CN103230517A - Adenophora radix ophiopogonis soup formula granules as well as preparation method and detection method thereof - Google Patents
Adenophora radix ophiopogonis soup formula granules as well as preparation method and detection method thereof Download PDFInfo
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Abstract
The invention provides adenophora radix ophiopogonis soup formula granules as well as a preparation method and a detection method thereof. The granules comprises the raw materials as follows: radix glehniae, radix polygonati officinalis, radix ophiopogonis, radices trichosanthis, hyacinth beans, mulberry leaves and raw liquorice in the mass ratio of (0.5-2):(0.5-2):(0.5-2):(1-3):(0.5-2):(0.1-1.2):(0.1-1), and the raw materials are respectively immersed for multiple times, boiled and filtered, so as to obtain cream after filter liquors are mixed and concentrated, and the cream is dried to be prepared into granules. The detection method comprises the following steps of: identifying the adenophora ophiopogonis soup formula granules through a using thin-layer chromatography; measuring the content of organic chloride pesticide residue in the adenophora ophiopogonis soup formula granules through using a pesticide residue measuring method; measuring the content of heavy metal in the adenophora ophiopogonis soup formula granules through using a residue on ignition examination method; measuring the content of extractum of the adenophora ophiopogonis soup formula granules through using a hot dipping method; and measuring the content of substances in the adenophora ophiopogonis soup formula granules through a using high-efficiency liquid chromatography.
Description
Technical field
The invention belongs to the field of Chinese medicines, relate to a kind of Chinese medicine and preparation method thereof and detection method, relate in particular to a kind of decoction made from radix adenophorea, tuber of dwarf lilyturf granule and preparation method thereof and detection method.
Background technology
Decoction made from radix adenophorea, tuber of dwarf lilyturf comes from " epidemic febrile disease regulations ", and ancient books opinion we are agent of clearing away heat and promoting production of body fluid.Mainly use Radix Adenophorae (Radix Glehniae) in the side, support the moon of lung stomach.And be aided with Radix Ophiopogonis, Radix Trichosanthis, the heat of lung heat clearing stomach.With Rhizoma Polygonati Odorati with tonify deficiency, Seem Lablab Album with middle medicine as double system.Quote the hardship of Folium Mori at last and light lung qi dispersing heat and the born fluid with the sweet of Radix Glycyrrhizae.Body fluid is given birth to, scorching removing, and each demonstrate,proves spontaneous recovery.
The research of decoction made from radix adenophorea, tuber of dwarf lilyturf modern pharmacology and clinical research show that decoction made from radix adenophorea, tuber of dwarf lilyturf has antibiotic, and antiinflammatory is eliminated the phlegm, antiallergic, raise immunity and raising hypoxia-bearing capability etc.
1. anti-inflammation: Radix Ophiopogonis, Folium Mori, Radix Trichosanthis all have inhibitory action to staphylococcus aureus, escherichia coli, Bacillus typhi etc., and Radix Glycyrrhizae, Radix Trichosanthis have antibacterial and anti-inflammation functions.
2. expelling phlegm for arresting cough: Radix Glycyrrhizae, Radix Adenophorae (Radix Glehniae) all have significantly eliminate the phlegm, antitussive effect.
3. antiallergic: Radix Glycyrrhizae has the effect of glucocorticoid sample, suppresses anaphylaxis and suppresses the immunoreation of macrophage.
4. raise immunity: Folium Mori can improve the phagocytic function of macrophage, make the eosinophilia.
5. raising hypoxia-bearing capability: Radix Ophiopogonis, Rhizoma Polygonati Odorati all can obviously prolong the time of mice anoxia enduring.
Comprehensive ancient literature and modern pharmacology as can be known, this side's clinical application range is wide.
Chinese medicinal granule is under Chinese medical theory instructs, and the prepared slices of Chinese crude drugs of concocting processing with standard are raw material, adopts Technology such as extraction, cryoconcentration, wink-dry and the granule made.It both can supply clinical flexible prescription, and allotment is taken after mixing it with water, and can be used as the raw material of industry that supplies of Chinese medicine preparation again, also provided new approach for the tcm clinical practice medication.Compare with traditional Chinese herbs decoction, the advantage of granule agent keeps the nature and flavor feature of original Chinese medicine, the characteristic that has kept differentiation of tcm, develop rational production technology according to the character of Chinese medicine, formulate advanced feasible quality control standard, be processed into and be standardization, standardization, industrialized modern Chinese medicine preparation.Overcome the Chinese medicine decoction decoct time-consuming, take inconvenience, technology extensive, lack drawback such as quality control, adapted to the demand of modern social development.
Aspect clinical practice, Chinese medicinal granule can be in strict accordance with the genuine high-quality medical material of standard application, the control prepared slice quality, help to improve the management level of Chinese medicine quality, can overcome because medical material home environment, natural conditions, gather, the prepared slices of Chinese crude drugs inherent quality of all multifactor impacts such as processing method, storage keeping, decoction pieces processing processing procedure, guarantee clinical efficacy; Can reduce the difference of the clinical efficacy that causes owing to prepared slices of Chinese crude drugs quality disunity.More traditional family decocts decoction pieces, Chinese medicinal granule overcome in traditional decoction pieces decoction process be decocted first, the back down, decoct a drug wrapped and decoct difficult problems such as container is lack of standardization, to guaranteeing and stable clinical efficacy has remarkable advantages.Chinese medicinal granule adopts aluminium foil bag or other to pack easily, dosage is accurate, avoided common in the storage of Chinese medicine decoction pieces and gone rancid, variable color, a difficult problem such as damage by worms, go mouldy, being convenient to medicine storage and patient portably uses, the patient has saved the trouble that decocts in the use, even go on business, travel, can therapy discontinued yet.Be conducive to expand the foreign market Chinese medicinal granule and in the production and processing overall process, implement the GMP monitoring, each kind has been set up production and quality management file separately respectively from each link of raw material, intermediate, semi-finished product, finished product, and according to standard operation, be conducive to promote internationalization of tcm.
The single medicinal material decoction pieces granule that the present Chinese medicinal granule of using is made by modern pharmaceutical technology with single medicinal material mostly, existing hundreds of single decoction pieces granules listings.Although yet Chinese medicinal granule has lot of advantages, make and clinical practice in also have many drawbacks, still have certain gap with the principal mode Chinese medicine decoction of traditional middle medical drugs.Chinese medicine decoction is that compound compatibility is fried in shallow oil and formed, the not simple addition of the chemical constituent of single medicinal material in the side of being equal to of the material base of its clinical efficacy, but the interactional synthesis result of various chemical constituent.Chinese medicine contains pigment, polysaccharide, protein, lipid, tannin, flavonoid, Coumarins, lignanoids, anthraquinone class, glycoside, organic acid, alkaloids, terpenoid and derivant thereof more, close in the process of frying in shallow oil at prescription, both may directly influence each composition dissolubility, also may be by changing for example pH value, viscosity and dissolubility and for example its dissolving of properties affect of optical activity, charge, osmotic pressure, relative molecular weight, degree of hydration etc. of solute of solvent, or act on mutually with other solutes and to cause water miscible increase and decrease.These effects comprise generation hydrotropy effect; change the dissolution with solvents characteristic; change the solution pH value; change material weak electrolyte ionization degree; generate the new component of high-dissolvability; generate the new component of low solubility; precipitation takes place; generate complex; inorganic ions is combined generation and is insoluble in the salt of water with Chinese medicine ingredients; generate and to play a role uniting of noval chemical compound and various effects etc.; cause single granule mixed dissolution not have whole effective ingredient of " group's medicine is fried in shallow oil altogether "; the effective ingredient that can not comprise middle medical drugs requirement in other words by the granule of existing prepared fully; cause traditional prescription working substance basis to change, so that existing granule medication can not be equal to traditional Chinese medicine decoction.
