CN1857642A - Quality control method for depression relieving and tranquilizing preparation - Google Patents
Quality control method for depression relieving and tranquilizing preparation Download PDFInfo
- Publication number
- CN1857642A CN1857642A CN 200610065647 CN200610065647A CN1857642A CN 1857642 A CN1857642 A CN 1857642A CN 200610065647 CN200610065647 CN 200610065647 CN 200610065647 A CN200610065647 A CN 200610065647A CN 1857642 A CN1857642 A CN 1857642A
- Authority
- CN
- China
- Prior art keywords
- solution
- water
- preparation
- reference substance
- jasminoidin
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Landscapes
- Medicines Containing Plant Substances (AREA)
- Medicinal Preparation (AREA)
Abstract
The present invention relates to quality control method for depression relieving and tranquilizing preparation. The quality control method includes thin layer chromatography process for material identification and spectrophotometric method for content measurement. The quality control method is precise, sensitive and stable, and can ensure the high and stable product quality.
Description
Technical field:
The present invention relates to the method for quality control of a kind of method of quality control of Chinese medicine preparation, particularly depression relieving and tranquilizing preparation.
Background technology:
The resolving stagnation for tranquilization electuary is listed the 4th the 208th page in the Sanitation Ministry medicine standard Chinese traditional patent formulation preparation in, be granule, the resolving stagnation for tranquilization electuary is selected not impairing the liver kidney for use in medication, to the high-quality rare Chinese medicine that the adjustment repairing and the tranquilizing the mind resolving depression of conscience kidney are excluded the difficulty and anxiety, contained brain function regulatory factor and NAOQING are removed the factor, energy two-ways regulation human central nervous system, improve and regulate brain excitement and suppress balance, improve oxygen-supplying amount, eliminate the brain anxiety, the people is gone to sleep peacefully.This electuary is the pure Chinese medicine that China develops symptoms such as insomnia, depression first, and treatment is directly started with from nervous system, reaches " treating both the principal and secondary aspects of a disease ".It sells well with the significant curative effect of uniqueness, gains national fame.This medicine drug effect is powerful, lasting, with strong points, and took effect the same day of taking medicine, and is rapidly sleeping.Cure mainly: intractable insomnia, anxiety, depression, vexed, neurasthenia, chest distress and palpitation symptoms, neurosis, dizzy headache, climacteric syndrome etc.Insomnia is called " being insomnia ", " unable to close the eyes ", " must not crouch ", " insomnia " again, and it is the internal organs disorders, deficiency of qi and blood, imbalance of YIN and YANG, and cause obtaining ortho sleep, be clinical in common disease.In the last few years, because rhythm of life is accelerated, operating pressure increased, dog-eat-dog, and the inter personal contact complexity, people's psychological burden increases the weight of, and therefore the sickness rate of insomnia also rises to some extent, and has become a kind of ciril disease in the modern society.Apoplexy retarded depression disease belongs to the melancholia category in Chinese medicine.Melancholia is because feelings will is not relaxed, the caused class disease of depression and stagnation of QI, finally causes the liver failing to maintain the normal flow of QI, and spleen loses fortuneization, and the mind is not normal, and the internal organs yin and yang qi and blood disorder forms.The first cause of disease stagnation of QI and hold damp-phlegm, food stagnation, heat stagnation person under the arm, how true card; Prolonged illness is by gas and blood, and Sthenia is transforming into asthenia, as for a long time strongly fragrantly overtax one's nerves, heart spleen all loses, hyperactivity of fire caused by deficiency of YIN etc. all belongs to deficiency syndrome.Melancholia patient's the rule of treatment is the mediation mechanism of qi, the resolving depression of calming the nerves, this is for the development that prevents the state of an illness, become sick it, significant.During clinical treatment, shrewd deficiency and excess.Excess syndrome is controlled with relieving depressed liver and clearing heat, the resolving depression of calming the nerves; Deficiency syndrome control with QI invigorating and in, the resolving depression of calming the nerves.Treatment should be taken specimen into account, can help the method with strengthening spleen, tonifying kidney, the logical stasis of blood of invigorating blood circulation.Medicinal Radix Bupleuri, Radix Curcumae depressed liver-energy dispersing and QI regulating, Poria the spleen strengthening and damp drying, the Radix Angelicae Sinensis logical stasis of blood of invigorating blood circulation, Semen Platycladi, Radix Polygalae, Semen Ziziphi Spinosae (parched) tranquilizing by nourishing the heart, the Radix Astragali, Radix Codonopsis, Fructus Lycii, Radix Rehmanniae Preparata, Fructus Corni are tonified Qi of the kidney, nourishing blood to tranquillize the mind.Reach the wholistic therapy purpose of giving consideration to both the incidental and fundamental by determination of treatment based on pathogenesis obtained through differentiation of symptoms and signs flexibly.
The resolving stagnation for tranquilization syrup is to develop through form improvement on the basis of former electuary dosage form, and existing depression relieving and tranquilizing preparation exists method of quality control to fall behind the uppity shortcoming of product quality.Its composition is not differentiated in the existing method of quality control, or its composition is carried out the content of assay.So existing method of quality control can not effectively be controlled the quality of depression relieving and tranquilizing preparation, thereby will influence the production of product and ensure the quality of products.
For effectively controlling product quality, we have set up the new method of quality control of depression relieving and tranquilizing preparation, and this method adopts thin layer chromatography to differentiate, adopt spectrophotography to carry out assay.This method of quality control precision, sensitivity, stability are all good, guarantee " safety, the homogeneous, stable, effective, controlled " of product quality.
Summary of the invention:
The object of the invention is to provide the method for quality control of depression relieving and tranquilizing preparation.
The depression relieving and tranquilizing preparation prescription consists of:
Radix Bupleuri 40g Fructus Jujubae 30g Rhizoma Acori Graminei 40g
The Rhizoma Pinelliae (processed) 30g Rhizoma Atractylodis Macrocephalae (stir-fry) 30g Fructus Tritici Levis 100g
Radix Polygalae (system) 40g Radix Glycyrrhizae (processing) 30g Fructus Gardeniae (stir-fry) 40g
Bulbus Lilii 100g Arisaema Cum Bile 40g Radix Curcumae 40g
Dens Draconis 100g Semen Ziziphi Spinosae (stir-fry) 50g Poria 50g
Radix Angelicae Sinensis 30g
Resolving stagnation for tranquilization syrup production technology
More than ten Six-elements, decoct with water three times, 3 hours for the first time, second and third time each 2 hours, collecting decoction filters, and filtrate is concentrated into the clear paste that relative density is about 1.06～1.08 (55 ℃～60 ℃), and adding sucrose 460g and potassium sorbate are an amount of, the dissolving back filters, and adds water to 1000ml, promptly.
The present invention be directed to the resolving stagnation for tranquilization syrup preparation and propose method of quality control, but also be not limited to the resolving stagnation for tranquilization syrup preparation, also can comprise other oral formulations of resolving stagnation for tranquilization such as tablet, capsule, pill, granule.
