CN103230517B - A kind of decoction made from radix adenophorea, tuber of dwarf lilyturf granule and preparation method thereof and detection method - Google Patents
A kind of decoction made from radix adenophorea, tuber of dwarf lilyturf granule and preparation method thereof and detection method Download PDFInfo
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Abstract
The invention provides a kind of decoction made from radix adenophorea, tuber of dwarf lilyturf granule and preparation method thereof and detection method, described granule comprises the Radix Glehniae of mass ratio 0.5 ~ 2:0.5 ~ 2:0.5 ~ 2:1 ~ 3:0.5 ~ 2:0.1 ~ 1.2:0.1 ~ 1, Rhizoma Polygonati Odorati, Radix Ophiopogonis, Radix Trichosanthis, Seem Lablab Album, Folium Mori and Radix Glycyrrhizae seven taste raw material, described raw material soaks through several times, decoct, filter and merging filtrate, be condensed into clear paste, granule is made in drying, both; Its detection method, comprises the following steps: identify described decoction made from radix adenophorea, tuber of dwarf lilyturf granule by thin layer chromatography; The Organochlorine Pesticide Residues content in described decoction made from radix adenophorea, tuber of dwarf lilyturf granule is measured by persticide residue algoscopy; The content of beary metal in described decoction made from radix adenophorea, tuber of dwarf lilyturf granule is measured by Residue on ignition check method; The extract content of described decoction made from radix adenophorea, tuber of dwarf lilyturf granule is measured by hot dipping; By the content of material in decoction made from radix adenophorea, tuber of dwarf lilyturf granule described in high effective liquid chromatography for measuring.
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, particularly relate 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.Main Radix Adenophorae (Radix Glehniae) in side, supports 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 using with the middle medicine as double system.Finally quote the hardship of Folium Mori and light lung qi dispersing heat, and with the sweet of Radix Glycyrrhizae born fluid.Body fluid is raw, scorchingly removes, and respectively demonstrate,proves spontaneous recovery.
The research of decoction made from radix adenophorea, tuber of dwarf lilyturf modern pharmacology and clinical research show, decoction made from radix adenophorea, tuber of dwarf lilyturf has antibacterial, antiinflammatory, eliminates the phlegm, antiallergic, strengthen immunologic function and improve 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 the immunoreation of anaphylaxis and suppression macrophage.
4. strengthen immunologic function: Folium Mori can improve the phagocytic function of macrophage, make eosinophilia.
5. improve hypoxia-bearing capability: Radix Ophiopogonis, Rhizoma Polygonati Odorati all obviously can extend the time of mice anoxia enduring.
Comprehensive ancient literature and modern pharmacology known, the party's clinical application range is wide.
Chinese medicinal granule is under guidance of traditional Chinese medicine theory, with the prepared slices of Chinese crude drugs of specification Preparation process for raw material, adopts the 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 what can be used as again Chinese medicine preparation supplies the raw material of industry, also for tcm clinical practice medication provides new approach.Compared with traditional Chinese herbs decoction, the advantage of Compatible Granule keeps the nature and flavor feature of original Chinese medicine, remain the characteristic of differentiation of tcm, rational production technology is developed according to the character of Chinese medicine, formulate advanced feasible quality control standard, be processed into as regulation and standardization, industrialized modern Chinese medicine preparation.Overcome Chinese medicine decoction decoct time-consuming, take inconvenience, technique extensive, lack the drawbacks such as quality control, adapted to the demand of modern social development.
In clinical practice, Chinese medicinal granule can in strict accordance with the genuine high-quality medical material of standard application, control prepared slice quality, contribute to the management level improving Chinese medicine quality, can overcome due to medical material home environment, natural conditions, gather, the prepared slices of Chinese crude drugs inherent quality of the many factors such as processing method, storage, decoction pieces Processing methods technique, guarantee clinical efficacy; The difference of the clinical efficacy caused due to About The Quality of Sliced Herbal Medicine disunity can be reduced.More traditional family decocts decoction pieces, Chinese medicinal granule overcome in traditional decoction pieces decoction process be decocted first, rear under, decoct a drug wrapped and decoct the difficult problems such as container is lack of standardization, to guarantee and stable clinical efficacy has obvious advantage.Chinese medicinal granule adopt aluminium foil bag or other pack easily, dosage is accurate, avoid commonly in the storage of Chinese medicine decoction pieces to go rancid, variable color, damage by worms, the difficult problem such as to go mouldy, be convenient to medicament storage and patient portably uses, patient eliminates the trouble of decoction on using, even if go on business, travel, also can not therapy discontinued.Be conducive to expanding foreign market Chinese medicinal granule in production and processing overall process, implement GMP monitoring, each kind establishes respective production and quality management file respectively from the links of raw material, intermediate, semi-finished product, finished product, and according to standard operation, be conducive to promoting internationalization of tcm.
