CN1935162A - Chinese medicine concentrate andits preparing method - Google Patents

Chinese medicine concentrate andits preparing method Download PDF

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Publication number
CN1935162A
CN1935162A CN 200510015123 CN200510015123A CN1935162A CN 1935162 A CN1935162 A CN 1935162A CN 200510015123 CN200510015123 CN 200510015123 CN 200510015123 A CN200510015123 A CN 200510015123A CN 1935162 A CN1935162 A CN 1935162A
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chinese medicine
reverse osmosis
concentrate
osmosis membrane
temperature
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孙小兵
张文生
张爱华
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Tianjin Tasly Pharmaceutical Co Ltd
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Tianjin Tasly Pharmaceutical Co Ltd
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Abstract

The present invention discloses a Chinese medicine concentrate. It is obtained by concentrating aqueous extract of said Chinese medicine by means of reverse osmosis membrane technology. The described reverse osmosis membrane is made up by using the following materials: cellulose, polyamide, polyphenylmethanamide, aromatic heterocycle, polysulfone, polyether sulphone, polyolefine, silicone rubber, fluorinated polymer, ceramics and inorganic polymer. The pressure of concentration process is 5-80 kg/sq.m, its temperature is 10-100 deg.C and liquid flow speed is 10-100 L/h, Besides, said invention also provides the concrete steps of its preparation method.

Description

A kind of Chinese medicine concentrate and preparation method thereof
Technical field
The present invention relates to Chinese medicine concentrate that a kind of Chinese medicine concentrate, especially Chinese medicine aqueous extract that adopts reverse osmosis membrane technology preparation obtain and preparation method thereof after reverse osmosis membrane technology concentrates.
Background technology
Concentration step is a crucial and requisite step in the Chinese medicine extracts active ingredients process, in the prior art, mainly takes uncovered concentrating and concentrating under reduced pressure, and wherein concentrating under reduced pressure is used more general because relative temperature is lower.But above-mentioned two kinds of method self properties have determined it to have the energy consumption height, and the operating time is long, the shortcoming of operative temperature height (minimum operation temperature>60 ℃), this is very disadvantageous for quite a few thermal sensitivity effective ingredient in the Chinese medicine, and heating certainly will cause its decomposition, the decline of tiring for a long time.Therefore, choose more energy-conservation, concentrate mode efficiently, energy savings reduces loss of effective components, becomes the matter of great urgency of development herbal pharmaceutical.
The reverse osmosis membrane concentration technique is meant the promotion by means of outside energy or chemical potential difference, selective osmosis by specific film, realization to the solute in the mixture separate with solvent, the technology of classification, purification or enrichment, because the many advantages of himself, the reverse osmosis membrane separation concentration technique is considered to one of the most rising new and high technology in mid-term 21 century, and its application develops into chemical industry, food, the paper industry separation of some organic and inorganic matter and concentrates from early stage desalination.
The reverse osmosis membrane separation concentration process is a process efficiently normally, do not undergo phase transition in the membrance separation process, heating or refrigerative energy consumption are very low, usually carry out at normal temperatures, be particularly suitable for separation, the classification and concentrated of heat-sensitive substance, help keeping biological activity, the physical and chemical stability of product, can significantly reduce loss of active ingredients.In addition, the movement-less part of the equipment that is adopted own, install simple, easy to operate, be easy to automatization and easy to maintenance; Disposal ability can in very large range change, and efficient, equipment unit price, operating cost then change not quite.And with respect to general concentration technique, the product quality that reverse osmosis membrane technology is produced is excellent more.Therefore, reverse osmosis membrane technology has significant advantage with respect to existing concentration technique, can replace chemical industry operation unit such as distillation extraction in the pharmaceutical technology, evaporation, absorption.
Reverse osmosis membrane technology is mainly used in the preparation of pure water or mineral water, application in pharmaceutical field seldom, and mainly concentrate on the preparation of biological product: disclose the RO reverse osmosis selectivity method of purification that bioactive peptide is purified in the Margarita enzymolysis solution as Chinese patent CN1415627, Chinese patent CN1569226 mentions with reverse osmosis and concentrates hirudin.Its application example report in the field of Chinese medicines is then considerably less, and in this example few in number, can be applicable to almost not having of technology production, also be in conceptual phase mostly, only be to mention this technology, but do not have concrete application parameter, as Chinese patent CN1593582.So the industrialization of reverse osmosis membrane technology in field of traditional Chinese medicine pharmacy has very important realistic meaning.