Its prescription of other dosage forms of the resolving stagnation for tranquilization that the present invention includes is identical with the resolving stagnation for tranquilization syrup preparation, and composition is by weight as proportioning, can increase or reduce according to corresponding proportion when producing, and be no more than 100% at most.
Large-scale production can be unit with the kilogram, or is unit with the ton.More than composition can be made into 1000 doses of pharmaceutical preparatioies, described 1000 doses of fingers, and the final drug preparation of making, as make 1000 of capsule preparations, and 1000 in tablet, granule 1000g, liquid preparation 1000ml etc.,
The preparation method of other dosage forms of resolving stagnation for tranquilization syrup of the present invention can adopt following method:
By the raw material of Chinese medicine of above-mentioned prescription is processed through extraction or other modes, making pharmaceutically active substance, subsequently, is raw material with this material, add the medicine acceptable carrier when needing, make capsule, tablet, syrup, granule according to the routine techniques of galenic pharmacy.Described active substance can obtain by the method that is selected from following mode, as: by pulverize, squeeze, calcine, grind, sieve, percolation, extraction, water are carried, alcohol extraction, ester are carried, methods such as ketone is carried, chromatography obtain, these active substances can be the materials of extractum form, can be that dry extract also can be a fluid extract, can also be the high-purity extract, make different concentration according to the different needs decision of preparation.
Other dosage forms of resolving stagnation for tranquilization of the present invention, when making preparation, can add the medicine acceptable carrier as required, these carriers can be any carriers that is fit to make preparation of the present invention, as: benzoic acid or potassium salt, mannitol, sorbitol, sorbic acid or potassium salt, xylitol, maltose, glucose, fructose, dextran, glycine, starch, sucrose, lactose, mannitol, Nepal's methyl ester, Nepal's ethyl ester, Nepal's propyl ester, Nepal's butyl ester, sodium pyrosulfite, sodium sulfite, sodium thiosulfate, cysteine hydrochloride, TGA, methionine, vitamin A, vitamin C, vitamin E, vitamin D, azone, the EDTA disodium, EDTA calcium sodium, the alkali-metal carbonate of monovalence, acetate, phosphate or its aqueous solution, hydrochloric acid, acetic acid, sulphuric acid, phosphoric acid, aminoacid, sodium chloride, potassium chloride, sodium lactate, silicon derivative, cellulose and derivant thereof, alginate, gelatin, polyvinylpyrrolidone, glycerol, propylene glycol, ethanol, soil temperature 60-80, Arlacel-80, Cera Flava, lanoline, liquid paraffin, hexadecanol, gallate ester, agar, triethanolamine, basic amino acid, carbamide, allantoin, surfactant, Polyethylene Glycol, cyclodextrin, beta-schardinger dextrin-, phospholipid material etc.
Depression relieving and tranquilizing preparation of the present invention, particularly resolving stagnation for tranquilization syrup preparation, it is as follows that its function cures mainly usage and dosage:
[function with cure mainly] soothing liver-QI for relieving depression, tranquilizing the mind.Be used for feelings will and do not relax, vexed, the anxiety due to the direct stimulations such as stagnation of QI due to depression of the liver, insomnia, forgetful, climacteric syndrome, neurosis etc.
[usage and consumption] is oral, a 10ml, 2 times on the one.
[specification] every bottle of 100ml.
Shady and cool place is put in [storage] sealing.
[effect duration] 2 years.
The present invention is to provide the method for quality control at above depression relieving and tranquilizing preparation, particularly the resolving stagnation for tranquilization syrup preparation is the quality of control depression relieving and tranquilizing preparation.At its characteristics and prescription of the present invention, we provide following method of quality control:
Method of quality control of the present invention may further comprise the steps:
The observation of character, the discriminating of content, the inspection of content is carried out assay to the composition that contains, and therefore, the main step of method of quality control of the present invention is:
The observation of character, step is:
[character] this product is brown to tan thick liquid; It is sweet to distinguish the flavor of.
The discriminating of content, step is:
This product 30ml is got in [discriminating] (1), uses extracted with diethyl ether 2 times, and each 15ml discards ether solution, water layer is with water-saturated n-butanol extraction 3 times, and each 15ml merges n-butyl alcohol liquid, with the ammonia solution washing of equivalent, divide and get n-butanol layer, evaporate to dryness, residue makes dissolving with 1ml methanol.Other gets Radix Bupleuri control medicinal material 2g, adds water 30ml and decocts 30min, filters, and filtrate is with water-saturated n-butanol extraction 3 times, and each 15ml below with the need testing solution preparation method, makes control medicinal material solution from " merging n-butyl alcohol liquid ... ".According to thin layer chromatography (" 2005 editions appendix VIB of Chinese pharmacopoeia) test, draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, the lower floor of transferring postpone with 10 ℃ in chloroform-methanol-water (65: 32: 10) is developing solvent, launches, and takes out, dry, spray is with 1% dimethylaminobenzaldehyde, 10% ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing in 105 ℃, puts under the ultra-violet lamp (365nm) and inspects.In the test sample chromatograph, with control medicinal material chromatograph relevant position on, show the fluorescence speckle of same color.
(2) get this product 40ml, use ethyl acetate extraction 2 times, each 20ml, combined ethyl acetate layer, evaporate to dryness, residue add 1ml methanol makes dissolving, as need testing solution.It is an amount of that other gets the jasminoidin reference substance, adds methanol and make the reference substance solution that every 1ml contains jasminoidin 1mg.According to thin layer chromatography (" 2005 editions appendix VIB of Chinese pharmacopoeia) test, draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with ethyl acetate-acetone-glacial acetic acid (3: 2: 1) is developing solvent, launches, and takes out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing in 105 ℃, puts under the ultra-violet lamp (254nm) and inspects.In the test sample chromatograph, with control medicinal material chromatograph relevant position on, show the fluorescence speckle of same color.
(3) get this product 40ml, use water saturation n-butanol extraction 2 times, each 30ml, merge n-butyl alcohol liquid, evaporate to dryness, residue add that water 2ml is ultrasonic to make dissolving, last D101 type macroporous resin column (internal diameter 1.5cm, the high 15cm of post), be washed till colourlessly with the flow velocity of 1ml/min water, 0.5% sodium hydroxide solution, 30% ethanol successively, discard eluent, reuse 70% ethanol 150ml eluting, collect eluent, evaporate to dryness, residue makes dissolving with 1ml methanol, as need testing solution.Other gets jujuboside A, the B reference substance is an amount of, adds methanol and makes the mixing reference substance solution that every 1ml contains 1mg.According to thin layer chromatography (" 2005 editions appendix VIB of Chinese pharmacopoeia) test, draw need testing solution 10 μ l, reference substance solution 5 μ l, put respectively on same silica gel g thin-layer plate, upper strata with n-butyl alcohol-glacial acetic acid-water (4: 1: 5) is developing solvent, launch, take out, dry, spray is inspected immediately with 1% vanillin sulfuric acid solution.In the test sample chromatograph, with control medicinal material chromatograph relevant position on, show the speckle of same color.