The Chinese medicinal granule of current application is greatly mainly with the single medicinal material decoction pieces granule that single medicinal material is made by modern pharmaceutical technique, and existing hundreds of single decoction pieces granule goes on the market.Although but Chinese medicinal granule has lot of advantages, in making and clinical practice, also there is many drawbacks, with traditional in the principal mode Chinese medicine decoction of medical drugs still there is certain gap.Chinese medicine decoction is that compound compatibility is decocted and formed, the not simple addition of the chemical composition 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 composition.Chinese medicine is many containing pigment, polysaccharide, protein, lipid, tannin, flavonoid, Coumarins, lignanoids, Anthraquinones, glycoside, organic acid, alkaloids, terpenoid and derivant thereof, closing at prescription decocts in process, both each ingredient solubility may directly be affected, also can by change solvent such as pH value, viscosity and dissolubility and solute such as optical activity, charge, osmotic pressure, relative molecular weight, degree of hydration etc. properties affect its dissolve, or act on mutually with other solutes and cause water miscible increase and decrease.These effects comprise generation hydrotropy effect, change dissolution with solvents characteristic, change solution ph, change material weak electrolyte ionization degree, generate the new component of high-dissolvability, generate the new component of low solubility, there is precipitation, generate complex, inorganic ions is combined the salt generating and be insoluble in water with Chinese medicine ingredients, generate noval chemical compound and play a role combining of various effect, single granule mixed dissolution is caused not have whole effective ingredient of " group's medicine is decocted altogether ", the granule prepared by existing technique in other words can not comprise the effective ingredient of middle medical drugs requirement completely, traditional prescription working substance basis is caused to change, so that existing granule medication can not be equal to traditional Chinese medicine decoction.
" decoct " this important step altogether owing to have ignored group medicine, ignore the globality of Chinese medicine decoction, finally may cause the change of clinical efficacy or the change of pharmacological action.Some patients are reflected that the flavour of a drug of Chinese medicinal granule are partially more bitter than traditional decoction, are laid particular stress on, and 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, its composition extracted is higher relative to decoction content, and consequent various side effect also can not be ignored.
Therefore, solve current single medicinal material granule Problems existing, give full play to the advantage of traditional compatibility of medicines in a prescription, reach attenuation synergistic, particularly necessary.Chinese medicine compound granule has passed on the advantage of Chinese medicine single granule, take into full account that again decoction pieces is decocting the interaction in (or other processing) process, the medication of traditional Chinese medical science tradition is more met theoretical than single granule, also possess other advantage of granule simultaneously, there is larger value.
Along with modernization of Chinese medicine development and Chinese medicine move towards the needs of international market, in order to ensure the quality controllable of tcm product, setting up quality standard and having very important significance.But decoction made from radix adenophorea, tuber of dwarf lilyturf granule there is no detection method at present at present, be unfavorable for the control of technique and the monitoring of medicine in production.
Summary of the invention
Therefore, the object of the invention is the deficiency for being simply added when single decoction pieces granule is taken in 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 specifically stated otherwise, " this product " herein all refers to " decoction made from radix adenophorea, tuber of dwarf lilyturf granule ".
Unless specifically stated otherwise, " Gamma Hexaochlorocyclohexane " herein all refers to " benzene hexachloride ".
Unless specifically stated otherwise, " clofenotane " herein all refers to " biconjugate chlorphenyl trichloroethane ".
Unless stated otherwise, the hot dipping under involved herein thin layer chromatography, high performance liquid chromatography and ethanol-soluble extractives algoscopy item is all carry out according to test method described in Chinese Pharmacopoeia version in 2010.
Unless specifically stated otherwise, involved 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 the Radix Glehniae of mass ratio 0.5 ~ 2:0.5 ~ 2:0.5 ~ 2:1 ~ 3:0.5 ~ 2:0.1 ~ 1.2:0.1 ~ 1, Rhizoma Polygonati Odorati, Radix Ophiopogonis, Radix Trichosanthis, Seem Lablab Album, Folium Mori and Radix Glycyrrhizae seven taste raw material, described raw material soaks through several times, decoct, filter and merging filtrate, be condensed into clear paste, granule is made in drying, both; Preferably, the mass ratio of Radix Glehniae, Rhizoma Polygonati Odorati, Radix Ophiopogonis, Radix Trichosanthis, Seem Lablab Album, Folium Mori and Radix Glycyrrhizae seven taste raw material 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 taste raw material is 1:1:1:1.5:1:0.6:0.3.