" fry in shallow oil " this important step altogether owing to ignored group's medicine, ignored the globality of Chinese medicine decoction, finally may cause change or the change of pharmacological actions of clinical efficacy.The flavour of a drug that some patients are reflected Chinese medicinal granule than the inclined to one side hardship of traditional decoction, lay particular stress on, this may be relevant with the content height of Chinese medicinal granule extract.Because the extraction time of Chinese medicinal granule is five or six times of decoction decocting, the relative decoction content of its composition that extracts is higher, and consequent various side effect also can not be ignored.
Therefore, solve the problem that present single medicinal material granule exists, give full play to the advantage of traditional compatibility of medicines in a prescription, reach attenuation synergistic, particularly necessary.The Chinese medicine compound granule has passed on the advantage of Chinese medicine single granule, taken into full account the interaction of decoction pieces in decocting (or other processing) process again, meet traditional Chinese medical science tradition medication theory more than single granule, also possess simultaneously other advantage of granule, have bigger value.
Along with modernization of Chinese medicine development and Chinese medicine move towards the needs of international market, in order to guarantee the quality controllable of tcm product, set up quality standard and have very important significance.But the decoction made from radix adenophorea, tuber of dwarf lilyturf granule does not still have detection method, the control of technology and the monitoring of medicine in being unfavorable for producing at present at present.
Summary of the invention
Therefore, the objective of the invention is the deficiency of simple addition when single decoction pieces granule is taken in the prior art, a kind of decoction made from radix adenophorea, tuber of dwarf lilyturf granule is provided, and a kind of preparation method and detection method of decoction made from radix adenophorea, tuber of dwarf lilyturf granule are provided.
Unless specialize, " this product " herein all refers to " decoction made from radix adenophorea, tuber of dwarf lilyturf granule ".
Unless specialize, herein " Gamma Hexaochlorocyclohexane " all refers to " benzene hexachloride ".
Unless specialize, " clofenotane " herein all refers to " biconjugate chlorphenyl trichloroethane ".
Unless stated otherwise, the hot dipping under involved thin layer chromatography, high performance liquid chromatography and the ethanol-soluble extractives algoscopy item all is to carry out according to the test method that Chinese Pharmacopoeia was put down in writing in the version in 2010 herein.
Unless specialize, related herein hydrochloric acid is the hydrochloric acid of mass fraction 37.5.
On the one hand, the invention provides a kind of decoction made from radix adenophorea, tuber of dwarf lilyturf granule, described decoction made from radix adenophorea, tuber of dwarf lilyturf granule comprises Radix Glehniae, Rhizoma Polygonati Odorati, Radix Ophiopogonis, Radix Trichosanthis, Seem Lablab Album, Folium Mori and the Radix Glycyrrhizae seven flavor raw materials of mass ratio 0.5～2:0.5～2:0.5～2:1～3:0.5～2:0.1～1.2:0.1～1, described raw material through several times soak, decoct, filter and merging filtrate, be condensed into clear paste, drying is made granule, both; Preferably, the mass ratio of Radix Glehniae, Rhizoma Polygonati Odorati, Radix Ophiopogonis, Radix Trichosanthis, Seem Lablab Album, Folium Mori and Radix Glycyrrhizae seven flavor raw materials is 1～2:1～2:1～2:1.5～2.5:1～2:0.6～1:0.3～1, more preferably, the mass ratio of Radix Glehniae, Rhizoma Polygonati Odorati, Radix Ophiopogonis, Radix Trichosanthis, Seem Lablab Album, Folium Mori and Radix Glycyrrhizae seven flavor raw materials is 1:1:1:1.5:1:0.6:0.3.
Described raw material and the described mass ratio that makes granule are 5～6:1～2, and preferably, described raw material and the described mass ratio that makes granule are 5.12:1.
On the other hand, the invention provides a kind of preparation method of made from radix adenophorea, tuber of dwarf lilyturf granule, said method comprising the steps of:
1) takes by weighing Radix Glehniae, Rhizoma Polygonati Odorati, Radix Ophiopogonis, Radix Trichosanthis, Seem Lablab Album, Folium Mori and the Radix Glycyrrhizae seven flavor raw materials of mass ratio 0.5～2:0.5～2:0.5～2:1～3:0.5～2:0.1～1.2:0.1～1; Preferably, the mass ratio of Radix Glehniae, Rhizoma Polygonati Odorati, Radix Ophiopogonis, Radix Trichosanthis, Seem Lablab Album, Folium Mori and Radix Glycyrrhizae seven flavor raw materials is 1～2:1～2:1～2:1.5～2.5:1～2:0.6～1:0.3～1, more preferably, the mass ratio of Radix Glehniae, Rhizoma Polygonati Odorati, Radix Ophiopogonis, Radix Trichosanthis, Seem Lablab Album, Folium Mori and Radix Glycyrrhizae seven flavor raw materials is 1:1:1:1.5:1:0.6:0.3;
2) described raw material is through soaking, decoct, filtering and merging filtrate;
3) with described filtrate simmer down to clear paste;
4) make granule with adding adjuvant after the described clear paste drying, both.
Wherein, step 2) amount of water that soaks described in is 6～10 weight portions of raw material, preferred 8 weight portions, and described soak time is 1～2 hour, preferred 1 hour;
Described decoction is carried out at twice, and decocting time is 1～2 hour for the first time, preferred 2 hours; For the second time decoct 6～10 weight portions that amount of water is raw material, preferred 6 weight portions, described decocting time are 1-2 hour, preferred 1 hour;
The clear paste of relative density 1.08～1.18 during 60 ℃ of simmer down tos of filtrate described in the step 3); Preferably, the relative density relative density is 1.14 clear paste during 60 ℃ of simmer down tos of filtrate described in the step 3).
Preferably, described simmer down to concentrating under reduced pressure.
Preferably, described drying is spray drying.
Preferably, described spray-dired inlet temperature is 154 ℃, and leaving air temp is 95 ℃.
Right-hand member, described adjuvant is pharmaceutically acceptable carrier or excipient.