The inspection of content, step is:
[inspection] relative density should be not less than 1.08 (an appendix VII of Chinese Pharmacopoeia version in 2005 A).
PH value should be 4.0～5.5 (an appendix VII of Chinese Pharmacopoeia version in 2005 G).
Other should meet every regulation relevant under the syrup item (an appendix I of Chinese Pharmacopoeia version in 2005 H).
The composition that contains is carried out assay, and step is:
[assay] measured according to high performance liquid chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 D).
It is filler with octadecylsilane chemically bonded silica that chromatographic condition and system are suitable for test; Acetonitrile-0.02M potassium dihydrogen phosphate (13.5: 86.5) is a mobile phase; The detection wavelength is 238nm.Number of theoretical plate calculates by the jasminoidin peak should be not less than 2000.
The preparation precision of reference substance solution takes by weighing through 24 hours jasminoidin reference substance of phosphorus pentoxide drying under reduced pressure an amount of, and thin up behind the dissolve with methanol is made the solution that every 1ml contains 40 μ g, promptly.
The preparation precision of need testing solution is measured this product 5ml, places the 50ml measuring bottle, and thin up shakes up to scale, filters with microporous filter membrane (0.45 μ m), gets subsequent filtrate, promptly.
Accurate respectively reference substance solution and each the 20 μ l of need testing solution of drawing of algoscopy inject chromatograph of liquid, measure, promptly.
The every 1ml of this product contains Fructus Gardeniae with jasminoidin (C
17H
24O
10) meter, must not be less than 0.25mg.
The present invention changes agent on former dosage form basis, simultaneously production technology reformed,
This determines that factor adopts single factor experiment method to investigate to amount of water, and promptly by the extraction time and the extraction time of primary standard technology, amount of water is selected four levels, i.e. 6,8,10,12 water yields extraordinarily.
2. the selection of evaluation index
1. the rate of transform of selecting jasminoidin in the medical material is as evaluation index.
2. paste-forming rate is a medicine day dosing, and so the foundation that single oral dose and packing specification are determined is with its another evaluation index as extraction process.
3. experimental technique: take by weighing the above-mentioned medical material of recipe quantity, get three parts altogether,, do following 3 technologies:
Technology one: extracting in water three times, 3 hours for the first time, add 12 times of water gagings, 2 hours for the second time, add 10 times of water gagings, 2 hours for the third time, add 8 times of water gagings, merge extractive liquid, filters, and filtrate decompression is concentrated into dried cream.
Technology two: extracting in water three times, 3 hours for the first time, add 10 times of water gagings, 2 hours for the second time, add 8 times of water gagings, 2 hours for the third time, add 8 times of water gagings, merge extractive liquid, filters, and filtrate decompression is concentrated into dried cream.
Technology three: extracting in water three times, 3 hours for the first time, add 8 times of water gagings, 2 hours for the second time, add 8 times of water gagings, 2 hours for the third time, add 6 times of water gagings, merge extractive liquid, filters, and filtrate decompression is concentrated into dried cream.
4 jasminoidin assays
Under No. 15 data items of resolving stagnation for tranquilization syrup, the jasminoidin assay.
It is filler with octadecylsilane chemically bonded silica that chromatographic condition and system are suitable for test; Acetonitrile-0.02M potassium dihydrogen phosphate (13.5: 86.5) is a mobile phase; The detection wavelength is 238nm.Number of theoretical plate calculates by the jasminoidin peak should be not less than 3000.
The preparation precision of reference substance solution takes by weighing through 24 hours jasminoidin reference substance of phosphorus pentoxide drying under reduced pressure an amount of, and thin up behind the dissolve with methanol is made the solution that every 1ml contains 40 μ g, promptly.
The preparation precision of need testing solution is measured in this product 5ml to 50ml measuring bottle, and thin up shakes up to scale, filters with microporous filter membrane (0.45 μ m), gets subsequent filtrate, promptly.
Accurate respectively reference substance solution and each the 20 μ l of need testing solution of drawing of algoscopy inject chromatograph of liquid, measure, promptly.
5. experimental result
Table 1 amount of water is investigated result of the test
| Crude drug amount (g) | Amount of water (doubly) | Dried cream amount (g) | Dried cream rate (%) | The jasminoidin rate of transform (%) |
| 790 790 790 | 12/10/8 10/8/8 8/8/6 | 127.4 126.9 126.4 | 16.13 16.06 16.00 | 46.85 46.79 46.82 |
The result shows that different amount of water are to the no significant difference that influences of jasminoidin content.Therefore for reducing energy loss, reduce production costs, determine the medical material extracting in water three times, 3 hours for the first time, add 8 times of water gagings, 2 hours for the second time, add 8 times of water gagings, 2 hours for the third time, add 6 times of water gagings.
(4) selection of antiseptic kind and consumption
The selection of a kind: the pH value that records this product medicinal liquid is 4～5, with reference to pharmacy of Chinese materia medica and relevant document [11], preservative benzoic acid commonly used and sodium benzoate (pH value is 2.5～4.5) fungistatic effect under acid condition are better, and when pH surpassed 4.5, effect significantly descended.Sorbic acid and potassium sorbate are to be that 4.5 o'clock activity are the strongest at pH value, and sorbic acid is easily oxidized, and increase dissolubility with the content of sugar descend in syrup, so this product selects for use potassium sorbate to cook antiseptic, and its consumption are carried out screening test:
2, the selection of potassium sorbate consumption
With reference to " under 581 pages of potassium sorbate items of pharmaceutic adjuvant handbook, potassium sorbate is 0.14% to the escherichia coli minimum inhibitory concentration, is 0.014%～0.04% to the antibacterial minimum inhibitory concentration; To yeast, fungus minimum inhibitory concentration is 0.8%～1.2%.Under Chinese Pharmacopoeia version appendix in 2005 I rules of preparations item, the consumption of antiseptic sorbic acid must not surpass 0.3%, and therefore, the amount that adds potassium sorbate with reference to pertinent literature is 0.3%, show that through long-term and accelerated stability test result microbial limit is up to specification.Can well guarantee product quality so add 0.3% potassium sorbate.
(5) selection of correctives
This product bitter in the mouth needs to add suitable correctives to reach the purpose of improving mouthfeel.Therefore, consider in preparation, to add a small amount of correctives, to cover bitter taste.This product is a syrup, and sucrose is as a kind of sweeting agent, and flavoring is effective, be widely used in the industries such as food, medicine, therefore directly with sucrose as correctives.