The mass ratio of described raw material and described obtained granule is 5 ~ 6:1 ~ 2, and preferably, the mass ratio of described raw material and described obtained granule is 5.12:1.
On the other hand, the invention provides a kind of preparation method of radix adenophorea, tuber of dwarf lilyturf granule, said method comprising the steps of:
1) Radix Glehniae of mass ratio 0.5 ~ 2:0.5 ~ 2:0.5 ~ 2:1 ~ 3:0.5 ~ 2:0.1 ~ 1.2:0.1 ~ 1, Rhizoma Polygonati Odorati, Radix Ophiopogonis, Radix Trichosanthis, Seem Lablab Album, Folium Mori and Radix Glycyrrhizae seven taste raw material is taken; Preferably, the mass ratio of Radix Glehniae, Rhizoma Polygonati Odorati, Radix Ophiopogonis, Radix Trichosanthis, Seem Lablab Album, Folium Mori and Radix Glycyrrhizae seven taste raw material 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 taste raw material is 1:1:1:1.5:1:0.6:0.3;
2) described raw material is through soaking, decocting, filter and merging filtrate;
3) by described filtrate simmer down to clear paste;
4) granule is made by adding adjuvant after described clear paste drying, both.
Wherein, step 2) described in the amount of water that soaks be 6 ~ 10 weight portions of raw material, preferably 8 weight portions, described soak time is 1 ~ 2 hour, preferably 1 hour;
Described decoction is carried out at twice, and decocting time is 1 ~ 2 hour for the first time, preferably 2 hours; Second time decocts 6 ~ 10 weight portions that amount of water is raw material, preferably 6 weight portions, and described decocting time is 1-2 hour, preferably 1 hour;
The clear paste of relative density 1.08 ~ 1.18 during the simmer down to of filtrate described in step 3) 60 DEG C; Preferably, during the simmer down to of filtrate described in step 3) 60 DEG C, relative density relative density is the clear paste of 1.14.
Preferably, described simmer down to concentrating under reduced pressure.
Preferably, described drying is spraying dry.
Preferably, described spray-dired inlet temperature is 154 DEG C, and leaving air temp is 95 DEG C.
Right-hand member, described adjuvant is pharmaceutically acceptable carrier or excipient.
Preferably, after described step 4) makes granule, subpackage obtains finished product.
Again 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:
A): qualitative detection composition Radix Ophiopogonis; Wherein, described qualitative detection is undertaken by thin layer chromatography; Wherein, test sample is decoction made from radix adenophorea, tuber of dwarf lilyturf granule, and control medicinal material is Radix Ophiopogonis;
B): qualitative detection licorice ingredient; Wherein, described qualitative detection is undertaken by thin layer chromatography; Wherein, test sample is decoction made from radix adenophorea, tuber of dwarf lilyturf granule, and control medicinal material is Radix Glycyrrhizae;
C): measure the content of beary metal in described decoction made from radix adenophorea, tuber of dwarf lilyturf granule by Residue on ignition check method;
D): measure the Organochlorine Pesticide Residues content in described decoction made from radix adenophorea, tuber of dwarf lilyturf granule by persticide residue algoscopy;
E): detect extract content by ethanol-soluble extractives hot dipping algoscopy;
F): by the content of material in decoction made from radix adenophorea, tuber of dwarf lilyturf granule described in high effective liquid chromatography for measuring.
Preferably, in step a), described test sample and control medicinal material, respectively by chloroform extraction process, obtain residue by after chloroform evaporate to dryness, add ethanol to dissolving, with obtained need testing solution and control medicinal material solution in residue;
In step a), developing solvent is chloroform-acetone; Developer is the ethanol solution of sulfuric acid of volume ratio 10%;
In step b), described test sample and control medicinal material are respectively by adding methanol, supersound process, filtration treatment, after filtrate water is dissolved, use n-butanol extraction, again with the washing of n-butyl alcohol saturation water, abandon water liquid and by after n-butyl alcohol evaporate to dryness, in residue, add methanol to dissolving, with obtained need testing solution and control medicinal material solution;
In step b), developing solvent is acetic ether-methanoic acid-glacial acetic acid-water; Developer is the ethanol solution of sulfuric acid of volume ratio 10%;
In step c), the content of beary metal≤25ppm recorded;
Steps d) in, 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 comprised the following steps:
1) carrying out chromatographic condition and system suitability test, is wherein filler with octadecylsilane chemically bonded silica; Take methanol as mobile phase A, with 0.2mol/L ammonium acetate 2% acetic acid solution for Mobile phase B (58:42), determined wavelength is 237nm, and number of theoretical plate calculates should be not less than 5000 by ammonium glycyrrhizinate peak;
2) prepare 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 obtained result.