Summary of the invention
One of purpose of the present invention is according to the deficiencies in the prior art, provides a kind of Chinese medicine concentrate, especially Chinese traditional medicine water extract of obtaining of concentrating through reverse osmosis membrane technology to concentrate the Chinese medicine concentrate that obtains through reverse osmosis membrane technology.
Another object of the present invention provides the preparation method of this Chinese medicine concentrate.
The present invention is implemented by following technical scheme.
Chinese medicine concentrate of the present invention is characterized in that, to be this Chinese traditional medicine water extract through reverse osmosis membrane technology concentrate makes.
Wherein, described Chinese traditional medicine water extract is meant generalized water extract, the needs that promptly to be solvent with water carry out obtaining after conventional the extraction to Chinese medicine carry out spissated solution (water extract truly), or other organic solvents that contain that obtain through processing after to Chinese medicine extraction with solvent are lower than 30% aqueous solution.As containing eluent after containing the alcohol amount in filtrate after alcohol amount is lower than 30% alcohol extracting-water precipitating, the filtrate and being lower than filtrate, macroporous adsorbent resin behind 30% the water extract-alcohol precipitation and separating etc. in the filtrate; The alcohol amount of containing in preferred water extract and the filtrate is lower than the filtrate behind 30% the alcohol extracting-water precipitating; The best is the water extract.
In the present invention, during all uses " Chinese traditional medicine water extract " term, promptly show it is one of above-mentioned two kinds of solution; And when using " water extract " term, only show that then being is the solution that obtains after solvent extracts with water.
Described reverse osmosis membrane to be selected from but the material that is not limited to following kind make: cellulose, polyamide, polyphenyl Methanamide, aromatic heterocycle, polysulfones, polyether sulfone, TPO, silicone rubber, fluoro containing polymers, pottery, inorganic polymer; Preferably make: cellulose, polyamide, polyphenyl Methanamide, polysulfones, polyether sulfone, pottery, inorganic polymer with the material of following kind; The best is made with the material of following kind: polyamide, polysulfones, pottery, inorganic polymer class.
Described concentration process pressure limit is 5~80kg/m 2, preferred 10~80kg/m 2, more preferably 10~60kg/m 2, the best is 10~40kg/m 2
Described concentration process temperature range is: 10~100 ℃, preferred 10~80 ℃, more preferably 10~60 ℃, the best is 20~35 ℃.
Described concentration process flow rate of liquid is: 10~100L/h, and preferred 20~80L/h, more preferably 30~60L/h, the best is 40~50L/h.
Chinese medicine concentrate of the present invention is the compositions of native compound or native compound, mostly is the liquid in certain density range.This liquid can directly add acceptable accessories and make preparation, also can be the extract of single in the compound recipe or a few flavor medicines, after mixing with the extract of other medical materials in the prescription, makes final product through preparation process again.
The preparation method of Chinese medicine concentrate of the present invention may further comprise the steps:
1, Chinese crude drug extracts with The suitable solvent;
2, extracting solution merges, and puts cold solution to be concentrated, or the preliminary remove impurity of merge extractive liquid, is got solution to be concentrated, or goes up macroporous adsorbent resin and get solution to be concentrated;
3, solution to be concentrated is concentrated by reverse osmosis membrane, get concentrate.
Wherein the extraction described in the step 1 comprises conventional Chinese medicine extraction method, as immersion, backflow, ultrasonic, extract solvent and determine according to the character of effective ingredient in the Chinese medicine that extracts, can be organic solvent, also can be water, can also be water and the mixing of organic solvent; Preferred solvent is a water.
Solution to be concentrated described in the step 2 is a Chinese medicine extraction liquid, i.e. water extract or other organic solution.
Macroporous adsorbent resin described in the step 2 is an acceptable macroporous adsorbent resin in the pharmaceutical industry, as D101, H103, D3520, D4006, D4020, D14, D16, AB-8, SA-1, X-5, HPD100, HPD400 etc.