(6), the syrup prescription determines
Resolving stagnation for tranquilization electuary prescription is:
Radix Bupleuri 40g Fructus Jujubae 30g Rhizoma Acori Graminei 40g
The Rhizoma Pinelliae (processed) 30g Rhizoma Atractylodis Macrocephalae (stir-fry) 30g Fructus Tritici Levis 100g
Radix Polygalae (system) 40g Radix Glycyrrhizae (processing) 30g Fructus Gardeniae (stir-fry) 40g
Bulbus Lilii 100g Arisaema Cum Bile 40g Radix Curcumae 40g
Dens Draconis 100g Semen Ziziphi Spinosae (stir-fry) 50g Poria 50g
Radix Angelicae Sinensis 30g
Make 500g (100 bags)
Each dose is 5g (being equivalent to crude drug 0.79g).According to the rate of extract this prescription being made syrupy amount is 1000ml, takes 10ml (being equivalent to crude drug 0.79g) at every turn, consistent with the electuary dose.Therefore the syrup prescription is defined as:
Radix Bupleuri 40g Fructus Jujubae 30g Rhizoma Acori Graminei 40g
The Rhizoma Pinelliae (processed) 30g Rhizoma Atractylodis Macrocephalae (stir-fry) 30g Fructus Tritici Levis 100g
Radix Polygalae (system) 40g Radix Glycyrrhizae (processing) 30g Fructus Gardeniae (stir-fry) 40g
Bulbus Lilii 100g Arisaema Cum Bile 40g Radix Curcumae 40g
Dens Draconis 100g Semen Ziziphi Spinosae (stir-fry) 50g Poria 50g
Radix Angelicae Sinensis 30g
Make 1000ml
Do not have in the former preparation quality standard and differentiate and the assay item that we study this product quality standard, set up Radix Bupleuri, Fructus Gardeniae, the thin layer discriminating of Semen Ziziphi Spinosae and the content assaying method of jasminoidin.
14.2.1 differentiate
14.2.1.1 differentiating the thin layer of Radix Bupleuri in (1) side of being differentiates
We serve as that Study on Identification is carried out in contrast with the Radix Bupleuri control medicinal material, make negative control simultaneously, and the result shows that negative control is not seen interference, in the test sample chromatograph, with contrast chromatograph corresponding position on, show the speckle of same color.So this discriminating is listed in this product quality standard.
14.2.1.2 differentiating the thin layer of Fructus Gardeniae in (2) side of being differentiates
We serve as that Study on Identification is carried out in contrast with the jasminoidin reference substance, make negative control simultaneously, and the result shows that negative control is not seen interference, in the test sample chromatograph, with contrast chromatograph corresponding position on, show the speckle of same color.So this discriminating is listed in this product quality standard.
14.2.1.3 differentiating the thin layer of Semen Ziziphi Spinosae in (3) side of being differentiates
We serve as that Study on Identification is carried out in contrast with jujuboside A, B reference substance, make negative control simultaneously, and the result shows: negative control is not seen interference, in the test sample chromatograph with contrast chromatograph corresponding position on, show the speckle of same color.So this discriminating is listed in this product quality standard.
14.2.1.4 other
14.2.1.4.1 the Study on Identification of the Rhizoma Atractylodis Macrocephalae
Once the method on the reference literature in the experiment, adopted multiple extraction solvents such as normal hexane to handle sample with different sample treatments, screened different developing solvents, but because this product technology is decocting and boils, therefore specific examples of such components is seldom in the sample, all do not occur and the corresponding speckle of control medicinal material in the gained test sample chromatograph, so we do not include this discriminating in this product quality standard in temporarily.
14.2.1.4.2 the Study on Identification of Fructus Jujubae
We are contrast with reference to the method on the pharmacopeia with the oleanolic acid reference substance in the experiment, adopt the extracted with diethyl ether sample to carry out the thin layer Study on Identification, as a result in the test sample chromatograph, with the corresponding position of reference substance chromatograph on speckle unintelligible, and feminine gender has interference, so exclude text.
14.2.1.4.3 the Study on Identification of Arisaema Cum Bile
Mainly containing compositions such as deoxycholic acid in the Arisaema Cum Bile, adopt the chloroform extraction sample in the test, is contrast with the deoxycholic acid, and the Arisaema Cum Bile in the sample is studied.As a result in the test sample chromatograph, with the corresponding position of reference substance chromatograph on speckle colour generation band shape, and feminine gender has interference, so exclude text.
14.2.2 check
14.2.2.1 relative density
Photograph checks that to densitometry (an appendix VII of Chinese Pharmacopoeia version in 2005 A) result is all up to specification.
14.2.2.2pH value
Check that according to pH value algoscopy (an appendix VII of Chinese Pharmacopoeia version in 2005 G) result is all up to specification.
14.2.2.3 heavy metal
Checked 3 batch samples by heavy metal inspection technique (2005 editions one appendix IX E of Chinese Pharmacopoeia, second method), the result all surpasses 10/1000000ths, so quality standard is not included in an inspection temporarily in.
14.2.2.4 arsenic salt
Checked 3 batch samples according to arsenic salt inspection technique (2005 editions one appendix IX F of Chinese Pharmacopoeia, second method), the result all surpasses 2/1000000ths, so quality standard is not included in an inspection temporarily in.
14.2.2.5 limit test of microbe
Press 2005 editions one appendix XIII C of Chinese Pharmacopoeia " microbial limit standard " regulation, the oral Preparation bacterial population that does not contain the former powder of medical material must not be crossed 100/ml, and mycete and yeast count must not be crossed 100/ml, and escherichia coli must not detect.Several batches of testing results of this preparation are all up to specification.
14.2.2.5 loading amount
Check that by minimum fill inspection technique (2005 editions one appendix XII C of Chinese Pharmacopoeia) result is all up to specification.
14.2.3 assay
The resolving stagnation for tranquilization syrup is made by medical materials such as Radix Bupleuri, Fructus Gardeniae, Semen Ziziphi Spinosae, the Rhizoma Atractylodis Macrocephalae, Fructus Jujubae, Arisaema Cum Bile, Radix Angelicae Sinensis, jasminoidin is the main component in the Fructus Gardeniae, can be as quality control index, the content that adopts the high effective liquid chromatography for measuring jasminoidin is with the control end product quality.Investigate through methodology, this method is accurately feasible.
14.2.3.1 instrument and reagent
Instrument: high performance liquid chromatograph Agilent 1100 types, Luna C-18 analytical column (4.6 * 250mm, 5 μ m), 1cm C18 pre-column.
Reagent: methanol is chromatographically pure, and other reagent are analytical pure, and water is ultra-pure water.
Reference substance: jasminoidin reference substance (assay with) Nat'l Pharmaceutical ﹠ Biological Products Control Institute provides lot number 110749-200410.
Resolving stagnation for tranquilization syrup: Jiangxi Huiren Pharmaceutical Co., Ltd's self-control
Research lot number: 20040704,20040705,20040706
14.2.3.2 method and result
14.2.3.2.1 chromatographiccondition
Immobile phase: octadecylsilane chemically bonded silica
Mobile phase: acetonitrile-0.02M potassium dihydrogen phosphate (13.5: 86.5)
Detect wavelength: 238nm; Flow velocity: 1.00ml/min; Column temperature: 25 ℃
14.2.3.2.2 system suitability test
In the above conditions, the adjacent component with other of jasminoidin all can reach baseline separation, and separating degree meets the requirements, and number of theoretical plate calculates by the jasminoidin peak and is not less than 3000.And the negative control of scarce Fructus Gardeniae does not have absworption peak (seeing accompanying drawing) under identical retention time, illustrate with this condition feasible.