More preferably, in step a), described need testing solution and control medicinal material solution are obtained by following steps: get test sample 1g, add water 15mL, add hydrochloric acid 0.5ml, to put in water-bath reflux 10 minutes, let cool, extract with chloroform 20ml jolting, divide and get chloroform liquid, evaporate to dryness, residue adds ethanol 1ml makes dissolving, makes need testing solution; Separately get control medicinal material 1g Radix Ophiopogonis, add water 20ml, decocts 10 minutes, filters, filtrate adds hydrochloric acid 0.5ml, to put in water-bath reflux 10 minutes, lets cool, extract with chloroform 20ml jolting, divide and get chloroform liquid, evaporate to dryness, residue adds ethanol 1ml makes dissolving, makes control medicinal material solution;
In step b), described need testing solution and control medicinal material solution are obtained by following steps: get test sample 0.5g, add methanol 40ml, supersound process 30 minutes, filters, filtrate evaporate to dryness, the residue 20ml that adds water makes dissolving, extracts 2 times, each 25ml with water saturated n-butyl alcohol jolting, merge extractive liquid, wash with the water 30ml that n-butyl alcohol is saturated again, discard water liquid, n-butyl alcohol liquid evaporate to dryness, residue adds methanol 1ml makes dissolving, makes need testing solution;
Another extracting liquorice control medicinal material 0.5g, adds methanol 40ml, supersound process 30 minutes, filter, filtrate evaporate to dryness, the residue 20ml that adds water makes dissolving, 2 times are extracted with water saturated n-butyl alcohol jolting, each 25ml, merge extractive liquid, then wash with the water 30ml that n-butyl alcohol is saturated, discard water liquid, n-butyl alcohol liquid evaporate to dryness, residue adds methanol 1ml makes dissolving, makes control medicinal material solution;
In step f), described reference substance solution is by the preparation of the method that comprises the following steps: described extracting liquorice acid ammonium reference substance is appropriate, accurately weighed, adds 70% and adds ethanol and make the solution of every 1ml containing ammonium glycyrrhizinate 10 μ g respectively, to obtain final product;
In step f), the method preparation of described need testing solution by comprising the following steps: get this product 2.0g, accurately weighed, put in tool plug conical flask, precision adds 70% alcoholic solution 100ml, close plug, weighed weight, supersound process 30 minutes, lets cool, weighed weight again, supply the weight of less loss with 70% ethanol, shake up, filter, get subsequent filtrate, to obtain final product;
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 100mg be less than.
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.Therefore this granule function is described as promoting production of body fluid with drugs sweet in flavor and cold in nature with curing mainly, clearly support lung stomach.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 traditionally closes and decocts, and gives full play to the advantage of drug matching, embodies Chinese medicine organic conception, guarantees that it reaches the object of attenuation synergistic, overcomes each flavour of a drug when current single granule is taken and is simply added the deficiency brought;
(2) detection method providing decoction made from radix adenophorea, tuber of dwarf lilyturf granule of knowing clearly perfect, effectively can control the quality of this granule, with better Instructing manufacture, make controlling of production process more rationally strict, in process of producing product, effectively can control the quality of product, thus guarantee clinical efficacy and the safety of decoction made from radix adenophorea, tuber of dwarf lilyturf granule.
(3) decoction made from radix adenophorea, tuber of dwarf lilyturf granule is convenient to medicament storage and patient portably uses, and patient eliminates the trouble of decoction on using; Granule preparation is simple, and meet Chinese medicine Medicinal Trait, quality is certainly controlled, portably uses conveniently, meets the requirement of modern people to medicine " three is little ", " triple effect " and " five convenience ".
(4) greater significance is had to the modernization of promotion Chinese Traditional Medicine.
This invention is with a wide range of applications.
Accompanying drawing explanation
Below, describe embodiment of the present invention in detail by reference to the accompanying drawings, 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 differentiated the Radix Ophiopogonis of decoction made from radix adenophorea, tuber of dwarf lilyturf granule of the present invention; In 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, and 3 is negative control solution;
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; In 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, and 5-6 is negative control solution;
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 linear relationship chart of ammonium glycyrrhizinate sample size in decoction made from radix adenophorea, tuber of dwarf lilyturf granule of the present invention and peak area.
