CN102309591B - Formula and preparation method of compound coptis injection - Google Patents
Formula and preparation method of compound coptis injection Download PDFInfo
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Abstract
Belonging to the field of traditional Chinese medicinal preparations, the invention relates to a compound coptis injection resisting staphylococcus aureus infection and inhibiting drug resistant staphylococcus aureus and its preparation technology. The preparation method comprises the steps of: formulating a prescription with four traditional Chinese medicinal materials of coptis, cape jasmine, phellodendron and scutellaria in certain proportion; then conducting the processes of water extraction, deposition with ethanol of different concentrations, deposition with improved gelatin, silica gel adsorption for decolouring, etc. With stable performance, the prepared compound coptis injection is pure natural, safety and nontoxic, and has an obvious anti-infection effect and an obvious function in drug resistance reversal. Suitable for pyogenic infection caused by staphylococcus aureus and drug resistant staphylococcus aureus, the injection provided in the invention boasts good market prospects and corresponding social benefits as well as economic benefits.
Description
Technical field
The invention belongs to field of traditional Chinese, be specifically related to a kind of anti-infection of staphylococcus aureus and the injection and the preparation technology thereof that suppress the drug resistance staphylococcus aureus, particularly a kind of novel livestock and poultry muscle injection use compound Rhizoma Coptidis injection and preparation method thereof.
Background technology
Rhizoma Coptidis toxic materials clearing away decoction is the classical Chinese medicinal formulae of heat-clearing and toxic substances removing, and its main component is Rhizoma Coptidis, Cortex Phellodendri, Radix Scutellariae, Fructus Gardeniae four flavor Chinese medicines.Rhizoma Coptidis with big bitter Great Cold in the side is monarch, and minister is with Radix Scutellariae, and assistant is with Cortex Phellodendri and Fructus Gardeniae, and four medicines share, and pathogenic fire purging is to separate pyretic toxicity.Rhizoma Coptidis toxic materials clearing away decoction still has dosage forms such as powder, granule, capsule except that traditional decoction.Though decoction can be added and subtracted according to the state of an illness flexibly, the trouble of decocting is then arranged, carry inconvenience, the difficult pharynx of bitter in the mouth, defective such as be easy to injure one's stomach; Powder, granule and capsule have and absorb slow, bitter in the mouth, and gastrointestinal mucosa is had stimulation, are prone to when taking cause nausea, defective such as vomiting.For overcoming the defective of these dosage forms, the spy carries out the invention research of Rhizoma Coptidis toxic materials clearing away decoction novel form one injection.Chinese medicine is " to be guidance with the Chinese medical theory, to adopt modern science and technology and method, from Chinese medicine or herbal mixture, extract the injection that active substance is processed." Chinese medicine directly gets into body and be distributed to histoorgan, walked around the first-pass effect of liver, has the bioavailability height, and is easy to use, advantage such as curative effect is fast.But because the Chinese medicine compound flavour of a drug are many; Complex chemical composition and character are different; The compound injection that method for distilling and preparation technology's imperfection may cause processing exists that clarity is not good enough, Impurity removal is incomplete; Problems, the particularly existence of impurity such as tannin, protein such as active constituent content and curative effect instability cause the body untoward reaction easily.
Summary of the invention
The present invention is guidance with the Chinese medical theory; Adopting modern study means and production technology, is foundation with external antibacterial and drug resistance inversion effect, to the active component of representative prescription one Rhizoma Coptidis toxic materials clearing away decoction of heat-clearing and toxic substances removing extract, purification and refining; Confirm the best prescription of flavour of a drug and extraction and purified method; Remove impurity such as protein, tannin, pigment to greatest extent, it is relatively stable, quality controllable to process effective ingredient, can supply the compound coptis chinensis injection of intramuscular injection.
The Chinese medicine preparation that the present invention adopted is: by weight; A kind of poultry are used the compound coptis chinensis injection, by 2～8 parts of Rhizoma Coptidis, and 2～8 parts of Cortex Phellodendris; 2～8 parts of Fructus Gardeniaes; 1～4 part of Radix Scutellariae, with twice of 5～30 times of moisture of raw material gross weight (a time 5～20 times, a time 5～10 times) reflux, extract,, concentrate then, refining forming.