14.2.3.2.3 test method
14.2.3.2.3.1 the preparation of reference substance solution: precision takes by weighing through 24 hours jasminoidin reference substance of phosphorus pentoxide drying under reduced pressure an amount of, and thin up behind the dissolve with methanol is made the solution that every 1ml contains 40 μ g, promptly.
14.2.3.2.3.2 the preparation of need testing solution: precision is measured in this product 5ml to 50ml measuring bottle, and thin up shakes up to scale, filters with microporous filter membrane (0.45 μ m), gets subsequent filtrate, promptly.
14.2.3.2.3.3 assay method: accurate respectively reference substance solution and each 20 μ l of need testing solution of drawing, inject chromatograph of liquid.
14.2.3.2.3.4 the preparation of negative sample: press the negative sample that the preparation of resolving stagnation for tranquilization syrup preparation method lacks Fructus Gardeniae, prepare negative sample solution by the need testing solution preparation method.
14.2.3.2.4 the investigation of linear relationship
Precision takes by weighing the about 10mg of jasminoidin reference substance, puts in the 50ml measuring bottle, adds dissolve with methanol and is diluted to scale, shakes up.A certain amount of this solution of accurate absorption is mixed with concentration successively and is about 10 μ g/ml, 20 μ g/ml, 30 μ g/ml, 40 μ g/ml, the serial reference substance solution of 50 μ g/ml.The accurate respectively 20 μ l of absorption inject high performance liquid chromatograph, measure peak area.With the peak area is vertical coordinate, with reference substance concentration is abscissa drawing standard curve, the result shows that jasminoidin has good linear relationship in 10.02 μ g/ml～50.10 μ g/ml concentration ranges, regression equation is Y=29.396X-0.3788, r=1, wherein Y is a peak area, and X is jasminoidin concentration (μ g/ml), and r is a correlation coefficient.
Table 4 linear relationship is investigated
| The concentration of reference substance (μ g/ml) | Peak area |
| 10.02 20.04 30.06 40.08 50.10 | 394.36405 588.74305 883.05374 1177.38702 1742.78406 |
14.2.3.2.5 precision test
Precision is measured reference substance solution 20 μ l, and continuous sample introduction 6 times calculates the relative standard deviation (RSD) of peak area, the results are shown in Table 5 and accompanying drawing.
The test of table 5 reference substance solution precision
| The sample introduction number of times | Peak area | Meansigma methods | RSD(％) |
| 1 2 3 4 5 6 | 1183.38733 1183.09045 1181.68433 1183.85913 1184.16699 1182.77563 | 1183.16064 | 0.07 |
The result shows: method precision is good, and the relative standard deviation of the peak area of jasminoidin is 0.07% in the reference substance solution.
14.2.3.2.6 the stability test of sample solution
Get test sample (lot number: 20040704) solution, at different time sample introduction 20 μ l respectively, calculate the RSD of peak area.
Table 6 need testing solution stability
| Time (hour) | Peak area | Meansigma methods | RSD(％) |
| 0 2 6 12 18 24 | 622950 622867 622457 622999 626311 622850 | 623406 | 0.23 |
The result shows that need testing solution is stable in 24 hours.
14.2.3.2.7 repeatability test
Precision take by weighing test sample (lot number: 20040704) five parts, press the content of method replication jasminoidin under the assay item, calculating mean value and RSD the results are shown in Table 7 and accompanying drawing.
The test of table 7 repeatability
| Number of times | Sampling amount (ml) | Peak area | Content (mg/ml) | Meansigma methods (mg/ml) | RSD(％) |
| 1 | 5 | 1205.8 | 0.408 | 0.407 | 0.51 |
| 2 3 4 5 | 5 5 5 5 | 1201.3 1211.3 1197.3 1196.6 | 0.407 0.410 0.405 0.405 |
The result shows that with the content of jasminoidin in the method working sample under [assay] item, repeatability is good.
14.2.3.2.8 average recovery
Precision is measured the resolving stagnation for tranquilization syrup (lot number: 20040704) 2.5ml of six parts of known content, add 1.0ml jasminoidin reference substance solution (1.006mg/ml) respectively, according to the content of jasminoidin in the method working sample under [assay], calculate recovery rate the results are shown in Table 8 and accompanying drawing.
Computing formula: the response rate=(content in measured value-sample)/standard addition * 100%
The test of table 8 average recovery
| Sampling amount (ml) | Content in the sample (mg) | Reference substance addition (mg) | Measured value (mg) | The response rate (%) | Average recovery rate (%) | RSD (％) |
| 2.5 2.5 2.5 2.5 2.5 2.5 | 1.018 1.018 1.018 1.018 1.018 1.018 | 1.006 1.006 1.006 1.006 1.006 1.006 | 2.026 2.024 2.022 2.055 2.054 2.024 | 99.86 99.99 100.19 97.01 97.13 100.03 | 99.03 | 1.54 |
The result shows: the average average recovery of jasminoidin is 99.03%, and RSD% is 1.54, and average recovery meets the requirements.
14.2.3.2.9 10 batches of resolving stagnation for tranquilization syrup sample sizes are measured
By the method under [assay] item 10 batches of resolving stagnation for tranquilization syrup samples are detected result such as following table:
Table 9 10 batch sample assay results
| Lot number | Content (mg/ml) | Meansigma methods (mg/ml) | |
| 20040704 20040705 20040706 | 0.408 0.408 0.407 | 0.407 0.407 0.406 | 0.408 0.408 0.407 |
| 20040707 20040708 20040709 20040710 20051211 20051212 20051213 | 0.429 0.431 0.429 0.408 0.433 0.434 0.408 | 0.420 0.433 0.431 0.407 0.433 0.436 0.406 | 0.425 0.432 0.430 0.408 0.433 0.435 0.407 |
14.2.3.2.10 the formulation of content limit: 10 batches of product jasminoidin assay meansigma methodss are 0.42mg/ml.By the rate of transform in the jasminoidin content limit of the Fructus Gardeniae medical material of a regulation of version pharmacopeia in 2005 and the 10 batches of pilot scales, calculate to such an extent that content is about 0.32mg/ml, consider big from now on production, be 0.25mg/ml by 8 foldings with content limit is tentative.
More than this product described in the method for quality control of the present invention, be meant resolving stagnation for tranquilization syrup preparation according to prepared of the present invention, when other dosage forms are measured, refer to corresponding other dosage forms.
The invention has the advantages that: method of quality control of the present invention has guaranteed that the quality inspection standard of preparation of the present invention can be than the qualitative character of effectively controlling preparation comprehensively, have accuracy and advance, can be used as the effective technology means of the stability of quality control and investigation technology.Be of great importance to improving the quality of products.
The specific embodiment:
Further specify the present invention by the following examples, but not as limitation of the present invention.