Concentration process pressure limit described in the step 3 is 5~80kg/m 2, preferred 10~80kg/m 2, more preferably 10~60kg/m 2, the best is 10~40kg/m 2Described concentration process temperature range is: 10~100 ℃, preferred 10~80 ℃, more preferably 10~60 ℃, the best is 20~35 ℃; Described concentration process flow rate of liquid is: 10~100L/h, and preferred 20~80L/h, more preferably 30~60L/h, the best is 40~50L/h.
Reverse osmosis membrane described in the step 3 to be selected from but the material that is not limited to following kind make: cellulose, polyamide, polyphenyl Methanamide, aromatic heterocycle, polysulfones, polyether sulfone, TPO, silicone rubber, fluoro containing polymers, pottery, inorganic polymer; Preferably make: cellulose, polyamide, polyphenyl Methanamide, polysulfones, polyether sulfone, pottery, inorganic polymer with the material of following kind; The best is made with the material of following kind: polyamide, polysulfones, pottery, inorganic polymer.
In preparation Chinese medicine concentrate of the present invention, the gained dialysis solution can be directly used in and drink, or alternative distilled water is used for water for injection.
The present invention has following beneficial effect:
1. reduce the decomposes of heat-sensitive materials;
2. membrane material does not have absorption to effective ingredient;
3. save the steam energy consumption;
4. quick;
5. dialysis solution can be directly used in utilization, or alternative distilled water is used for water for injection.
The specific embodiment
Variation test and specific embodiment below by Chinese medicine active constituent content before and after the reverse osmosis membrane processing further specify the present invention, but are not construed as limiting the invention.
Embodiment 1
Radix Salviae Miltiorrhizae 60kg, Radix Notoginseng 20kg adds 6 times of water gagings and extracts twice, and each 2 hours, merge extractive liquid,, 200 order filter clothes filter, and put and are chilled to room temperature.Last reverse osmosis membrane concentrator adopts polyamide-based 6m 2Reverse osmosis membrane, pressure 12-35kg/m 2, 10 ℃ of temperature, flow velocity 45L/h, being concentrated into relative density is 1.06~1.20 (40 ℃), promptly gets concentrate, sprays into dextrin 15kg, it is dry to granulate, canned capsule.
Adopt the HPLC method that extracting solution and concentrate are measured, the results are shown in Table 1.
Content of Danshensu contrast before and after the table 1 compound Salviae Miltiorrhizae extracting solution membrance separation
Extracting solution (before crossing film) Concentrate (after crossing film)
Proportion 1.00 1.06~1.08
Weight (kg) 50 15
Content of Danshensu (mg/g) 0.99 3.28
Total amount (mg) 49.5 49.2
The result shows that reverse osmosis membrane does not have absorption substantially.
Embodiment 2
Radix Bupleuri 20kg adds 6 times of water gagings and extracts 2 times, and each 1 hour, merge extractive liquid,, 200 order filter clothes filter, and put and are chilled to room temperature.Last membrance concentration equipment adopts polysulfones 6m 2Reverse osmosis membrane, pressure 20-40kg/m 2, 20 ℃ of temperature, flow velocity 60L/h, being concentrated into relative density is 1.06~1.20 (40 ℃), promptly gets concentrate, adds Polyethylene Glycol-6000 adjuvant 15kg, drop pill.
Adopt the HPLC method that extracting solution and concentrate are measured, the results are shown in Table 2.
Total saponin content contrast before and after the table 2 Radix Bupleuri extracting solution membrance separation
Extracting solution (before crossing film) Concentrated solution (after crossing film)
Weight (kg) 100 20
Total saponin content (mg/g) 0.15 0.73
Total amount (mg) 15 14.6
The result shows that reverse osmosis membrane does not have absorption substantially.
Embodiment 3
Radix Notoginseng 20kg adds 8 times of water gagings and extracts 2 times, and each 2 hours, merge extractive liquid,, 200 order filter clothes filter, and put and are chilled to room temperature.Last membrance concentration equipment adopts polyether sulfone 6m 2Reverse osmosis membrane, pressure 30-50kg/m 2, 35 ℃ of temperature, flow velocity 75L/h, being concentrated into relative density is 1.06~1.20 (40 ℃), promptly gets concentrate.