The method for preparing of a kind of compound coptis chinensis injection of the present invention; Take following method; By different material-water ratios extract twice, different concentration ethanol deposition three times, improvement gelatin deposition once, silica gel adsorption decolouring etc. is combined into preparation technology; Be divided into batching, lixiviate, reflux, extract,, concentrate, steps such as purification, decolouring, fill, sterilization, specifically carry out as follows:
(1) batching: take by weighing through oven dry by weight respectively, pulverize and cross 2～8 parts of the crude drug Rhizoma Coptidis of 40 mesh sieves, 2～8 parts of Cortex Phellodendris, 2～8 parts of Fructus Gardeniaes, 1～4 part of Radix Scutellariae;
(2) lixiviate:, add 5～20 times of water room temperature of gross weight and soaked into 2～12 hours with four Chinese medicine powder mixture material;
(3) reflux, extract: reflux, extract, 2 times.The boiling water bath reflux, extract, is 1～3 hour after the lixiviate; Sucking filtration must be filtrated; 5～10 times of amounts of medicinal residues reuse water by volume reflux, extract, 1～3 hour; Sucking filtration is abandoned medicinal residues, merges filtrating twice;
(4) concentrate: the rotary evaporation in vacuo of will filtrating, the medicinal liquid of simmer down to crude drug composition 1～2 grams per milliliter is put and is chilled to room temperature;
(5) purification: slowly add and contain alcohol amount in 95% cold ethanol to the concentrated medicament and reach 50%～65%, the limit edged stirs; Sealing covers completely, leaves standstill 24～48 hours under 4 ℃ of conditions; Sucking filtration is abandoned deposition, alcoholic solution, slowly add again and contain alcohol amount in 95% cold ethanol to the filtrating and reach 65%～80%, the limit edged stirs; Sealing covers completely, leaves standstill 24～48 hours under 4 ℃ of conditions; Sucking filtration is abandoned deposition, must contain alcohol filtrating; To contain alcohol filtrating rotary evaporation in vacuo and reclaim ethanol, and, put and be chilled to room temperature to there not being the alcohol flavor; The gelatin of dosing liquid long-pending 3～5%, the limit edged stirs; Under 4 ℃ of conditions, left standstill 12～24 hours; Slowly add and contain alcohol amount in 95% cold ethanol to the filtrating and reach 75～85%, the limit edged stirs; Sealing covers completely, leaves standstill 24～48 hours under 4 ℃ of conditions; Sucking filtration is abandoned deposition, must filtrate; Rotary evaporation in vacuo reclaims ethanol, to there not being the alcohol flavor, puts and is chilled to room temperature;
(6) decolouring: add the silica gel of above-mentioned medicine liquid volume amount 25%～40%, 20 ℃～40 ℃ decoloured 2～12 hours; Sucking filtration gets injection stock solution, adjusts concentration with water for injection, can be mixed with the injection that concentration is equivalent to crude drug composition 1 grams per milliliter;
(7) fill: but embedding becomes the injection of different size as requested, like the peace bowl of 5 milliliters/, 10 milliliters/specifications;
(8) sterilization: circulation steam disinfection 30 minutes; Promptly get clear, faint yellow or pale brown color compound coptis chinensis injection.