The quality control of embodiment 1 resolving stagnation for tranquilization syrup preparation
The observation of character, step is:
[character] this product is brown to tan thick liquid; It is sweet to distinguish the flavor of.
The discriminating of content, step is:
This product 30ml is got in [discriminating] (1), uses extracted with diethyl ether 2 times, and each 15ml discards ether solution, water layer is with water-saturated n-butanol extraction 3 times, and each 15ml merges n-butyl alcohol liquid, with the ammonia solution washing of equivalent, divide and get n-butanol layer, evaporate to dryness, residue makes dissolving with 1ml methanol.Other gets Radix Bupleuri control medicinal material 2g, adds water 30ml and decocts 30min, filters, and filtrate is with water-saturated n-butanol extraction 3 times, and each 15ml below with the need testing solution preparation method, makes control medicinal material solution from " merging n-butyl alcohol liquid ... ".According to thin layer chromatography (" 2005 editions appendix VIB of Chinese pharmacopoeia) test, draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, the lower floor of transferring postpone with 10 ℃ in chloroform-methanol-water (65: 32: 10) is developing solvent, launches, and takes out, dry, spray is with 1% dimethylaminobenzaldehyde, 10% ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing in 105 ℃, puts under the ultra-violet lamp (365nm) and inspects.In the test sample chromatograph, with control medicinal material chromatograph relevant position on, show the fluorescence speckle of same color.
(2) get this product 40ml, use ethyl acetate extraction 2 times, each 20ml, combined ethyl acetate layer, evaporate to dryness, residue add 1ml methanol makes dissolving, as need testing solution.It is an amount of that other gets the jasminoidin reference substance, adds methanol and make the reference substance solution that every 1ml contains jasminoidin 1mg.According to thin layer chromatography (" 2005 editions appendix VIB of Chinese pharmacopoeia) test, draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with ethyl acetate-acetone-glacial acetic acid (3: 2: 1) is developing solvent, launches, and takes out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing in 105 ℃, puts under the ultra-violet lamp (254nm) and inspects.In the test sample chromatograph, with control medicinal material chromatograph relevant position on, show the fluorescence speckle of same color.
(3) get this product 40ml, use water saturation n-butanol extraction 2 times, each 30ml, merge n-butyl alcohol liquid, evaporate to dryness, residue add that water 2ml is ultrasonic to make dissolving, last D101 type macroporous resin column (internal diameter 1.5cm, the high 15cm of post), be washed till colourlessly with the flow velocity of 1ml/min water, 0.5% sodium hydroxide solution, 30% ethanol successively, discard eluent, reuse 70% ethanol 150ml eluting, collect eluent, evaporate to dryness, residue makes dissolving with 1ml methanol, as need testing solution.Other gets jujuboside A, the B reference substance is an amount of, adds methanol and makes the mixing reference substance solution that every 1ml contains 1mg.According to thin layer chromatography (" 2005 editions appendix VIB of Chinese pharmacopoeia) test, draw need testing solution 10 μ l, reference substance solution 5 μ l, put respectively on same silica gel g thin-layer plate, upper strata with n-butyl alcohol-glacial acetic acid-water (4: 1: 5) is developing solvent, launch, take out, dry, spray is inspected immediately with 1% vanillin sulfuric acid solution.In the test sample chromatograph, with control medicinal material chromatograph relevant position on, show the speckle of same color.
The inspection of content, step is:
[inspection] relative density should be not less than 1.08 (an appendix VII of Chinese Pharmacopoeia version in 2005 A).
PH value should be 4.0～5.5 (an appendix VII of Chinese Pharmacopoeia version in 2005 G).
Other should meet every regulation relevant under the syrup item (an appendix I of Chinese Pharmacopoeia version in 2005 H).
The composition that contains is carried out assay, and step is:
[assay] measured according to high performance liquid chromatography (appendix VID of Chinese Pharmacopoeia version in 2005).
It is filler with octadecylsilane chemically bonded silica that chromatographic condition and system are suitable for test; Acetonitrile-0.02M potassium dihydrogen phosphate (13.5: 86.5) is a mobile phase; The detection wavelength is 238nm.Number of theoretical plate calculates by the jasminoidin peak should be not less than 2000.
The preparation precision of reference substance solution takes by weighing through 24 hours jasminoidin reference substance of phosphorus pentoxide drying under reduced pressure an amount of, and thin up behind the dissolve with methanol is made the solution that every 1ml contains 40 μ g, promptly.
The preparation precision of need testing solution is measured this product 5ml, places the 50ml measuring bottle, and thin up shakes up to scale, filters with microporous filter membrane (0.45 μ m), gets subsequent filtrate, promptly.
Accurate respectively reference substance solution and each the 20 μ l of need testing solution of drawing of algoscopy inject chromatograph of liquid, measure, promptly.
The every 1ml of this product contains Fructus Gardeniae with jasminoidin (C
17H
24O
10) meter, must not be less than 0.25mg.
The preparation of embodiment 2 resolving stagnation for tranquilization syrup preparations
Radix Bupleuri 40g Fructus Jujubae 30g Rhizoma Acori Graminei 40g
The Rhizoma Pinelliae (processed) 30g Rhizoma Atractylodis Macrocephalae (stir-fry) 30g Fructus Tritici Levis 100g
Radix Polygalae (system) 40g Radix Glycyrrhizae (processing) 30g Fructus Gardeniae (stir-fry) 40g
Bulbus Lilii 100g Arisaema Cum Bile 40g Radix Curcumae 40g
Dens Draconis 100g Semen Ziziphi Spinosae (stir-fry) 50g Poria 50g
Radix Angelicae Sinensis 30g
Resolving stagnation for tranquilization syrup production technology
More than ten Six-elements, decoct with water three times, 3 hours for the first time, second and third time each 2 hours, collecting decoction filters, and filtrate is concentrated into the clear paste that relative density is about 1.06～1.08 (55 ℃～60 ℃), and adding sucrose 460g and potassium sorbate are an amount of, the dissolving back filters, and adds water to 1000ml, promptly.
Claims (8)
1, a kind of method of quality control of depression relieving and tranquilizing preparation is characterized in that, comprises the observation of character, the discriminating of content, and the step of assay is carried out in the inspection of content to the composition that contains.
2, the method for claim 1 is characterized in that, described depression relieving and tranquilizing preparation is an oral formulations.
3, the method for claim 2 is characterized in that, described oral formulations is the resolving stagnation for tranquilization syrup.