Preferably, after described step 4) was made granule, packing obtained finished product.
On the one hand, the present invention also provides a kind of detection method of decoction made from radix adenophorea, tuber of dwarf lilyturf granule, said method comprising the steps of again:
A): qualitative detection composition Radix Ophiopogonis; Wherein, described qualitative detection is undertaken by thin layer chromatography; Wherein, test sample is the decoction made from radix adenophorea, tuber of dwarf lilyturf granule, and control medicinal material is Radix Ophiopogonis;
B): the qualitative detection licorice ingredient; Wherein, described qualitative detection is undertaken by thin layer chromatography; Wherein, test sample is the decoction made from radix adenophorea, tuber of dwarf lilyturf granule, and control medicinal material is Radix Glycyrrhizae;
C): measure content of beary metal in the described decoction made from radix adenophorea, tuber of dwarf lilyturf granule by the residue on ignition inspection technique;
D): measure organochlorine pesticide residual content in the described decoction made from radix adenophorea, tuber of dwarf lilyturf granule by the persticide residue algoscopy;
E): detect extract content by ethanol-soluble extractives hot dipping algoscopy;
F): by the content of material in the described decoction made from radix adenophorea, tuber of dwarf lilyturf granule of high effective liquid chromatography for measuring.
Preferably, in the step a), described test sample and control medicinal material are handled by chloroform extraction respectively, will obtain residue behind the chloroform evaporate to dryness, add ethanol to dissolving, to make need testing solution and control medicinal material solution in residue;
In the step a), developing solvent is chloroform-acetone; Developer is the ethanol solution of sulfuric acid of volume ratio 10%;
In the step b), described test sample and control medicinal material are respectively by adding methanol, supersound process, filtration treatment, after the filtrate water dissolving, use n-butanol extraction, the washing of reuse n-butyl alcohol saturation water, abandon water liquid and with behind the n-butyl alcohol evaporate to dryness, in residue, add methanol to dissolving, to make need testing solution and control medicinal material solution;
In the step b), developing solvent is ethyl acetate-formic acid-glacial acetic acid-water; Developer is the ethanol solution of sulfuric acid of volume ratio 10%;
In the step c), the content of beary metal≤25ppm that records;
In the step d), described organochlorine pesticide is Gamma Hexaochlorocyclohexane, clofenotane and pentachloronitrobenzene, the content≤0.20ppm of described Gamma Hexaochlorocyclohexane; Content≤the 0.20ppm of described clofenotane, the content≤0.10ppm of described pentachloronitrobenzene;
Step f) is undertaken by the method that may further comprise the steps:
1) carrying out chromatographic condition and system suitability test, wherein is filler with the octadecylsilane chemically bonded silica; Being mobile phase A with methanol, is Mobile phase B (58:42) with 0.2mol/L ammonium acetate 2% acetic acid solution, and the detection wavelength is 237nm, and number of theoretical plate calculates by the ammonium glycyrrhizinate peak should be not less than 5000;
2) preparation testing sample solution, by high effective liquid chromatography for measuring, described testing sample solution comprises reference substance solution and need testing solution;
3) measure, both got the result.
More preferably, in the step a), described need testing solution and control medicinal material solution make by following steps: get test sample 1g, add water 15mL, add hydrochloric acid 0.5ml, put in the water-bath reflux 10 minutes, and put coldly, extract with chloroform 20ml jolting, divide and get chloroform liquid, evaporate to dryness, residue add ethanol 1ml makes dissolving, makes need testing solution; Other gets control medicinal material 1g Radix Ophiopogonis, adds water 20ml, decocts 10 minutes, filters, filtrate adds hydrochloric acid 0.5ml, puts in the water-bath reflux 10 minutes, puts coldly, extracts with chloroform 20ml jolting, divide and get chloroform liquid, evaporate to dryness, residue add ethanol 1ml makes dissolving, makes control medicinal material solution;
In the step b), described need testing solution and control medicinal material solution make by following steps: get test sample 0.5g, add methanol 40ml, supersound process 30 minutes filters the filtrate evaporate to dryness, residue adds water 20ml makes dissolving, extracts 2 times with water saturated n-butyl alcohol jolting, each 25ml, merge extractive liquid,, the water 30ml washing that the reuse n-butyl alcohol is saturated discards water liquid, n-butyl alcohol liquid evaporate to dryness, residue adds methanol 1ml makes dissolving, makes need testing solution;
Extracting liquorice control medicinal material 0.5g adds methanol 40ml, supersound process 30 minutes in addition, filter, filtrate evaporate to dryness, residue add water 20ml makes dissolving, extract 2 times with water saturated n-butyl alcohol jolting, each 25ml, merge extractive liquid,, the water 30ml washing that the reuse n-butyl alcohol is saturated, discard water liquid, n-butyl alcohol liquid evaporate to dryness, residue add methanol 1ml makes dissolving, makes control medicinal material solution;
In the step f), the method preparation of described reference substance solution by may further comprise the steps: described extracting liquorice acid ammonium reference substance is an amount of, accurately claims surely, adds 70% and adds ethanol and make the solution that every 1ml contains ammonium glycyrrhizinate 10 μ g respectively, namely;
In the step f), the method preparation of described need testing solution by may further comprise the steps: get this product 2.0g, the accurate title, decide, put in the tool plug conical flask accurate 70% alcoholic solution 100ml, the close plug of adding, claim to decide weight, supersound process 30 minutes is put cold, claim to decide weight again, supply the weight that subtracts mistake with 70% ethanol, shake up, filter, get subsequent filtrate, namely;
Preferably, the power of described supersound process is 240W, and frequency is 45kHZ.
This product is pressed dry product and is calculated, and every bag contains with glycyrrhizic acid (C
21H
22O
9) meter, must not be less than 100mg.
Decoction made from radix adenophorea, tuber of dwarf lilyturf is used for dry impairing the lung stomach, and body fluid loses and sees thirsty and dry pharynx or the few expectorant of dry cough, the few tongue of red tongue, thready and rapid pulse person.So this granule function is described as promoting production of body fluid with drugs sweet in flavor and cold in nature with curing mainly, support the lung stomach clearly.Be used for dry impairing the lung stomach, body fluid loses and sees thirsty and dry pharynx or the few expectorant of dry cough, the few tongue of red tongue, thready and rapid pulse person.Clinical practice is extensive.
Compared with prior art, the present invention has the following advantages:
(1) decoction made from radix adenophorea, tuber of dwarf lilyturf closes by traditional method and fries in shallow oil, and gives full play to the advantage of drug matching, has embodied the Chinese medicine organic conception, guarantees that it reaches the purpose of attenuation synergistic, the deficiency that the simple addition of each flavour of a drug brings when having overcome present single granule and taking;
(2) provide the perfect detection method of decoction made from radix adenophorea, tuber of dwarf lilyturf granule of knowing clearly, can control the quality of this granule effectively, with better guidance production, make controlling of production process stricter rationally, in process of producing product, the quality of product be can effectively control, thereby clinical efficacy and the safety of decoction made from radix adenophorea, tuber of dwarf lilyturf granule guaranteed.