Detailed description of the invention
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 meets " Chinese Pharmacopoeia " each decoction pieces of version in 2010, is provided by Kangmei Pharmaceutical Co., Ltd, and source and the place of production are in table 1.
Table 1 crude drug source table
1.2 instrument and equipment
B-290 type spraying dry instrument, Bu Qi company of Switzerland;
RE-5205 type Rotary Evaporators, Shanghai Yarong Biochemical Instrument Plant.
2. pair decoction made from radix adenophorea, tuber of dwarf lilyturf soup formula granule Study on extraction is as follows:
Influence factor has: extraction time, extraction time, amount of water (all representing by the times amount of quality of medicinal material).Adopt orthogonal test Optimized extraction techniques, select L
9(3
4) orthogonal table, above-mentioned three factors of high spot reviews, with the content of ammonium glycyrrhizinate for inspection target, factor level table is in table 2
Table 2
Test method: take Radix Glehniae 50g in prescription ratio, Rhizoma Polygonati Odorati 50g, Radix Ophiopogonis 50g, Radix Trichosanthis 75g, Seem Lablab Album 50g, Folium Mori 30g, Radix Glycyrrhizae 15g, numbering 1 ~ 9, by L
9(3
4) orthogonal table arrangement test, result of the test is in 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 | 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 | 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 |
Find out from table 4 and table 5, with the yield of the content of ammonium glycyrrhizinate and spray drying powder for index analysis, each factor does not make significant difference, and Optimizing Technical is: A
2b
1c
2; Comprehensive above-mentioned analysis of experiments, reduces the angle of energy consumption from industrialized great production, under ensureing the prerequisite of effective component content, amount of water is changed into first time 8 times amount, second time 6 times amount.
the preparation of embodiment 2 decoction made from radix adenophorea, tuber of dwarf lilyturf granule
Take Radix Glehniae 50g in prescription ratio, Rhizoma Polygonati Odorati 50g, Radix Ophiopogonis 50g, Radix Trichosanthis 75g, Seem Lablab Album 50g, Folium Mori 30g, Radix Glycyrrhizae 15g water soaking 1h, decoct secondary, 8 times amount that add water for the first time decoct 2 hours, and second time adds 6 times amount soak by water 1 hour, filter, merging filtrate, 80 DEG C of concentrating under reduced pressure, be concentrated into the clear paste of relative density 1.14 (60 DEG C), spraying dry, inlet temperature is 154 DEG C, leaving air temp 95 DEG C, revolution speed 25%, dry dry extract.Repeat six times by same method, obtained dry extract the results are shown in Table 6
Table 6 dry extract yield and character
This method yield is high, process stabilizing, and is loyal to former side's method for making.
And be yellowish-brown granule according to the decoction made from radix adenophorea, tuber of dwarf lilyturf granule that 6 batch samples are described as obtaining 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 granule
Take Radix Glehniae 50g in prescription ratio, Rhizoma Polygonati Odorati 50g, Radix Ophiopogonis 50g, Radix Trichosanthis 75g, Seem Lablab Album 50g, Folium Mori 30g, Radix Glycyrrhizae 15g water soaking 1h, decocts secondary, 8 times amount that add water for the first time decoct 2 hours, and second time adds 6 times amount soak by water 1 hour, filter, merging filtrate, 80 DEG C of concentrating under reduced pressure, are concentrated into the clear paste of relative density 1.08-1.18 (60 DEG C), spraying dry, inlet temperature is 154 DEG C, leaving air temp 95 DEG C, revolution speed 25%, dry dry extract, granulates cream powder, both.
the preparation of embodiment 4 decoction made from radix adenophorea, tuber of dwarf lilyturf granule
Take Radix Glehniae 50g in prescription ratio, Rhizoma Polygonati Odorati 50g, Radix Ophiopogonis 50g, Radix Trichosanthis 62.5g, Seem Lablab Album 50g, Folium Mori 50g, Radix Glycyrrhizae 50g water soaking 5h, decoct secondary, 6 times amount that add water for the first time decoct 2 hours, and second time adds 10 times amount soak by water 1 hour, filter, merging filtrate, 80 DEG C of concentrating under reduced pressure, be concentrated into the clear paste of relative density 1.14 (60 DEG C), spraying dry, inlet temperature is 154 DEG C, leaving air temp 95 DEG C, revolution speed 25%, dry dry extract.