4, the method for claim 3 is characterized in that, described method step is as follows:
The observation of character, step is:
[character] this product is brown to tan thick liquid; It is sweet to distinguish the flavor of;
The discriminating of content, step is:
This product 30ml is got in [discriminating] (1), uses extracted with diethyl ether 2 times, and each 15ml discards ether solution, water layer is with water-saturated n-butanol extraction 3 times, and each 15ml merges n-butyl alcohol liquid, with the ammonia solution washing of equivalent, divide and get n-butanol layer, evaporate to dryness, residue makes dissolving with 1ml methanol; Other gets Radix Bupleuri control medicinal material 2g, adds water 30ml and decocts 30min, filters, and filtrate is with water-saturated n-butanol extraction 3 times, and each 15ml below with the need testing solution preparation method, makes control medicinal material solution from " merging n-butyl alcohol liquid ... "; According to thin layer chromatography (" 2005 editions appendix VIB of Chinese pharmacopoeia) test, draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, the lower floor of transferring postpone with 10 ℃ in chloroform-methanol-water (65: 32: 10) is developing solvent, launches, and takes out, dry, spray is with 1% dimethylaminobenzaldehyde, 10% ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing in 105 ℃, puts under the ultra-violet lamp (365nm) and inspects; In the test sample chromatograph, with control medicinal material chromatograph relevant position on, show the fluorescence speckle of same color;
(2) get this product 40ml, use ethyl acetate extraction 2 times, each 20ml, combined ethyl acetate layer, evaporate to dryness, residue add 1ml methanol makes dissolving, as need testing solution; It is an amount of that other gets the jasminoidin reference substance, adds methanol and make the reference substance solution that every 1ml contains jasminoidin 1mg; According to thin layer chromatography (" 2005 editions appendix VIB of Chinese pharmacopoeia) test, draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with ethyl acetate-acetone-glacial acetic acid (3: 2: 1) is developing solvent, launches, and takes out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing in 105 ℃, puts under the ultra-violet lamp (254nm) and inspects; In the test sample chromatograph, with control medicinal material chromatograph relevant position on, show the fluorescence speckle of same color;
(3) get this product 40ml, use water saturation n-butanol extraction 2 times, each 30ml, merge n-butyl alcohol liquid, evaporate to dryness, residue add that water 2ml is ultrasonic to make dissolving, last D101 type macroporous resin column (internal diameter 1.5cm, the high 15cm of post), be washed till colourlessly with the flow velocity of 1ml/min water, 0.5% sodium hydroxide solution, 30% ethanol successively, discard eluent, reuse 70% ethanol 150ml eluting, collect eluent, evaporate to dryness, residue makes dissolving with 1ml methanol, as need testing solution; Other gets jujuboside A, the B reference substance is an amount of, adds methanol and makes the mixing reference substance solution that every 1ml contains 1mg; According to thin layer chromatography (" 2005 editions appendix VIB of Chinese pharmacopoeia) test, draw need testing solution 10 μ l, reference substance solution 5 μ l, put respectively on same silica gel g thin-layer plate, upper strata with n-butyl alcohol-glacial acetic acid-water (4: 1: 5) is developing solvent, launch, take out, dry, spray is inspected immediately with 1% vanillin sulfuric acid solution; In the test sample chromatograph, with control medicinal material chromatograph relevant position on, show the speckle of same color;
The inspection of content, step is:
[inspection] relative density should be not less than 1.08 (an appendix VII of Chinese Pharmacopoeia version in 2005 A);
PH value should be 4.0～5.5 (an appendix VII of Chinese Pharmacopoeia version in 2005 G);
Other should meet every regulation relevant under the syrup item (appendix IH of Chinese Pharmacopoeia version in 2005);
The composition that contains is carried out assay, and step is:
[assay] measured according to high performance liquid chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 D);
It is filler with octadecylsilane chemically bonded silica that chromatographic condition and system are suitable for test; Acetonitrile-0.02M potassium dihydrogen phosphate (13.5: 86.5) is a mobile phase; The detection wavelength is 238nm; Number of theoretical plate calculates by the jasminoidin peak should be not less than 2000;
The preparation precision of reference substance solution takes by weighing through 24 hours jasminoidin reference substance of phosphorus pentoxide drying under reduced pressure an amount of, and thin up behind the dissolve with methanol is made the solution that every 1ml contains 40 μ g, promptly;
The preparation precision of need testing solution is measured this product 5ml, places the 50ml measuring bottle, and thin up shakes up to scale, filters with microporous filter membrane (0.45 μ m), gets subsequent filtrate, promptly;
Accurate respectively reference substance solution and each the 20 μ l of need testing solution of drawing of algoscopy inject chromatograph of liquid, measure, promptly;
The every 1ml of this product contains Fructus Gardeniae in jasminoidin (C17H24O10), must not be less than 0.25mg.
According to the method for claim 1, it is characterized in that 5, described depression relieving and tranquilizing preparation is to be made by the raw material of Chinese medicine of following weight:
Radix Bupleuri 40g Fructus Jujubae 30g Rhizoma Acori Graminei 40g
The Rhizoma Pinelliae (processed) 30g Rhizoma Atractylodis Macrocephalae (stir-fry) 30g Fructus Tritici Levis 100g
Radix Polygalae (system) 40g Radix Glycyrrhizae (processing) 30g Fructus Gardeniae (stir-fry) 40g
Bulbus Lilii 100g Arisaema Cum Bile 40g Radix Curcumae 40g
Dens Draconis 100g Semen Ziziphi Spinosae (stir-fry) 50g Poria 50g
Radix Angelicae Sinensis 30g.
6, according to the method for claim 1, it is characterized in that, wherein said depression relieving and tranquilizing preparation is by raw material of Chinese medicine is processed through extraction or other modes, make pharmaceutically active substance, subsequently, be raw material with this material, add the medicine acceptable carrier when needing, make according to the routine techniques of galenic pharmacy, described active substance obtains by the method that is selected from following mode: pulverize, squeeze, calcine, grind, sieve, percolation, extraction, water are carried, alcohol extraction, ester are carried, ketone is carried or chromatography.
According to the method for claim 6, it is characterized in that 7, wherein said depression relieving and tranquilizing preparation is a syrup.