(3) the decoction made from radix adenophorea, tuber of dwarf lilyturf granule is convenient to that medicine stores and the patient portably uses, and the patient has saved the trouble of decoction in the use; The granule preparation is simple, meets Chinese medicine medication characteristics, and quality is certainly controlled, portably uses conveniently, meets modern people to the requirement of medicine " three is little ", " triple effect " and " five convenience ".
(4) to promoting traditional Chinese medicine modernization that big meaning is arranged.
This invention is with a wide range of applications.
Description of drawings
Below, describe embodiment of the present invention by reference to the accompanying drawings in detail, wherein:
Fig. 1 is the process chart of decoction made from radix adenophorea, tuber of dwarf lilyturf granule of the present invention;
Fig. 2 is the thin layer chromatography chromatogram of differentiating the Radix Ophiopogonis of decoction made from radix adenophorea, tuber of dwarf lilyturf granule of the present invention; Among the figure, 1 is the need testing solution of decoction made from radix adenophorea, tuber of dwarf lilyturf granule, and 2 is control medicinal material solution Radix Ophiopogonis, 3 negative contrast solutions;
Fig. 3 is the thin layer chromatography chromatogram that the Radix Glycyrrhizae of decoction made from radix adenophorea, tuber of dwarf lilyturf granule of the present invention is differentiated; Among the figure, 1-2 is the need testing solution of decoction made from radix adenophorea, tuber of dwarf lilyturf granule, and 3-4 is Radix Glycyrrhizae control medicinal material solution, the negative contrast solution of 5-6;
Fig. 4 is the specificity result of the test of decoction made from radix adenophorea, tuber of dwarf lilyturf granule of the present invention, and wherein, Fig. 4 a is the high-efficient liquid phase chromatogram of blank solvent (methanol) reference substance solution; Fig. 4 b is sample (lot number: the 20121101) high-efficient liquid phase chromatogram of reference substance; Fig. 4 c is the high-efficient liquid phase chromatogram of Radix Glycyrrhizae negative sample solution; Fig. 4 d is the high-efficient liquid phase chromatogram of ammonium glycyrrhizinate sample solution.
Fig. 5 is the ammonium glycyrrhizinate sample size in the decoction made from radix adenophorea, tuber of dwarf lilyturf granule of the present invention and the linear relationship chart of peak area.
The specific embodiment
The preparation condition of embodiment 1 decoction made from radix adenophorea, tuber of dwarf lilyturf granule is selected
1 material and instrument
1.1 crude drug source
Pharmaceutical decocting piece all meet " Chinese pharmacopoeia each decoction pieces of version in 2010 is provided by Kangmei Pharmaceutical Co., Ltd, the source and the place of production see Table 1.
Table 1 crude drug source table
1.2 instrument and equipment
B-290 type spray drying instrument, Switzerland goes on foot outstanding company;
RE-5205 type Rotary Evaporators, Shanghai Yarong Biochemical Instrument Plant.
2. as follows to decoction made from radix adenophorea, tuber of dwarf lilyturf soup formula granule Study on extraction:
The influence factor has: extraction time, extraction time, amount of water (all times scale with quality of medicinal material shows).Adopt the preferred extraction process of orthogonal test, select L
9(3
4) orthogonal table, above-mentioned three factors of high spot reviews serve as to investigate index with the content of ammonium glycyrrhizinate, the factor level table sees Table 2
Table 2
Test method: take by weighing Radix Glehniae 50g in the prescription ratio, Rhizoma Polygonati Odorati 50g, Radix Ophiopogonis 50g, Radix Trichosanthis 75g, Seem Lablab Album 50g, Folium Mori 30g, Radix Glycyrrhizae 15g, the numbering 1～9, press L
9(3
4) orthogonal table arrangement test, result of the test sees Table 3:
Table 3L
9(3
4) orthogonal experiments
The content analysis of variance table of table 4 ammonium glycyrrhizinate
| Soruces of variation | Sum of square of deviations | Degree of freedom | F Ratio | The F marginal value | Significance |
| A | 0.256 | 2 | 2.277 | 5.140 | ? |
| B | 0.016 | 2 | 0.161 | 5.140 | ? |
| C | 0.026 | 2 | 0.262 | 5.140 | ? |
| Error | 0.30 | 6 | ? | ? | ? |
The content analysis of variance table of table 5 spray drying powder yield
| Soruces of variation | Sum of square of deviations | Degree of freedom | F Ratio | The F marginal value | Significance |
| A | 0.309 | 2 | 0.251 | 5.140 | ? |
| B | 1.182 | 2 | 0.962 | 5.140 | ? |
| C | 2.196 | 2 | 1.787 | 5.140 | ? |
| Error | 3.69 | 6 | ? | ? | ? |
Finding out from table 4 and table 5, is index analysis with the content of ammonium glycyrrhizinate and the yield of spray drying powder, and each factor does not make significant difference, and optimizes process conditions to be: A
2B
1C
2; Comprehensive above-mentioned analysis of experiments from the angle that industrialized great production cuts down the consumption of energy, guarantees under the prerequisite of effective component content, changes amount of water into 8 times of amounts for the first time, 6 times of amounts for the second time.
The preparation of embodiment 2 decoction made from radix adenophorea, tuber of dwarf lilyturf granules
Take by weighing Radix Glehniae 50g in the prescription ratio, Rhizoma Polygonati Odorati 50g, Radix Ophiopogonis 50g, Radix Trichosanthis 75g, Seem Lablab Album 50g, Folium Mori 30g, Radix Glycyrrhizae 15g water logging bubble 1h, decoct secondary, add 8 times of amounts of water for the first time and decocted 2 hours, add 6 times of water gagings for the second time and decocted 1 hour, filter merging filtrate, 80 ℃ of concentrating under reduced pressure, be concentrated into the clear paste of relative density 1.14 (60 ℃), spray drying, inlet temperature are 154 ℃, 95 ℃ of leaving air temps, revolution speed 25%, the dry dry extract that gets.Press with quadrat method and repeat six times, the dry extract that makes the results are shown in Table 6
Table 6 dry extract yield and character
This method yield height, process stabilizing, and be loyal to former side's method for making.
And be the yellowish-brown granule according to the decoction made from radix adenophorea, tuber of dwarf lilyturf granule that 6 batch samples are described as making strictly according to the facts; Feeble QI, bitter in the mouth.
The preparation of embodiment 3 decoction made from radix adenophorea, tuber of dwarf lilyturf granules
Take by weighing Radix Glehniae 50g in the prescription ratio, Rhizoma Polygonati Odorati 50g, Radix Ophiopogonis 50g, Radix Trichosanthis 75g, Seem Lablab Album 50g, Folium Mori 30g, Radix Glycyrrhizae 15g water logging bubble 1h decocts secondary, add for the first time 8 times of amounts of water and decocted 2 hours, add 6 times of water gagings for the second time and decocted 1 hour, filter merging filtrate, 80 ℃ of concentrating under reduced pressure are concentrated into the clear paste of relative density 1.08-1.18 (60 ℃), spray drying, inlet temperature is 154 ℃, 95 ℃ of leaving air temps, revolution speed 25%, the dry dry extract that gets is granulated the cream powder, both.