Embodiment 4
Radix Salviae Miltiorrhizae 20kg adds 6~8 times of water gagings and extracts 2 times, and each 1 hour, merge extractive liquid,, 200 order filter clothes filter, and put and are chilled to room temperature.Last membrance concentration equipment adopts cellulose family 6m 2Reverse osmosis membrane, pressure 50-70kg/m 2, 50 ℃ of temperature, flow velocity 85L/h, being concentrated into relative density is 1.05~1.20 (40 ℃), promptly gets concentrate.
Embodiment 5
Radix Ginseng 20kg adds 6 times of water gagings and extracts 2 times, and each 2 hours, merge extractive liquid,, 200 order filter clothes filter, and put and are chilled to room temperature.Last membrance concentration equipment adopts polyamide-based 6m 2Reverse osmosis membrane, pressure 60-80kg/m 2, 25 ℃ of temperature, flow velocity 80L/h, being concentrated into relative density is 1.06~1.20 (40 ℃), promptly gets concentrate.
Embodiment 6
Radix Astragali 20kg adds 6 times of water gagings and extracts 2 times, and each 1 hour, merge extractive liquid,, 200 order filter clothes filter, and put and are chilled to room temperature.Last membrance concentration equipment adopts polyphenyl benzamide type 6m 2Reverse osmosis membrane, pressure 20-40kg/m 2, 35 ℃ of temperature, flow velocity 65L/h, being concentrated into relative density is 1.06~1.25 (40 ℃), promptly gets concentrate.
Embodiment 7
Radix Codonopsis 30kg adds 5 times of water gagings and extracts 2 times, and 2 hours for the first time, 1 hour for the second time, merge extractive liquid,, 200 order filter clothes filter, and put and are chilled to room temperature.Last membrance concentration equipment adopts ceramic 2m 2Reverse osmosis membrane, pressure 10-25kg/m 2, 100 ℃ of temperature, flow velocity 50L/h, being concentrated into relative density is 1.06~1.25 (40 ℃), promptly gets concentrate.
Embodiment 8
Radix Scutellariae 3kg section, decocting boils 3 times, and 2 hours for the first time, the 2nd, 3 time each 1 hour, collecting decoction filtered, and 200 order filter clothes filter, and put and are chilled to room temperature.Last membrance concentration equipment adopts aluminium oxide, zirconium oxide polymer 2m 2Reverse osmosis membrane, pressure 15-30kg/m 2, 80 ℃ of temperature, flow velocity 55L/h is concentrated into density 1.06~1.12 (60 ℃), adding 2mol/L hydrochloric acid solution adjusting pH value in 80 ℃ is 1.0~2.0, is incubated 1 hour, leaves standstill 24 hours, filters, the precipitation wash with water to pH be 5.0, continuing and being washed till pH value with 70% ethanol is 7.0, cold drying is standby; Flos Lonicerae 30kg, Fructus Forsythiae 6kg soak half an hour, decoct 2 times, and each 1.5 hours, filter, merging filtrate is put and is chilled to room temperature.Last membrance concentration equipment adopts cellulose family 6m 2Reverse osmosis membrane, pressure 20-35kg/m 2, 25 ℃ of temperature, flow velocity 60L/h, be concentrated into density 1.20~1.25 (40 ℃), stir down, it is an amount of slowly to add ethanol, make and contain alcohol amount and reach 75%, fully stir, left standstill the leaching supernatant 12 hours, it is an amount of that residue adds 75% ethanol, stir evenly, left standstill 12 hours, filter, merge ethanol liquid, reclaim ethanol and do not distinguish the flavor of, and be concentrated into the clear paste that relative density is 1.30~1.32 (60~65 ℃), drying under reduced pressure to there being alcohol, be ground into fine powder with Radix Scutellariae extract, add right amount of auxiliary materials such as dextrin, make granule 2000g, promptly.