the preparation of embodiment 5 decoction made from radix adenophorea, tuber of dwarf lilyturf granule
Take Radix Glehniae 50g in prescription ratio, Rhizoma Polygonati Odorati 50g, Radix Ophiopogonis 50g, Radix Trichosanthis 100g, Seem Lablab Album 50g, Folium Mori 5g, Radix Glycyrrhizae 5g water soaking 1h, decoct secondary, 10 times amount that add water for the first time decoct 2 hours, and second time adds 8 times amount soak by water 1 hour, filter, merging filtrate, 80 DEG C of concentrating under reduced pressure, be concentrated into the clear paste of relative density 1.14 (60 DEG C), spraying dry, inlet temperature is 154 DEG C, leaving air temp 95 DEG C, revolution speed 25%, dry dry extract.
the preparation of embodiment 6 decoction made from radix adenophorea, tuber of dwarf lilyturf granule
Take Radix Glehniae 50g in prescription ratio, Rhizoma Polygonati Odorati 50g, Radix Ophiopogonis 50g, Radix Trichosanthis 75g, Seem Lablab Album 50g, Folium Mori 30g, Radix Glycyrrhizae 25g water soaking 1h, decoct secondary, 8 times amount that add water for the first time decoct 2 hours, and second time adds 6 times amount soak by water 1 hour, filter, merging filtrate, 80 DEG C of concentrating under reduced pressure, be concentrated into the clear paste of relative density 1.14 (60 DEG C), spraying dry, inlet temperature is 154 DEG C, leaving air temp 95 DEG C, revolution speed 25%, dry dry extract.
the decoction made from radix adenophorea, tuber of dwarf lilyturf granule that embodiment 7 thin layer chromatography qualification embodiment 2 is obtained
Differentiate that item is formulated with reference to " Chinese Pharmacopoeia " version in 2010 " yin nourishing Shengxue Heji ", " stomach nourishing granule ", " SUNJU GANMAO PIAN ", and 20121101 batch sample differentiated, be described as follows:
1, reagent and reagent
Radix Ophiopogonis control medicinal material: lot number is 1201013-200607, is purchased from Nat'l Pharmaceutical & Biological Products Control Institute;
Radix Glycyrrhizae control medicinal material: lot number is 120904-200511, is purchased from 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) differentiate Radix Ophiopogonis
Prepared by test sample: get this product 0.9g, the 15ml that adds water dissolves, and adds hydrochloric acid 0.5ml, and in water-bath, reflux 10 minutes, lets cool, and extracts with chloroform 20ml jolting, and divide and get chloroform liquid, evaporate to dryness, residue adds ethanol 1ml makes dissolving, as need testing solution.
Prepared by control medicinal material: get control medicinal material 1g Radix Ophiopogonis, be made in the same way of control medicinal material solution.
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, dries;
Develop the color and inspect: spraying with 10% ethanol solution of sulfuric acid, be heated to spot development at 105 DEG C clear.
Result: control medicinal material characteristic point is unintelligible, 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
Prepared by test sample: get this product 0.5g, add methanol 40ml, supersound process 30 minutes, filters, filtrate evaporate to dryness, and the residue 20ml that adds water makes dissolving, extracts 2 times, each 25ml, merge extractive liquid, then wash with the water 30ml that n-butyl alcohol is saturated with water saturated n-butyl alcohol jolting.Discard water liquid, n-butyl alcohol liquid evaporate to dryness, residue adds methanol 1ml makes dissolving, as need testing solution;
Prepared by control medicinal material solution: extracting liquorice control medicinal material 0.5g, is made in the same way of control medicinal material solution;
Negative control: manufacture the decoction made from radix adenophorea, tuber of dwarf lilyturf control sample lacking Radix Glycyrrhizae.Made by oneself by Kang Mei drug research institute.
Lamellae: silica gel G thin layer version prepared by 1% sodium hydroxide solution;
Point sample amount: each 5 μ l;
Point sample mode: spot application;
Developing solvent: acetic ether-methanoic acid-glacial acetic acid-water (15: 1: 1: 2) is developing solvent, is expanded to about 12cm, takes out, dries;
Develop the color and inspect: spraying with 10% ethanol solution of sulfuric acid, be heated to spot development at 105 DEG C clear, the results are shown in Figure 3.
embodiment 8 measures the content of beary metal of the obtained decoction made from radix adenophorea, tuber of dwarf lilyturf granule of embodiment 2
With reference under " Chinese Pharmacopoeia " version in 2010 coptos bolus for clearing the upper heat [inspection] item, check that the method for heavy metal is formulated, to this product sample, (lot number: 20121101) check, result conforms with the regulations.