According to the method for claim 7, it is characterized in that 8, wherein said syrup is by preparing through following method: the material of getting it filled, decoct with water three times, 3 hours for the first time, second and third time each 2 hours, collecting decoction, filter, filtrate is concentrated into the clear paste that relative density is about 1.06 ~ 1.08 (55 ℃～60 ℃), and adding sucrose 460g and potassium sorbate are an amount of, and the dissolving back filters, add water to 1000ml, promptly.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100656478A CN100533140C (en) | 2006-03-23 | 2006-03-23 | Checking method for depression relieving and tranquilizing preparation |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100656478A CN100533140C (en) | 2006-03-23 | 2006-03-23 | Checking method for depression relieving and tranquilizing preparation |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1857642A true CN1857642A (en) | 2006-11-08 |
| CN100533140C CN100533140C (en) | 2009-08-26 |
Family
ID=37296630
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2006100656478A Expired - Fee Related CN100533140C (en) | 2006-03-23 | 2006-03-23 | Checking method for depression relieving and tranquilizing preparation |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN100533140C (en) |
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101757564A (en) * | 2010-02-27 | 2010-06-30 | 赵世明 | Traditional Chinese medicine composition for treating liver depression and qi stagnation |
| CN101773641A (en) * | 2009-01-12 | 2010-07-14 | 北京亚东生物制药有限公司 | Chinese medicine composition preparation for liver soothing and depression relief and quality control method |
| CN102626474A (en) * | 2011-08-08 | 2012-08-08 | 仲崇琳 | Pharmaceutical composition with efficacy of relieving depressed liver and tranquilizing mind |
| CN103920089A (en) * | 2014-01-15 | 2014-07-16 | 曹红梅 | Traditional Chinese medicinal composition for treating climacteric syndrome |
| CN104950069A (en) * | 2015-06-23 | 2015-09-30 | 南京海昌中药集团有限公司 | Method for detecting quality of depression-relieving heart-comforting tablet |
| CN105021762A (en) * | 2015-07-23 | 2015-11-04 | 河北中医学院 | Spine date seed water extract product rapid multi-information thin layer discriminating method |
| CN105079699A (en) * | 2015-05-17 | 2015-11-25 | 王兰英 | Traditional Chinese medicine composition for treating climacteric syndrome |
| CN105194586A (en) * | 2015-11-11 | 2015-12-30 | 通化斯威药业股份有限公司 | Medicine for regulating vital energy, dispelling melancholy, calming and soothing nerves, removing anxiety and insomnia and treating climacteric syndrome and preparation method |
| CN105343639A (en) * | 2015-12-11 | 2016-02-24 | 马艳华 | Traditional Chinese medicine composition for treating insomnia |
| CN107801819A (en) * | 2017-12-07 | 2018-03-16 | 陈英英 | A kind of spina date seed mind easing tea and preparation method thereof |
| CN110873776A (en) * | 2018-08-30 | 2020-03-10 | 四川新绿色药业科技发展有限公司 | Identification method of gardenia and fried gardenia formula granules |
-
2006
- 2006-03-23 CN CNB2006100656478A patent/CN100533140C/en not_active Expired - Fee Related
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101773641A (en) * | 2009-01-12 | 2010-07-14 | 北京亚东生物制药有限公司 | Chinese medicine composition preparation for liver soothing and depression relief and quality control method |
| CN101757564A (en) * | 2010-02-27 | 2010-06-30 | 赵世明 | Traditional Chinese medicine composition for treating liver depression and qi stagnation |
| CN102626474A (en) * | 2011-08-08 | 2012-08-08 | 仲崇琳 | Pharmaceutical composition with efficacy of relieving depressed liver and tranquilizing mind |
| CN103920089A (en) * | 2014-01-15 | 2014-07-16 | 曹红梅 | Traditional Chinese medicinal composition for treating climacteric syndrome |
| CN105079699A (en) * | 2015-05-17 | 2015-11-25 | 王兰英 | Traditional Chinese medicine composition for treating climacteric syndrome |
| CN104950069A (en) * | 2015-06-23 | 2015-09-30 | 南京海昌中药集团有限公司 | Method for detecting quality of depression-relieving heart-comforting tablet |
| CN104950069B (en) * | 2015-06-23 | 2016-08-24 | 南京海昌中药集团有限公司 | A kind of resolving depression satisfactory tablet quality detection method |
| CN105021762A (en) * | 2015-07-23 | 2015-11-04 | 河北中医学院 | Spine date seed water extract product rapid multi-information thin layer discriminating method |
| CN105194586A (en) * | 2015-11-11 | 2015-12-30 | 通化斯威药业股份有限公司 | Medicine for regulating vital energy, dispelling melancholy, calming and soothing nerves, removing anxiety and insomnia and treating climacteric syndrome and preparation method |
| CN105343639A (en) * | 2015-12-11 | 2016-02-24 | 马艳华 | Traditional Chinese medicine composition for treating insomnia |
| CN107801819A (en) * | 2017-12-07 | 2018-03-16 | 陈英英 | A kind of spina date seed mind easing tea and preparation method thereof |
| CN110873776A (en) * | 2018-08-30 | 2020-03-10 | 四川新绿色药业科技发展有限公司 | Identification method of gardenia and fried gardenia formula granules |
Also Published As
| Publication number | Publication date |
|---|---|
| CN100533140C (en) | 2009-08-26 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN1857642A (en) | Quality control method for depression relieving and tranquilizing preparation | |
| CN1895617A (en) | Kidney-warming and heart-nourishing Chinese-medicinal preparation, its making method and quality control | |
| CN1876040A (en) | Pharmaceutical composition for treating hepatitis, its preparation process and quality control method | |
| CN1785380A (en) | Quality control method of Chinese medicinal preparation | |
| CN1876089A (en) | A pharmaceutical composition for treating kidney-qi deficiency syndrome and preparation method thereof | |
| CN1876161A (en) | Pharmaceutical formulation and preparing method for breast nodules for treating hyperplasia of mammary glands, and its quality control method | |
| CN1903325A (en) | Blood-sugar lowering A prepn. for treating diabetes, its prepn. method and quality-control method | |
| CN1785295A (en) | Quality control method of cbinese medicinal preparation | |
| CN1857551A (en) | Quality control method for Chinese medicine preparation | |
| CN1785281A (en) | Quality control method of spirit quieting oral liquid preparation | |
| CN1895410A (en) | Medicinal composition for treating cough and its preparation | |
| CN1907481A (en) | Medicinal composition for treating summer heat-dampness rheum and preparation method thereof | |
| CN100344321C (en) | Medicinal composition, its preparation process and quality control method | |
| CN1907436A (en) | Medicinal composition for treating children's anorexia and preparation method thereof | |
| CN1857588A (en) | Quality control method for Xianlinggubao preparation | |
| CN103550398A (en) | Composition for relieving fatigue as well as preparation method and medical application thereof | |
| CN1824245A (en) | Quality control method of bone sinew medicinal pill preparation | |
| CN101472600A (en) | Medicament composition for regulating blood sugar and blood fat as well as preparation method and application thereof | |
| CN1857445A (en) | Quality control method for Desheng preparation | |
| CN1857406A (en) | Quality control method for Chinese medicine preparation | |
| CN1857592A (en) | Quality control method for trauma treating Diedahongyao preparation | |
| CN1857424A (en) | Compound Chinese medicine preparation and its preparing process and quality control method | |
| CN1323700C (en) | Traditional Chinese medicine composition for treating deficiency disease and preparation method and quality standard thereof | |
| CN1850268A (en) | Semen caesalpiniae Chinese medicine preparation for treating cold, its preparing method and quality control method | |
| CN1843442A (en) | Oral disintegration tablet of 'Huo Xiang Zheng Qi' and preparation method and quality control method |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C56 | Change in the name or address of the patentee | ||
| CP03 | Change of name, title or address |
Address after: 1266 No. 330052 Nanchang Huiren Jiangxi economic and Technological Development Zone Avenue. Patentee after: JIANGXI HUIREN PHARMACEUTICAL CO.,LTD. Address before: 330043 1189 Yingbin Avenue, Nanchang, Jiangxi Patentee before: Jiangxi Huiren Pharmaceutical Co.,Ltd. |
|
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20090826 |