Embodiment 9
Radix Salviae Miltiorrhizae 20kg, 80~90% ethanol extractions three times, each 1 hour, merge extractive liquid, was put and is chilled to room temperature.Last membrance concentration equipment adopts ceramic 2m 2Reverse osmosis membrane, pressure limit 12-35kg/m 2, 85 ℃ of temperature, flow velocity 50L/h, being concentrated into relative density is 1.15~1.20 (60 ℃), adds 8 times of water gagings, stirs, cold putting 12 hours filtered.Membrance concentration equipment on the filtrate adopts polyamide-based 6m 2Reverse osmosis membrane, pressure limit 12-35kg/m 2, 35 ℃ of temperature, flow velocity 50L/h, being concentrated into density is 1.15~1.25 (40 ℃), promptly.
Embodiment 10
Radix Astragali 20kg adds the water extraction twice of 5 times of amounts, and each 1 hour, merge extractive liquid,, last AB-8 macroporous adsorbent resin is used 25% alcohol flushing, collects ethanol stream fluid and water lotion.Last membrance concentration equipment adopts polysulfones 6m 2Reverse osmosis membrane, pressure 5-25kg/m 2, 20 ℃ of temperature, flow velocity 35L/h, being concentrated into relative density is 1.15~1.25 (60 ℃), and adding ethanol is 80% to containing the alcohol amount, filters, and precipitation is dry, pulverizes.
Embodiment 11
Radix Ginseng 10kg, Radix Ophiopogonis, 10kg, Fructus Schisandrae Chinensis 20kg added the water extraction 2 times of 6 times of amounts, and each 1.5 hours, merge extractive liquid,, 200 order filter clothes filter, and put and are chilled to room temperature.Last membrance concentration equipment adopts polysulfones 4m 2Reverse osmosis membrane, pressure 20-35kg/m 2, 30 ℃ of temperature, flow velocity 50L/h, being concentrated into relative density is 1.10~1.15 (60 ℃), and adding ethanol is 70% to containing the alcohol amount, filters, and supernatant is evaporated to density 1.20~1.25, and drying is pulverized.
Embodiment 12
Rhizoma Coptidis 10kg adds the 1-5% hydrochloric acid solution of 8 times of amounts, extracts 2 times, and merge extractive liquid,, 200 order filter clothes filter, and put and are chilled to room temperature.Last membrance concentration equipment adopts polyamide-based 6m 2Reverse osmosis membrane, pressure 10-40kg/m 2, 25 ℃ of temperature, flow velocity 70L/h, being concentrated into relative density is 1.15~1.20 (60 ℃), and adding ethanol is 80% to containing the alcohol amount, filters, and precipitation is dry, pulverizes.
Embodiment 13
Herba Andrographis 15kg, add 6 times of amount 80~85% ethanol, extract each 1 hour 3 times, merge extractive liquid,, be evaporated to and contain alcohol amount and be lower than 25%, filter AB-8 type macroporous adsorbent resin on the filtrate, 6 times of amounts of 30% ethanol eluting, collect eluent,, collect effluent with the ultrafiltration apparatus filtration of the molecular weight 5000 that dams.Last polysulfones 4m 2Reverse osmosis membrane, pressure 20-50kg/m 2, 35 ℃ of temperature, flow velocity 40L/h, being concentrated into relative density is 1.15~1.20 (60 ℃), is drying to obtain.
Embodiment 14
Radix Astragali 20kg adds 6 times of water gagings and extracts 2 times, and each 1 hour, merge extractive liquid,, 200 order filter clothes filter, and put and are chilled to room temperature.Last membrance concentration equipment adopts aluminium oxide, zirconium oxide polymer 2m 2Reverse osmosis membrane, pressure 10-40kg/m 2, 50 ℃ of temperature, flow velocity 70L/h, being concentrated into relative density is 1.06~1.25 (60 ℃), promptly gets concentrate.
Embodiment 15
Radix Salviae Miltiorrhizae 40kg, Radix Notoginseng 20kg adds 6 times of water gagings and extracts twice, and each 2 hours, merge extractive liquid,, 200 order filter clothes filter, and put and are chilled to room temperature.Last reverse osmosis membrane concentrator adopts polyamide-based 6m 2Reverse osmosis membrane, pressure 30-50kg/m 2, 40 ℃ of temperature, flow velocity 75L/h, being concentrated into relative density is 1.06~1.20 (40 ℃), promptly gets concentrate.

Claims (10)

1, a kind of Chinese medicine concentrate is characterized in that, it is made through reverse osmosis membrane technology is concentrated by the water extract of this Chinese medicine.