The preparation of embodiment 4 decoction made from radix adenophorea, tuber of dwarf lilyturf granules
Take by weighing Radix Glehniae 50g in the prescription ratio, Rhizoma Polygonati Odorati 50g, Radix Ophiopogonis 50g, Radix Trichosanthis 62.5g, Seem Lablab Album 50g, Folium Mori 50g, Radix Glycyrrhizae 50g water logging bubble 5h, decoct secondary, add 6 times of amounts of water for the first time and decocted 2 hours, add 10 times of water gagings for the second time and decocted 1 hour, filter merging filtrate, 80 ℃ of concentrating under reduced pressure, be concentrated into the clear paste of relative density 1.14 (60 ℃), spray drying, inlet temperature are 154 ℃, 95 ℃ of leaving air temps, revolution speed 25%, the dry dry extract that gets.
The preparation of embodiment 5 decoction made from radix adenophorea, tuber of dwarf lilyturf granules
Take by weighing Radix Glehniae 50g in the prescription ratio, Rhizoma Polygonati Odorati 50g, Radix Ophiopogonis 50g, Radix Trichosanthis 100g, Seem Lablab Album 50g, Folium Mori 5g, Radix Glycyrrhizae 5g water logging bubble 1h, decoct secondary, add 10 times of amounts of water for the first time and decocted 2 hours, add 8 times of water gagings for the second time and decocted 1 hour, filter merging filtrate, 80 ℃ of concentrating under reduced pressure, be concentrated into the clear paste of relative density 1.14 (60 ℃), spray drying, inlet temperature are 154 ℃, 95 ℃ of leaving air temps, revolution speed 25%, the dry dry extract that gets.
The preparation of embodiment 6 decoction made from radix adenophorea, tuber of dwarf lilyturf granules
Take by weighing Radix Glehniae 50g in the prescription ratio, Rhizoma Polygonati Odorati 50g, Radix Ophiopogonis 50g, Radix Trichosanthis 75g, Seem Lablab Album 50g, Folium Mori 30g, Radix Glycyrrhizae 25g water logging bubble 1h, decoct secondary, add 8 times of amounts of water for the first time and decocted 2 hours, add 6 times of water gagings for the second time and decocted 1 hour, filter merging filtrate, 80 ℃ of concentrating under reduced pressure, be concentrated into the clear paste of relative density 1.14 (60 ℃), spray drying, inlet temperature are 154 ℃, 95 ℃ of leaving air temps, revolution speed 25%, the dry dry extract that gets.
Embodiment 7 thin layer chromatography are identified the decoction made from radix adenophorea, tuber of dwarf lilyturf granule that embodiment 2 makes
With reference to " Chinese pharmacopoeia version in 2010 " yin nourishing hemopoietic mixture ", " stomach nourishing granule ", " SUNJU GANMAO PIAN " are differentiated a formulation, and 20121101 batches of samples are differentiated, specify as follows:
1, reagent and reagent
Radix Ophiopogonis control medicinal material: lot number is 1201013-200607, purchases in Nat'l Pharmaceutical ﹠ Biological Products Control Institute;
The Radix Glycyrrhizae control medicinal material: lot number is 120904-200511, purchases in Nat'l Pharmaceutical ﹠ Biological Products Control Institute;
Test sample: made by oneself by Kangmei Pharmaceutical Co., Ltd;
Lamellae: silica gel G plate (self-control).
Reagent is analytical pure
2, experimental record
(1) differentiates Radix Ophiopogonis
Test sample preparation: get this product 0.9g, add water 15ml dissolving, add hydrochloric acid 0.5ml, reflux is 10 minutes in the water-bath, puts coldly, extracts with chloroform 20ml jolting, divides and gets chloroform liquid, and evaporate to dryness, residue add ethanol 1ml makes dissolving, as need testing solution.
Control medicinal material preparation: get control medicinal material 1g Radix Ophiopogonis, shine medical material solution in pairs with legal system.
Lamellae: silica gel G plate;
Point sample amount: each 5 μ l;
Point sample mode: spot application;
Developing solvent: chloroform-acetone (4: 1) is developing solvent, is expanded to about 8～13cm, takes out, and dries;
Colour developing and inspecting: spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to speckle colour developing at 105 ℃.
The result: the control medicinal material characteristic point is unintelligible, and test sample characteristic point Radix Ophiopogonis is not obvious, and negative control is noiseless, the results are shown in Figure 2.
(2) Radix Glycyrrhizae is differentiated
The test sample preparation: get this product 0.5g, add methanol 40ml, supersound process 30 minutes filters, and filtrate evaporate to dryness, residue add water 20ml makes dissolving, extracts 2 times with water saturated n-butyl alcohol jolting, each 25ml, merge extractive liquid,, the water 30ml washing that the reuse n-butyl alcohol is saturated.Discard water liquid, n-butyl alcohol liquid evaporate to dryness, residue add methanol 1ml makes dissolving, as need testing solution;
The control medicinal material formulations prepared from solutions: extracting liquorice control medicinal material 0.5g, shine medical material solution in pairs with legal system;
Negative control: make the decoction made from radix adenophorea, tuber of dwarf lilyturf control sample that lacks Radix Glycyrrhizae.Made by oneself by Kang Mei drug research institute.
Lamellae: the silica gel G thin layer version of 1% sodium hydroxide solution preparation;
Point sample amount: each 5 μ l;
Point sample mode: spot application;
Developing solvent: ethyl acetate-formic acid-glacial acetic acid-water (15: 1: 1: 2) be developing solvent, be expanded to about 12cm, take out, dry;
Colour developing and inspecting: spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to speckle colour developing at 105 ℃, the results are shown in Figure 3.
The content of beary metal of the decoction made from radix adenophorea, tuber of dwarf lilyturf granule that embodiment 8 mensuration embodiment 2 make
With reference to " a Chinese pharmacopoeia coptos bolus for clearing the upper heat of version [inspection] in 2010 item checks that the method for heavy metal is formulated, to this product sample (lot number: check that 20121101) result is up to specification down.
The organochlorine pesticide residual content of the decoction made from radix adenophorea, tuber of dwarf lilyturf granule that embodiment 9 mensuration embodiment 2 make
With reference to " the residual algoscopy of Chinese pharmacopoeia version in 2010 appendix IX Q organic chlorine agriculture chemicals reaches " under a Chinese pharmacopoeia Radix Glycyrrhizae of version [inspection] in 2010 item, the method that checks Residual Levels of Organochlorine Pesticides is formulated, to this product sample (lot number: check that 20121101) result is up to specification.