embodiment 9 measures the Organochlorine Pesticide Residues of the obtained decoction made from radix adenophorea, tuber of dwarf lilyturf granule of embodiment 2
content
With reference under " Chinese Pharmacopoeia " version in 2010 annex Ⅸ Q organic chlorine agriculture chemicals residues detecton method and " Chinese Pharmacopoeia " version in 2010 Radix Glycyrrhizae [inspection] item, check that the method for Residual Levels of Organochlorine Pesticides is formulated, to this product sample, (lot number: 20121101) check, result conforms with the regulations.
embodiment 10 measures other of the obtained decoction made from radix adenophorea, tuber of dwarf lilyturf granule of embodiment 2
Specify with reference under " Chinese Pharmacopoeia " version in 2010 annex I C granule item, to this product sample, (lot number: [granularity], [moisture], [melting] 20121101), [content uniformity], [microbial limit] check, result is above-mentioned everyly all to conform with the regulations.
embodiment 11 measures the extractum of the obtained decoction made from radix adenophorea, tuber of dwarf lilyturf granule of embodiment 2
Get this product sample (lot number: 20121101) powder 2g, accurately weighed, precision adds ethanol 50ml, the accurately weighed weight of tool plug, leaves standstill 1 hour, connects condensing tube, be heated to boiling, and keep micro-and boil 1 hour, after letting cool, take off conical flask, close plug, weigh again, supply the weight of less loss with ethanol, shake up, filter with dry filter, precision measures subsequent filtrate 25ml, puts and is dried in the evaporating dish of constant weight, in water-bath after evaporate to dryness, in 105 DEG C of dryings 3 hours, put in exsiccator, cool 30 minutes, rapid accurately weighed weight.
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 granule
Character: yellowish-brown granule; Feeble QI, bitter in the mouth.
1. instrument and reagent
1.1 instruments: high performance liquid chromatograph: waterse, Empower chem workstation; Chromatographic column: Water-C
18(4.6mm × 250mm, 5 μm); Electronic analytical balance: FA2104, XP6; Ultrasonic cleaning instrument: (KQ-300VDB).
1.2 reagent: methanol is chromatographically pure, water is ultra-pure water, and other reagent are analytical pure.
1.3 reagents: 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: take octadecylsilane chemically bonded silica as filler; Take methanol as mobile phase A, with 0.2mol/L ammonium acetate, 2% acetic acid is Mobile phase B, and the volume ratio of A:B is 58:42, and determined wavelength is 237nm, and number of theoretical plate calculates should be not less than 5000 by ammonium glycyrrhizinate peak.
3. the preparation of solution
The preparation of 3.1 reference substance solution: precision takes, ammonium glycyrrhizinate 1.060mg, 1.020mg puts in 20ml volumetric flask respectively, add 70% dissolve with ethanol and be diluted to scale, shake up, measure 5ml again to put in 25ml volumetric flask and add the ethanol dilution of 70% to scale, obtain reference substance solution (every 1ml is containing ammonium glycyrrhizinate 10.6 μ g, 10.2 μ g).
The preparation of 3.2 need testing solutions: get this product 2.0g, accurately weighed, put in tool plug conical flask, precision adds volume fraction 70% alcoholic solution 100ml, close plug, weighed weight, power 240W, frequency 45kHz supersound process 30 minutes, lets cool, more weighed weight, the weight of less loss is supplied with volume fraction 70% alcoholic solution, shake up, filter, to obtain final product.