For above-mentioned steps, can further be undertaken by following mode:
(1) batching: take by weighing through oven dry by weight respectively, pulverize and cross 2～8 parts of the crude drug Rhizoma Coptidis of 40 mesh sieves, 2～8 parts of Cortex Phellodendris, 2～8 parts of Fructus Gardeniaes, 1～4 part of Radix Scutellariae;
(2) lixiviate:, add 10～20 times of water room temperature of gross weight and soaked into 4～10 hours with four Chinese medicine powder mixture material;
(3) reflux, extract: reflux, extract, 2 times, the boiling water bath reflux, extract, is 2～3 hours after the lixiviate; Sucking filtration must be filtrated; 5～10 times of amounts of medicinal residues reuse water by volume reflux, extract, 1～3 hour; Sucking filtration is abandoned medicinal residues, merges filtrating twice;
(4) concentrate: the rotary evaporation in vacuo of will filtrating, simmer down to contains the medicinal liquid of crude drug composition 1～2 grams per milliliter, puts to be chilled to room temperature;
(5) purification: slowly add and contain the alcohol amount in 95% cold ethanol (the cold ethanol of indication of the present invention is the ethanol of about 4 ℃ of temperature, down with) to the concentrated medicament and reach 50%～65%, the limit edged stirs; Sealing covers completely, leaves standstill 24～40 hours under 4 ℃ of conditions; Sucking filtration is abandoned deposition, must filtrate, and slowly adds to contain alcohol amount in 95% cold ethanol to the filtrating and reach 65%～80% again, and the limit edged stirs; Sealing covers completely, under 4 ℃ of conditions, leaves standstill 24～40 hours; Sucking filtration is abandoned deposition, must contain alcohol filtrating; To contain alcohol filtrating rotary evaporation in vacuo and reclaim ethanol, and, put and be chilled to room temperature to there not being the alcohol flavor; The gelatin of dosing liquid long-pending 3～5%, the limit edged stirs; Under 4 ℃ of conditions, left standstill 12～24 hours; Slowly add and contain alcohol amount in 95% cold ethanol to the filtrating and reach 75～85%, the limit edged stirs; Sealing covers completely, under 4 ℃ of conditions, leaves standstill 24～48 hours; Sucking filtration is abandoned deposition, must contain alcohol filtrating; Rotary evaporation in vacuo reclaims ethanol to there not being the alcohol flavor, puts and is chilled to room temperature;
(6) decolouring: the silica gel that adds above-mentioned medicine liquid volume amount 25～40% decoloured 2～10 hours for 20 ℃～40 ℃; Sucking filtration gets injection stock solution, adjusts concentration with water for injection, is mixed with the injection that concentration is equivalent to crude drug 1 grams per milliliter;
(7) fill: but embedding becomes the injection of different size as requested, like the peace bowl of 5 milliliters/, 10 milliliters/specifications;
(8) sterilization: circulation steam disinfection 35 minutes; Promptly get clear, faint yellow or pale brown color compound coptis chinensis injection.
As follows, be quality control index with the berberine that content is the highest in the compound coptis chinensis injection, adopt the content of rp-hplc determination berberine.Chromatographic condition is: Luna-C18 (2) post (4.6 * 250mm, 5 μ m), mobile phase is methanol: 6% triethylamine aqueous solution (28: 72).Regulating pH value with phosphoric acid is 3.0, and the detection wavelength is 345nm, and flow velocity is lmL/min, and sample size is 20 μ L, 30 ℃ of column temperatures.
Extract effective ingredient such as alkaloid in Rhizoma Coptidis toxic materials clearing away decoction prescription medical material Rhizoma Coptidis, Cortex Phellodendri, Fructus Gardeniae, the Radix Scutellariae, glycoside, organic acid etc. with water extracting alcohol deposition method, the ethanol precipitation that adds debita spissitudo is then removed impurity.Add for the first time 95% cold ethanol; Make concentrated medicament contain alcohol amount (concentration of alcohol) and reach 50%～65%; Remove starch, inorganic salt etc., add 95% cold ethanol for the second time, make concentrated medicament contain the alcohol amount and reach 65%～80%; Remove deproteinize and polysaccharide, also can remove some tannins, pigment, resin etc. simultaneously.Add the gelatin of medicine liquid volume 3～5% again in the medicinal liquid, remove tannin; Add 95% cold ethanol for the third time and make and contain the alcohol amount and reach 75%～85%, further remove impurity such as tannin.Remove the faint yellow or brown xanchromatic injection material liquid that pigment obtains clear with silica decoloration with absorption after reclaiming ethanol.With content is the highest in the monarch drug Rhizoma Coptidis in the prescription chemical compound one berberine index, adopt the content of berberine in the rp-hplc determination compound coptis chinensis injection, and provide the finger printing of compound coptis chinensis injection as qualitative or quantitative control.
The compound coptis chinensis injection not only has the drug resistance inversion effect, and anti-infection of staphylococcus aureus effect is better, and preparation technology is simple, and cost is low, reduction of expenditure.The preparation process that combines with water extraction, different concentration ethanol deposition three times, improvement gelatin method deposition 1 time, silica gel adsorption decolouring; Effectively remove impurity such as starch, inorganic salt, protein, polysaccharide, tannin, pigment, resin in the Rhizoma Coptidis toxic materials clearing away decoction prescription herbal extract, kept effective ingredient such as alkaloid and salt thereof, glycoside, organic acid.The compound coptis chinensis preparation of the present invention's development is through the preparation check analysis, and each item index meets the requirement under the 1st Chinese medicine item of " Chinese veterinary drug allusion quotation " version in 2005.The preparation stable performance, pure natural, safety non-toxic, curative effect is obvious, is applicable to the pyogenic infection that staphylococcus aureus and drug resistance staphylococcus aureus cause, has good market prospect and corresponding social benefit, economic benefit.