Other of the decoction made from radix adenophorea, tuber of dwarf lilyturf granule that embodiment 10 mensuration embodiment 2 make
With reference to " stipulating under an appendix I of Chinese pharmacopoeia version in 2010 the C granule item, (lot number: [granularity] 20121101), [moisture], [melting], [content uniformity], [microbial limit] check that the result is above-mentioned every all up to specification to this product sample.
The extractum of the decoction made from radix adenophorea, tuber of dwarf lilyturf granule that embodiment 11 mensuration embodiment 2 make
Get this product sample (lot number: 20121101) powder 2g, accurate claim fixed, the accurate ethanol 50ml that adds, weight decided in the accurate title of tool plug, left standstill 1 hour, connects condensing tube, be heated to boiling, and keep little and boiled 1 hour, put cold after, take off conical flask, close plug, weigh again, supply the weight that subtracts mistake with ethanol, shake up, filter with dry filter, precision is measured subsequent filtrate 25ml, puts in the evaporating dish that is dried to constant weight, behind evaporate to dryness in the water-bath, in 105 ℃ of dryings 3 hours, put in the exsiccator, cooled off 30 minutes, weight decided in accurate title rapidly.
The assay of table 7 extractum
| Sample number into spectrum | Sampling amount (g) | Extractum (%) |
| 1 | 2.0495 | 9.38 |
| 2 | 2.0252 | 9.64 |
| 3 | 2.0553 | 9.51 |
The detection method of embodiment 12 decoction made from radix adenophorea, tuber of dwarf lilyturf granules
Character: yellowish-brown granule; Feeble QI, bitter in the mouth.
1. instrument and reagent
1.1 instrument: high performance liquid chromatograph: waterse, the Empower chem workstation; Chromatographic column: Water-C
18(4.6mm * 250mm, 5 μ m); Electronic analytical balance: FA2104, XP6; Ultrasonic cleaning instrument: (KQ-300VDB).
1.2 reagent: methanol is chromatographically pure, and water is ultra-pure water, and other reagent are analytical pure.
1.3 reagent: made from radix adenophorea, tuber of dwarf lilyturf granule (lot number: 20121101); Ammonium glycyrrhizinate (Nat'l Pharmaceutical ﹠ Biological Products Control Institute, content 96.6wt%, lot number: 110731-200409)
2. chromatographic condition and system suitability: be filler with the octadecylsilane chemically bonded silica; Be mobile phase A with methanol, with the 0.2mol/L ammonium acetate, 2% acetic acid is Mobile phase B, and the volume ratio of A:B is 58:42, and the detection wavelength is 237nm, and number of theoretical plate calculates by the ammonium glycyrrhizinate peak should be not less than 5000.
3. the preparation of solution
3.1 the preparation of reference substance solution: precision takes by weighing, ammonium glycyrrhizinate 1.060mg, 1.020mg put respectively in the 20ml volumetric flask, add 70% dissolve with ethanol and be diluted to scale, shake up, measure 5ml again and put and add 70% ethanol dilution in the 25ml volumetric flask to scale, namely get reference substance solution (every 1ml contains ammonium glycyrrhizinate 10.6 μ g, 10.2 μ g).
3.2 the preparation of need testing solution: get this product 2.0g, the accurate title, decide, and puts in the tool plug conical flask, the accurate volume fraction 70% alcoholic solution 100ml that adds, close plug claims to decide weight, power 240W, frequency 45kHz supersound process 30 minutes is put coldly, claims to decide weight again, supply the weight that subtracts mistake with volume fraction 70% alcoholic solution, shake up, filter, namely.
4. methodology checking
4.1 accuracy test
Get 6 parts of this product, the accurate title, decide, and puts in the tool plug conical flask, the accurate volume fraction 70% alcoholic solution 100ml that adds, adding concentration is the close plug of 0.5030mg/ml reference substance, claims to decide weight, supersound process (power 240W, frequency 45kHz) 30 minutes, put coldly, claim to decide weight again, supply the weight that subtracts mistake with volume fraction 70% alcoholic solution, shake up, filter, namely.: be filler with the octadecylsilane chemically bonded silica; Be mobile phase A with methanol, with the 0.2mol/L ammonium acetate, 2% acetic acid is Mobile phase B, and the volume ratio of A:B is 58:42, and detecting wavelength is the 237nm sample introduction,
Table 8
4.2 precision test
4.2.1 replica test
Get 6 parts of this product, the accurate title, decide, and puts in the tool plug conical flask, the accurate volume fraction 70% alcoholic solution 100ml that adds, close plug claims to decide weight, power 240W, frequency 45kHz supersound process 30 minutes is put coldly, claims to decide weight again, supply the weight that subtracts mistake with volume fraction 70% alcoholic solution, shake up, filter, namely.By above-mentioned chromatographic condition, repeat sample introduction 6 times, the record peak area the results are shown in Table 9
Table 9 ammonium glycyrrhizinate replica test result
4.2.2 precision test
Get this product 2.0015g, the accurate title, decide, and puts in the tool plug conical flask, the accurate volume fraction 70% alcoholic solution 100ml that adds, close plug claims to decide weight, power 240W, frequency 45kHz supersound process 30 minutes is put coldly, claims to decide weight again, supply the weight that subtracts mistake with volume fraction 70% alcoholic solution, shake up, filter, namely.By above-mentioned chromatographic condition, repeat sample introduction 6 times, the record peak area the results are shown in Table 4-5.
Table 10 ammonium glycyrrhizinate Precision test result
This law precision is good as seen from the above table, meets the requirement of assay.
4.3 specificity test
Get this product 2.0015g, Radix Glycyrrhizae negative sample 2.1026g, the accurate title, decide, and puts in the tool plug conical flask, the accurate volume fraction 70% alcoholic solution 100ml that adds, close plug claims to decide weight, power 240W, frequency 45kHz supersound process 30 minutes is put coldly, claims to decide weight again, supply the weight that subtracts mistake with volume fraction 70% alcoholic solution, shake up, filter, namely.
Get blank solvent (methanol), sample solution, Radix Glycyrrhizae negative sample solution and ammonium glycyrrhizinate reference substance solution and press method mensuration under the assay item.From collection of illustrative plates as can be known, the sample collection of illustrative plates is having corresponding chromatographic peak with the identical retention time of ammonium glycyrrhizinate reference substance collection of illustrative plates place, and no corresponding chromatographic peak in blank solvent and the negative sample solution, therefore, this content method specificity is good.Chromatogram is seen Fig. 4 a-4d:
4.4 linear relationship
Accurate above-mentioned ammonium glycyrrhizinate reference substance solution 2,5,10,15, the 20 μ l of drawing measure peak area by above-mentioned chromatographic condition, with the peak area integrated value peoniflorin concentration are carried out regression treatment, and regression equation is y=805858x-12438, r=0.9999
Peak area 200,020 159,167 116,789 72,882 29610
Sample size 0.265 0.212 0.159 0.106 0.053
4.5 stability test
Get same made from radix adenophorea, tuber of dwarf lilyturf granule (lot number: 20121101) test liquid, by above-mentioned chromatographic condition, respectively at 0,2,4,6,8,12 hour sample introduction, measure ammonium glycyrrhizinate reference substance peak area.The results are shown in Table 6-7, the result shows that ammonium glycyrrhizinate is stable in 12 hours.
