-27 | 高峰 | Treat bathomorphic liniment and preparation method thereof |
| CN1037237C (en) * | 1994-08-11 | 1998-02-04 | 林继华 | "Qianliming" oculentum |
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| 千里明眼膏致不良反应. 周莉等.中国现代应用药学杂志，第15卷第4期. 1998 |
| 千里明眼膏致不良反应. 周莉等.中国现代应用药学杂志，第15卷第4期. 1998 * |
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| CN101095722A (en) | 2008-01-02 |
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Effective date of registration: 20081205 Address after: No. 76, unity Road, Shenhe District, Shenyang, Liaoning Patentee after: Liaoning Qianliming Pharmaceutical (Group) Co., Ltd. Address before: No. 76, unity Road, Shenhe District, Shenyang, Liaoning Patentee before: Lin Jihua |
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Owner name: LIAONING QIANLIMING PHARMACY ( GROUP ) CO., LTD. Free format text: FORMER OWNER: LIN JIHUA Effective date: 20081205 |