The specific embodiment
Embodiment 1 is below in conjunction with preferred embodiment, to details are as follows according to the specific embodiment provided by the invention:
A kind of poultry are used the compound coptis chinensis injection, by Rhizoma Coptidis 42.86 gram, and Cortex Phellodendri 14.29 grams, Fructus Gardeniae 28.57 grams, Radix Scutellariae 14.29 grams, ultra-pure water 1500 grams extract at twice, precipitate, separate, make with extra care and form.
A kind of poultry carry out with the method for preparing of compound coptis chinensis injection as follows:
(1) take by weighing respectively by weight through drying, pulverize and cross crude drug Rhizoma Coptidis 42.86 grams of 40 mesh sieves, Cortex Phellodendri 14.29 restrains, and Fructus Gardeniae 28.57 restrains, Radix Scutellariae 14.29 grams.
(2), add 10 times of gross weights (1000 gram) ultra-pure water soak at room temperature 2 hours with four Chinese medicine powder mixture material;
(3) boiling water bath reflux, extract, 2 hours;
(4) sucking filtration must be filtrated;
(5) 5 times of amounts of medicinal residues reuse volume (500 gram) boiling water bath reflux, extract, is 2 hours;
(6) sucking filtration is abandoned medicinal residues, merges filtrating twice;
(7) filtrating rotary evaporation in vacuo concentrated filtrate is 1～2 grams per milliliter to containing the crude drug constituent concentration, puts and is chilled to room temperature;
(8) slowly add and contain alcohol amount in 95% cold ethanol to the concentrated medicament and reach 60%, the limit edged stirs;
(9) sealing covers completely, and 4 ℃ of refrigerators left standstill 24 hours;
(10) sucking filtration is abandoned deposition, slowly adds to contain alcohol amount in 95% cold ethanol to the filtrating and reach 80% again, and the limit edged stirs;
(11) sealing covers completely, leaves standstill 48 hours under 4 ℃ of conditions;
(12) sucking filtration is abandoned deposition, must filtrate;
(13) the filtrating rotary evaporation in vacuo reclaims ethanol, to there not being the alcohol flavor, puts and is chilled to room temperature;
(14) gelatin of dosing liquid long-pending 3%, the limit edged stirs;
Left standstill 24 hours under (15) 4 ℃ of conditions;
(16) slowly add and contain alcohol amount in 95% cold ethanol to the filtrating and reach 80%, the limit edged stirs;
(17) sealing covers completely, leaves standstill 48 hours under 4 ℃ of conditions;
(18) sucking filtration is abandoned deposition, must filtrate;
(19) rotary evaporation in vacuo of will filtrating reclaims ethanol, to there not being the alcohol flavor, puts and is chilled to room temperature;
(20) silica gel of adding medicine liquid volume amount 35% decoloured 3 hours for 30 ℃ in above-mentioned solution;
(21) sucking filtration is adjusted original liquid concentration with water for injection, is mixed with the injection that concentration is equivalent to crude drug composition 1～2 grams per milliliter;
(22) embedding becomes 5 milliliters/, 10 milliliters/specification peace bowls;
(23) the circulation steam disinfection is 30 minutes;
(24) promptly get clear, faint yellow or pale brown color compound coptis chinensis injection;
(25) with the berberine be quality control index, adopt reversed phase high-performance liquid chromatography to record that content of berberine is about 20 mg/ml in every batch of compound coptis chinensis injection.
The extracorporeal bacteria inhibitor test of embodiment 2 compound coptis chinensis injections
(1) mensuration of minimum inhibitory concentration (MIC)
Method adopts tube dilution method.The compound coptis chinensis injection is made two times of concentration dilutions that successively decrease, 1～No. 9 in vitro drug level be 0.5,0.25,0.125,0.0625,0.0313,0.0156,0.0078,0.0039,0.00195 grams per milliliter.Prepare the golden yellow staphylococcus liquid of 5 strain drug resistance by general test methods, every pipe all adds bacterium liquid 0.1mL, and No. 10 test tube adds medicinal liquid and do not add bacterium liquid, and as negative control, the o.11 test tube adds bacterium liquid and do not add medicinal liquid, as positive control.Each pipe is put 35 ℃ of shaken cultivation 18 hours, observe and judge the minimum inhibitory concentration (MIC) of medicine.