Table 12 stability test result (ammonium glycyrrhizinate)
5. sample size is measured
Get the made from radix adenophorea, tuber of dwarf lilyturf granule, measure by drafting content assaying method, record ammonium glycyrrhizinate (C
21H
22O
9) contain scale 8.
Table 13 sample size measurement result
6. content limit determines
Content limit calculates by 80% of measurement result, because every packed 5g, therefore tentative content limit is every bag and contains Radix Glycyrrhizae with glycyrrhizic acid (C
21H
22O
9) meter, must not be less than 144mg.
Claims (9)
1. decoction made from radix adenophorea, tuber of dwarf lilyturf granule, described decoction made from radix adenophorea, tuber of dwarf lilyturf granule comprises Radix Glehniae, Rhizoma Polygonati Odorati, Radix Ophiopogonis, Radix Trichosanthis, Seem Lablab Album, Folium Mori and the Radix Glycyrrhizae seven flavor raw materials of mass ratio 0.5～2:0.5～2:0.5～2:1～3:0.5～2:0.1～1.2:0.1～1, described raw material through several times soak, decoct, filter and merging filtrate, be condensed into clear paste, drying is made granule, both; Preferably, the mass ratio of Radix Glehniae, Rhizoma Polygonati Odorati, Radix Ophiopogonis, Radix Trichosanthis, Seem Lablab Album, Folium Mori and Radix Glycyrrhizae seven flavor raw materials is 1～2:1～2:1～2:1.5～2.5:1～2:0.6～1:0.3～1, more preferably, the mass ratio of Radix Glehniae, Rhizoma Polygonati Odorati, Radix Ophiopogonis, Radix Trichosanthis, Seem Lablab Album, Folium Mori and Radix Glycyrrhizae seven flavor raw materials is 1:1:1:1.5:1:0.6:0.3.
2. the preparation method of made from radix adenophorea, tuber of dwarf lilyturf granule according to claim 1 said method comprising the steps of:
1) takes by weighing Radix Glehniae, Rhizoma Polygonati Odorati, Radix Ophiopogonis, Radix Trichosanthis, Seem Lablab Album, Folium Mori and the Radix Glycyrrhizae seven flavor raw materials of mass ratio 0.5～2:0.5～2:0.5～2:1～3:0.5～2:0.1～1.2:0.1～1; Preferably, the mass ratio of Radix Glehniae, Rhizoma Polygonati Odorati, Radix Ophiopogonis, Radix Trichosanthis, Seem Lablab Album, Folium Mori and Radix Glycyrrhizae seven flavor raw materials is 1～2:1～2:1～2:1.5～2.5:1～2:0.6～1:0.3～1, more preferably, the mass ratio of Radix Glehniae, Rhizoma Polygonati Odorati, Radix Ophiopogonis, Radix Trichosanthis, Seem Lablab Album, Folium Mori and Radix Glycyrrhizae seven flavor raw materials is 1:1:1:1.5:1:0.6:0.32) described raw material is through soaking, decoct, filtering and merging filtrate;
3) with described filtrate simmer down to clear paste;
4) described clear paste drying is added adjuvant and make granule, both, preferably, described adjuvant is pharmaceutically acceptable carrier or excipient.
3. the preparation method of made from radix adenophorea, tuber of dwarf lilyturf granule according to claim 2 is characterized in that step 2) described in the amount of water that soaks be 6～10 weight portions of raw material gross weight, preferred 8 weight portions, soak time is 1～2 hour, preferred 1 hour.
4. the preparation method of made from radix adenophorea, tuber of dwarf lilyturf granule according to claim 2 is characterized in that step 2) described in decoct and carry out at twice, decocting time is 1～2 hour for the first time, preferred 2 hours; For the second time decoct 6～10 weight portions that amount of water is the raw material gross weight, preferred 6 weight portions, described decocting time are 1-2 hour, preferred 1 hour.
5. according to the preparation method of each described made from radix adenophorea, tuber of dwarf lilyturf granule in the claim 2 to 4, it is characterized in that relative density is 1.08～1.18 to be preferably 1.14 clear paste during 60 ℃ of simmer down tos of filtrate described in the step 3).
6. the preparation method of made from radix adenophorea, tuber of dwarf lilyturf granule according to claim 2 is characterized in that described simmer down to concentrating under reduced pressure; Described drying is spray drying, and preferably, described spray-dired inlet temperature is 154 ℃, and leaving air temp is 95 ℃.
7. the detection method of a decoction made from radix adenophorea, tuber of dwarf lilyturf granule said method comprising the steps of:
A): qualitative detection composition Radix Ophiopogonis: described qualitative detection is undertaken by thin layer chromatography; Wherein, test sample is the decoction made from radix adenophorea, tuber of dwarf lilyturf granule, and control medicinal material is Radix Ophiopogonis;
B): the qualitative detection licorice ingredient: described qualitative detection is undertaken by thin layer chromatography; Wherein, test sample is the decoction made from radix adenophorea, tuber of dwarf lilyturf granule, and control medicinal material is Radix Glycyrrhizae;
C): measure content of beary metal in the described decoction made from radix adenophorea, tuber of dwarf lilyturf granule by the residue on ignition inspection technique;
D): measure organochlorine pesticide residual content in the described decoction made from radix adenophorea, tuber of dwarf lilyturf granule by the persticide residue algoscopy;
E): detect extract content by ethanol-soluble extractives hot dipping algoscopy;
F): by the content of material in the described decoction made from radix adenophorea, tuber of dwarf lilyturf granule of high effective liquid chromatography for measuring.
8. the detection method of decoction made from radix adenophorea, tuber of dwarf lilyturf granule according to claim 7 is characterized in that,
In the step a), described test sample and control medicinal material are handled by chloroform extraction respectively, to obtain residue behind the chloroform evaporate to dryness, in residue, add ethanol to dissolving, to make need testing solution and control medicinal material solution, wherein, developing solvent is that chloroform-acetone and developer are the ethanol solution of sulfuric acid of volume ratio 10%;
In the step b), described test sample and control medicinal material are respectively by adding methanol, supersound process, filtration treatment, after the filtrate water dissolving, use n-butanol extraction, the washing of reuse n-butyl alcohol saturation water is abandoned water liquid and with behind the n-butyl alcohol evaporate to dryness, in residue, add methanol to dissolving, to make need testing solution and control medicinal material solution, wherein, developing solvent is that ethyl acetate-formic acid-glacial acetic acid-water and developer are the ethanol solution of sulfuric acid of volume ratio 10%;
In the step c), the content of beary metal≤25ppm that records;
In the step d), described organochlorine pesticide is Gamma Hexaochlorocyclohexane, clofenotane and pentachloronitrobenzene, the content≤0.20ppm of described Gamma Hexaochlorocyclohexane; Content≤the 0.20ppm of described clofenotane, the content≤0.10ppm of described pentachloronitrobenzene;
Step f) is undertaken by the method that may further comprise the steps:
1) carrying out chromatographic condition and system suitability test, wherein is filler with the octadecylsilane chemically bonded silica; Being mobile phase A with methanol, is Mobile phase B (58:42) with 0.2mol/L ammonium acetate 2% acetic acid solution, and the detection wavelength is 237nm, and number of theoretical plate calculates by the ammonium glycyrrhizinate peak should be not less than 5000;
2) preparation testing sample solution, by high effective liquid chromatography for measuring, described testing sample solution comprises reference substance solution and need testing solution;
3) measure, both got the result.