2, the described Chinese medicine concentrate of claim 1, it is characterized in that described Chinese traditional medicine water extract carries out the solution that obtains after conventional the extraction or other organic solvents that contain of obtaining through processing after to Chinese medicine extraction with solvent are lower than 30% aqueous solution for being solvent with water to Chinese medicine.
3, the described Chinese medicine concentrate of the arbitrary claim of claim 1~2, it is characterized in that described reverse osmosis membrane is selected from following kind: cellulose, polyamide, polyphenyl Methanamide, aromatic heterocycle, polysulfones, polyether sulfone, TPO, silicone rubber, fluoro containing polymers, pottery, inorganic polymer.
4, the described Chinese medicine concentrate of the arbitrary claim of claim 1~2 is characterized in that, pressure is 5~80kg/m in the described concentration process 2, temperature is 10~100 ℃, flow rate of liquid is 10~100L/h.
5, the described Chinese medicine concentrate of claim 4 is characterized in that, pressure is 10~80kg/m in the described concentration process 2, temperature is 10~80 ℃, flow rate of liquid is 20~80L/h.
6, the described Chinese medicine concentrate of claim 5 is characterized in that, pressure is 10~60kg/m in the described concentration process 2, temperature is 10~60 ℃, flow rate of liquid is 30~60L/h.
7, the described Chinese medicine concentrate of claim 6 is characterized in that, pressure is 10~40kg/m in the described concentration process 2, temperature is 20~35 ℃, flow rate of liquid is 40~50L/h.
8, the preparation method of the concentrate of Chinese medicine described in the claim 1 is characterized in that, may further comprise the steps:
The I Chinese crude drug extracts with The suitable solvent;
The II extracting solution merges, and puts cold solution to be concentrated, or the preliminary remove impurity of merge extractive liquid, is got solution to be concentrated, or goes up macroporous adsorbent resin and get solution to be concentrated;
III concentrates solution to be concentrated by reverse osmosis membrane, get concentrate;
Wherein the solvent described in the step I is organic solvent or water or water and the mixing of organic solvent;
Macroporous adsorbent resin described in the Step II is selected from D101, H103, D3520, D4006, D4020, D14, D16, AB-8, SA-1, X-5, HPD100, HPD400 etc.;
Reverse osmosis membrane is selected from following kind among the Step II I: cellulose, polyamide, polyphenyl Methanamide, aromatic heterocycle, polysulfones, polyether sulfone, TPO, silicone rubber, fluoro containing polymers, pottery, inorganic polymer; Pressure is 5~80kg/m in the described concentration process 2, temperature is 10~100 ℃, flow rate of liquid is 10~100L/h.
9, the preparation method of the Chinese medicine concentrate described in the claim 8 is characterized in that, reverse osmosis membrane is selected from following kind among the described Step II I: cellulose, polyamide, polyphenyl Methanamide, polysulfones, fluoro containing polymers, pottery, inorganic polymer class; Pressure is 10~80kg/m in the described concentration process 2, temperature is 10~80 ℃, flow rate of liquid is 20~80L/h.
10, the preparation method of the Chinese medicine concentrate described in the claim 8 is characterized in that, reverse osmosis membrane is selected from following kind among the described Step II I: polyamide, polysulfones, inorganic polymer, ceramic-like; Pressure is 10~40kg/m in the described concentration process 2, temperature is 20~35 ℃, flow rate of liquid is 40~50L/h.
CN 200510015123 2005-09-20 2005-09-20 Chinese medicine concentrate andits preparing method Pending CN1935162A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102068468A (en) * 2009-12-31 2011-05-25 成都科尔医药技术有限公司 Method for treating traditional Chinese medicinal extraction solution before preparation
CN103182247A (en) * 2012-12-18 2013-07-03 神威药业集团有限公司 Method for improving safety of traditional Chinese medicine injection

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102068468A (en) * 2009-12-31 2011-05-25 成都科尔医药技术有限公司 Method for treating traditional Chinese medicinal extraction solution before preparation
CN103182247A (en) * 2012-12-18 2013-07-03 神威药业集团有限公司 Method for improving safety of traditional Chinese medicine injection

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Application publication date: 20070328