The MIC of compound coptis chinensis injection mensuration result sees table 1 as a result.The result shows that the compound coptis chinensis injection is 0.0078 grams per milliliter to the minimum inhibitory concentration of Sa1～Sa5.
Table 1 compound coptis chinensis injection is measured the result to the MIC of the golden yellow staphylococcus of drug resistance
(2) antibacterial circle diameter is measured the result
The method cut-off directly is 6 millimeters a sterilization filter paper, drips the compound coptis chinensis injection, behind the natural drying, drips the compound coptis chinensis injection again, repeats 3 times.Get the MH agar culture dish of sterilization, draw 0.1 milliliter of dilution bacterium liquid in plate, even with the glass rod shop.Each plate is divided into 4 districts, sticks the compound coptis chinensis injection scraps of paper then, puts in 35 ℃ of incubators and cultivates 18 hours, measures antibacterial circle diameter with the vernier ruler, averages.
The compound coptis chinensis injection is seen table 2 to the antibacterial circle diameter mensuration result of 5 strain drug resistance staphylococcus aureuses as a result.
The result shows: Sa1, Sa2, Sa4 and Sa5 show as Gao Min to the compound coptis chinensis injection; It is quick during Sa3 shows as.
Table 2 compound coptis chinensis injection antibacterial circle diameter is measured the result
| Resistant strain | Antibacterial circle diameter (millimeter) | Sensitivity |
| Sa1 | 15.75+1.48 | Gao Min |
| Sa2 | 14.75+1.30 | Gao Min |
| Sa3 | 14.50±0.87 | In quick |
| Sa4 | 16.00±1.41 | Gao Min |
| Sa5 | 15.00±0.71 | Gao Min |
The external drug resistance inhibition test of embodiment 3 compound coptis chinensis injections
(1) dull and stereotyped borehole test
Method is cultivated 20h with the drug resistance staphylococcus aureus in the MH fluid medium, after dilution, get 0.1 milliliter and coat on the MH agar culture medium, makes a call to 4 holes with card punch; Back cover; About 20 millimeters of each pitch of holes adds 0.05 milliliter of compound coptis chinensis injection in symmetrical 2 holes, add 0.05 milliliter of ofloxacin or ciprofloxacin (concentration and consumption are with reference to the drug sensitive experiment method) in the adjacent symmetric hole; Cultivate 20h, observed result.
The result is with bacterial growth around two holes, but the zone that has antibacterial not grow between two holes is regarded as drug resistance and suppresses effectively; Antibacterial all grows into lamellar between around two holes and hole; Being regarded as the criterion that drug resistance suppresses invalid effect judges: all long bacterium in the middle of Sa1, Sa3, Sa5 two holes; Length has a small amount of antibacterial between Sa2 and Sa4 two holes; Explain that the compound coptis chinensis injection is strong to Sa1, Sa3, Sa5 drug resistance inhibitory action, to Sa2 and Sa4 drug resistance inhibitory action a little less than.
(2) drug sensitive test paper method
Method with the drug resistance staphylococcus aureus respectively at the compound coptis chinensis injection MH culture fluid that contains Mlc with do not contain in the MH culture fluid of compound coptis chinensis injection 35 ℃ of shaken cultivation and spend the night.Get 0.1 milliliter of culture fluid and coat on the MH agar culture medium, after L shaped glass rod coating evenly, paste ciprofloxacin or ofloxacin drug sensitive test paper, put 35 ℃ and cultivated 18 hours.The record result.
After the drug resistance staphylococcus aureus is handled through the compound coptis chinensis injection as a result, the sensitivity result of variations of different drug sensitive test papers is seen table 3.
Table 3 compound coptis chinensis injection is handled the different drug sensitive test paper antibacterial circle diameters in back and is measured result's (unit millimeter)
The ciprofloxacin drug sensitive test paper to the antibacterial circle diameter of untreated control bacterium between 16.38～17.89 millimeters; And handle the bacterium antibacterial circle diameter between 27.60～30.26 millimeters; Both differences are (P＜0.01) extremely significantly; The ofloxacin drug sensitive test paper to untreated control bacterium antibacterial circle diameter between 16.63～17.00 millimeters; To handling the bacterium antibacterial circle diameter between 29.50～30.60 millimeters; Both differences are (P＜0.01) extremely significantly, explains that drug resistance staphylococcus aureus sensitivity to ciprofloxacin and ofloxacin medicine after the compound coptis chinensis injection is handled improves greatly.