9. according to the detection method of claim 7 or 8 described decoction made from radix adenophorea, tuber of dwarf lilyturf granules, it is characterized in that,
In the step a), described need testing solution and control medicinal material solution make by following steps: get test sample 1g, add water 15mL, add hydrochloric acid 0.5ml, put in the water-bath reflux 10 minutes, put cold, extract with chloroform 20ml jolting, divide and get chloroform liquid, evaporate to dryness, residue adds ethanol 1ml makes dissolving, makes need testing solution; Other gets control medicinal material 1g Radix Ophiopogonis, adds water 20ml, decocts 10 minutes, filters, filtrate adds hydrochloric acid 0.5ml, puts in the water-bath reflux 10 minutes, puts coldly, extracts with chloroform 20ml jolting, divide and get chloroform liquid, evaporate to dryness, residue add ethanol 1ml makes dissolving, makes control medicinal material solution;
In the step b), described need testing solution and control medicinal material solution make by following steps: get test sample 0.5g, add methanol 40ml, supersound process 30 minutes filters the filtrate evaporate to dryness, residue adds water 20ml makes dissolving, extracts 2 times with water saturated n-butyl alcohol jolting, each 25ml, merge extractive liquid,, the water 30ml washing that the reuse n-butyl alcohol is saturated discards water liquid, n-butyl alcohol liquid evaporate to dryness, residue adds methanol 1ml makes dissolving, makes need testing solution; Extracting liquorice control medicinal material 0.5g adds methanol 40ml, supersound process 30 minutes in addition, filter, filtrate evaporate to dryness, residue add water 20ml makes dissolving, extract 2 times with water saturated n-butyl alcohol jolting, each 25ml, merge extractive liquid,, the water 30ml washing that the reuse n-butyl alcohol is saturated, discard water liquid, n-butyl alcohol liquid evaporate to dryness, residue add methanol 1ml makes dissolving, makes control medicinal material solution;
In the step f), the method preparation of described reference substance solution by may further comprise the steps: described extracting liquorice acid ammonium reference substance is an amount of, accurately claims surely, adds 70% and adds ethanol and make the solution that every 1ml contains ammonium glycyrrhizinate 10 μ g respectively, namely; Wherein, the method preparation of described need testing solution by may further comprise the steps: get this product 2.0g, the accurate title, decide, put in the tool plug conical flask accurate 70% alcoholic solution 100ml, the close plug of adding, claim to decide weight, supersound process 30 minutes is put cold, claim to decide weight again, supply the weight that subtracts mistake with 70% ethanol, shake up, filter, get subsequent filtrate, namely; Preferably, the power of described supersound process is 240W, and frequency is 45kHZ.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103432386A (en) * | 2013-08-19 | 2013-12-11 | 湖北丽益医药科技有限公司 | Chinese traditional medicine preparation for treating coughs and preparation method of same |
| CN104483408A (en) * | 2014-12-19 | 2015-04-01 | 王保安 | Detection method of traditional Chinese medicine preparation Xinsuning capsule |
| CN105477311A (en) * | 2015-12-23 | 2016-04-13 | 北京世纪合辉医药科技股份有限公司 | Health product for improving immunity and preparation method of health product |
| CN108096455A (en) * | 2017-12-25 | 2018-06-01 | 武汉市华本汇医药发展有限公司 | A kind of preparation method of radix adenophorea, tuber of dwarf lilyturf particle |
| CN108387655A (en) * | 2018-02-11 | 2018-08-10 | 四川省食品药品检验检测院 | A method of for detecting persticide residue in Radix Ophiopogonis |
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-
2013
- 2013-04-19 CN CN201310139316.4A patent/CN103230517B/en active Active
Non-Patent Citations (4)
| Title |
|---|
| 傅良杰: "中西医结合治疗组织细胞坏死性淋巴结炎38例", 《现代中西医结合杂志》, vol. 14, no. 21, 30 November 2005 (2005-11-30), pages 2837 - 2838 * |
| 刘建汉等: "益气养阴方合孟鲁司特纳治疗咳嗽变异性哮喘合并变应性鼻炎", 《湖北中医杂志》, vol. 33, no. 08, 31 August 2011 (2011-08-31), pages 43 - 44 * |
| 国家药典委员会编: "《中华人民共和国药典2010年版一部》", 31 January 2010, article "养阴生血合剂", pages: 948 - 1060-1061 * |
| 曹西华等: "沙参麦冬汤对大鼠慢性胃粘膜损伤的保护作用", 《中国中西医结合杂志1996年基础理论研究特辑》, 31 December 1996 (1996-12-31), pages 141 - 144 * |
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| CN103432386A (en) * | 2013-08-19 | 2013-12-11 | 湖北丽益医药科技有限公司 | Chinese traditional medicine preparation for treating coughs and preparation method of same |
| CN103432386B (en) * | 2013-08-19 | 2015-09-30 | 湖北丽益医药科技有限公司 | A kind of Chinese medicine preparation for the treatment of cough and preparation method thereof |
| CN104483408A (en) * | 2014-12-19 | 2015-04-01 | 王保安 | Detection method of traditional Chinese medicine preparation Xinsuning capsule |
| CN105477311A (en) * | 2015-12-23 | 2016-04-13 | 北京世纪合辉医药科技股份有限公司 | Health product for improving immunity and preparation method of health product |
| CN108096455A (en) * | 2017-12-25 | 2018-06-01 | 武汉市华本汇医药发展有限公司 | A kind of preparation method of radix adenophorea, tuber of dwarf lilyturf particle |
| CN108096455B (en) * | 2017-12-25 | 2020-12-04 | 武汉市华本汇医药发展有限公司 | Preparation method of radix adenophorae and radix ophiopogonis granules |
| CN108387655A (en) * | 2018-02-11 | 2018-08-10 | 四川省食品药品检验检测院 | A method of for detecting persticide residue in Radix Ophiopogonis |
| CN115343383A (en) * | 2022-07-18 | 2022-11-15 | 神威药业集团有限公司 | Method for measuring content of 8 chemical components in adenophora stricta and ophiopogon japonicus decoction |
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