Claims (3)
1. the method for preparing of a compound coptis chinensis injection comprises Rhizoma Coptidis, Cortex Phellodendri; Fructus Gardeniae; Radix Scutellariae is characterized in that: take following method, be combined into preparation technology by different material-water ratios extractions 2 times, ethanol precipitation 3 times, improvement gelatin deposition 1 time, silica gel adsorption decolouring; Be divided into batching, lixiviate, reflux, extract,, concentrate, purification, decolouring, fill, sterilization step, specifically carry out as follows:
(1) batching: take by weighing through oven dry by weight respectively, pulverize and cross 2～8 parts of the crude drug Rhizoma Coptidis of 40 mesh sieves, 2～8 parts of Cortex Phellodendris, 2～8 parts of Fructus Gardeniaes, 1～4 part of Radix Scutellariae;
(2) lixiviate:, add 5～20 times of water room temperature of gross weight and soaked into 2～12 hours with four Chinese medicine powder mixture material;
(3) reflux, extract: reflux, extract, 2 times, the boiling water bath reflux, extract, is 1～3 hour after the lixiviate; Sucking filtration must be filtrated; 5～10 times of amounts of medicinal residues reuse water by volume reflux, extract, 1～3 hour; Sucking filtration is abandoned medicinal residues, merges filtrating twice;
(4) concentrate: the rotary evaporation in vacuo of will filtrating, concentrated filtrate are put and are chilled to room temperature to the medicinal liquid that contains crude drug composition 1～2 grams per milliliter;
(5) purification: slowly add and contain alcohol amount in 95% cold ethanol to the concentrated medicament and reach 50%～65%, the limit edged stirs; Sealing covers completely, leaves standstill 24～48 hours under 4 ℃ of conditions; Sucking filtration is abandoned deposition, must contain pure medicinal liquid, slowly adds to contain alcohol amount in 95% cold ethanol to the filtrating and reach 65%～80% again, and the limit edged stirs; Sealing covers completely, moves under 4 ℃ of conditions to leave standstill 24～48 hours; Sucking filtration is abandoned deposition, must contain alcohol filtrating; To contain alcohol filtrating rotary evaporation in vacuo and reclaim ethanol, and, put and be chilled to room temperature to there not being the alcohol flavor; The gelatin of dosing liquid long-pending 3%～5%, the limit edged stirs; Under 4 ℃, left standstill 12～24 hours; Slowly add and contain alcohol amount in 95% cold ethanol to the filtrating and reach 75%～85%, the limit edged stirs; Sealing covers completely, leaves standstill 24～48 hours under 4 ℃ of conditions; Sucking filtration is abandoned deposition, must filtrate; Rotary evaporation in vacuo reclaims ethanol to there not being the alcohol flavor, puts and is chilled to room temperature;
(6) decolouring: the silica gel that adds above-mentioned medicine liquid volume amount 25%～40% decoloured 2～12 hours for 20 ℃～40 ℃; Sucking filtration gets injection stock solution, adjusts concentration with water for injection, is mixed with the injection that concentration is equivalent to crude drug composition 1 grams per milliliter;
(7) fill: embedding becomes the injection of different size as requested;
(8) sterilization: circulation steam disinfection 30 minutes promptly gets clear, faint yellow or pale brown color compound coptis chinensis injection.
2. the method for preparing of a kind of compound coptis chinensis injection according to claim 1; It is characterized in that: take following method; By different material-water ratios extract twice, different concentration ethanol deposition three times, improvement gelatin deposition once, the silica gel adsorption decolouring is combined into preparation technology; Be divided into batching, lixiviate, reflux, extract,, concentrate, purification, decolouring, fill, sterilization step, specifically carry out as follows:
(1) batching: take by weighing through oven dry by weight respectively, pulverize and cross 2～8 parts of the crude drug Rhizoma Coptidis of 40 mesh sieves, 2～8 parts of Cortex Phellodendris, 2～8 parts of Fructus Gardeniaes, 1～4 part of Radix Scutellariae;
(2) lixiviate:, add 10～20 times of water room temperature of gross weight and soaked into 4～10 hours with four Chinese medicine powder mixture material;
(3) reflux, extract: reflux, extract, 2 times, the boiling water bath reflux, extract, is 2～3 hours after the lixiviate; Sucking filtration must be filtrated; 5～10 times of amounts of medicinal residues reuse water by volume reflux, extract, 1～3 hour; Sucking filtration is abandoned medicinal residues, merges filtrating twice;
(4) concentrate: the rotary evaporation in vacuo of will filtrating, concentrated filtrate are put and are chilled to room temperature to the medicinal liquid that contains crude drug composition 1～2 grams per milliliter;
(5) purification: slowly add and contain alcohol amount in 95% cold ethanol to the concentrated medicament and reach 50%～65%, the limit edged stirs; Sealing covers completely, leaves standstill 24～40 hours under 4 ℃ of conditions; Sucking filtration is abandoned deposition, must contain alcohol filtrating, slowly adds to contain the alcohol amount in 95% cold ethanol to the filtrating and reach 65%～80% again, and the limit edged stirs; Sealing covers completely, leaves standstill 24～40 hours under 4 ℃ of conditions; Sucking filtration is abandoned deposition, must contain alcohol filtrating; Rotary evaporation in vacuo reclaims ethanol, to there not being the alcohol flavor, puts and is chilled to room temperature; The gelatin of dosing liquid long-pending 3～5%, the limit edged stirs; Left standstill 12～24 hours under 4 ℃ of conditions; Slowly add and contain alcohol amount in 95% cold ethanol to the filtrating and reach 75%～85%, the limit edged stirs; Sealing covers completely, leaves standstill 24～48 hours under 4 ℃ of conditions; Sucking filtration is abandoned deposition, must contain alcohol filtrating; Rotary evaporation in vacuo reclaims ethanol, to there not being the alcohol flavor, puts and is chilled to room temperature;
(6) decolouring: in above-mentioned solution, add the silica gel of medicine liquid volume amount 25～40%, 20 ℃～40 ℃ decoloured 2～10 hours; Sucking filtration gets injection stock solution, adjusts liquor strength with water for injection, is mixed with the injection that concentration is equivalent to crude drug composition 1 grams per milliliter;
(7) fill: embedding becomes the injection of different size as requested;
(8) sterilization: circulation steam disinfection 35 minutes promptly gets clear, faint yellow or pale brown color compound coptis chinensis injection.
3. the method for preparing of a kind of compound coptis chinensis injection according to claim 1; It is characterized in that: carry out content detection as follows; With the berberine that content is the highest in the compound coptis chinensis injection is quality control index, adopts the content of rp-hplc determination berberine; Chromatographic condition is: Luna-C18 (2) post, mobile phase are that Jia Chun ︰ 6% triethylamine aqueous solution is 28 ︰ 72, and regulating pH value with phosphoric acid is 3.0, and the detection wavelength is 345nm, and flow velocity is 1mL/min, and sample size is 20 μ L, 30 ℃ of column temperatures.
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Family Cites Families (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1207028C (en) * | 2002-12-30 | 2005-06-22 | 南京中医药大学 | Method for preparing 'Antidotal Decoction of Coptidis' solid preparation with combination of film and resin |
| CN1669570A (en) * | 2004-03-19 | 2005-09-21 | 丁永芳 | Medicinal composition for treating senile dementia and vascular dementia and preparing process thereof |
| CN100339098C (en) * | 2005-12-30 | 2007-09-26 | 山东省中医药研究院 | Application of coptic toxin resolving decoction in preparation of medicine for predventing and treating tumour chemotherapy tolerance |
| CN101336989A (en) * | 2007-07-05 | 2009-01-07 | 周秋丽 | New use of Chinese goldthread detoxication decoction in treating parkinsonism and parkinsonian syndrome |
| CN101181403A (en) * | 2007-12-12 | 2008-05-21 | 首都师范大学 | Pharmaceutical combination for curing hyperlipemia symptoms and preparation method thereof |
| CN101757207A (en) * | 2008-10-21 | 2010-06-30 | 天津生机集团股份有限公司 | Nanometer coptis antidotal preparation for birds and preparation method |
| CN101455749A (en) * | 2008-11-25 | 2009-06-17 | 洛阳市康一生物科技有限公司 | Combination method of heat-clearing and antitoxic medicine |
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