4. Method validation
4.1 accuracy test
Get this product 6 parts, accurately weighed, put in tool plug conical flask, precision adds volume fraction 70% alcoholic solution 100ml, and adding concentration is the close plug of 0.5030mg/ml reference substance, weighed weight, supersound process (power 240W, frequency 45kHz) 30 minutes, let cool, more weighed weight, the weight of less loss is supplied with volume fraction 70% alcoholic solution, shake up, filter, to obtain final product.: take octadecylsilane chemically bonded silica as filler; Take methanol as mobile phase A, with 0.2mol/L ammonium acetate, 2% acetic acid is Mobile phase B, and the volume ratio of A:B is 58:42, and determined wavelength is 237nm sample introduction,
Table 8
4.2 precision test
4.2.1 replica test
Get this product 6 parts, accurately weighed, put in tool plug conical flask, precision adds volume fraction 70% alcoholic solution 100ml, close plug, weighed weight, power 240W, frequency 45kHz supersound process 30 minutes, lets cool, more weighed weight, the weight of less loss is supplied with volume fraction 70% alcoholic solution, shake up, filter, to obtain final product.By above-mentioned chromatographic condition, repeat sample introduction 6 times, 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, accurately weighed, put in tool plug conical flask, precision adds volume fraction 70% alcoholic solution 100ml, close plug, weighed weight, power 240W, frequency 45kHz supersound process 30 minutes, lets cool, more weighed weight, the weight of less loss is supplied with volume fraction 70% alcoholic solution, shake up, filter, to obtain final product.By above-mentioned chromatographic condition, repeat sample introduction 6 times, 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 tests
Get this product 2.0015g, Radix Glycyrrhizae negative sample 2.1026g, accurately weighed, put in tool plug conical flask, precision adds volume fraction 70% alcoholic solution 100ml, close plug, weighed weight, power 240W, frequency 45kHz supersound process 30 minutes, lets cool, more weighed weight, the weight of less loss is supplied with volume fraction 70% alcoholic solution, shake up, filter, to obtain final product.
Get blank solvent (methanol), sample solution, Radix Glycyrrhizae negative sample solution and ammonium glycyrrhizinate reference substance solution to measure by method under assay item.From collection of illustrative plates, sample collection of illustrative plates is having corresponding chromatographic peak with ammonium glycyrrhizinate reference substance collection of illustrative plates identical retention time place, and without corresponding chromatographic peak in blank solvent and negative sample solution, therefore, this content method specificity is good.Chromatogram is shown in Fig. 4 a-4d:
4.4 linear relationship
Above-mentioned ammonium glycyrrhizinate reference substance solution 2,5,10,15, the 20 μ l of accurate absorption, measure peak area by above-mentioned chromatographic condition, carry out regression treatment with integrating peak areas value to peoniflorin concentration, regression equation is y=805858x-12438, r=0.9999
Peak area 2000201591671167897288229610
Sample size 0.2650.2120.1590.1060.053
4.5 stability test
(lot number: 20121101) test liquid, by above-mentioned chromatographic condition, respectively at 0,2,4,6,8,12 hour sample introduction, measures ammonium glycyrrhizinate reference substance peak area to get same radix adenophorea, tuber of dwarf lilyturf granule.The results are shown in Table 6-7, result shows that ammonium glycyrrhizinate is stable in 12 hours.
Table 12 stability test result (ammonium glycyrrhizinate)
5. sample size measures
Get radix adenophorea, tuber of dwarf lilyturf granule, measuring by drafting content assaying method, recording ammonium glycyrrhizinate (C
21h
22o
9) containing scale 8.
Table 13 sample size measurement result
6. the determination of content limit
Content limit calculates by 80% of measurement result because every packed 5g, therefore tentative content limit be every bag containing Radix Glycyrrhizae with glycyrrhizic acid (C
21h
22o
9) meter, must not 144mg be less than.
Claims (11)
1. a preparation method for decoction made from radix adenophorea, tuber of dwarf lilyturf granule, said method comprising the steps of:
1) Radix Glehniae of mass ratio 0.5 ~ 2:0.5 ~ 2:0.5 ~ 2:1 ~ 3:0.5 ~ 2:0.1 ~ 1.2:0.1 ~ 1, Rhizoma Polygonati Odorati, Radix Ophiopogonis, Radix Trichosanthis, Seem Lablab Album, Folium Mori and Radix Glycyrrhizae seven taste raw material is taken;
2) described raw material is through soaking, decocting, filter and merging filtrate;
Wherein, the amount of water of described immersion is 8 times of raw material gross weight, and soak time is 1 hour;
Described decoction is carried out at twice, and decocting time is 2 hours for the first time; Second time decocts 6 times that amount of water is raw material gross weight, and described decocting time is 1 hour;
3) by described filtrate simmer down to clear paste;
Wherein, during described filtrate simmer down to 60 DEG C, relative density is 1.08 ~ 1.18;
4) described clear paste drying is added adjuvant and make granule, to obtain final product.
2. the preparation method of decoction made from radix adenophorea, tuber of dwarf lilyturf granule according to claim 1, it is characterized in that, described step 1) in, the mass ratio of Radix Glehniae, Rhizoma Polygonati Odorati, Radix Ophiopogonis, Radix Trichosanthis, Seem Lablab Album, Folium Mori and Radix Glycyrrhizae seven taste raw material is 1 ~ 2:1 ~ 2:1 ~ 2:1.5 ~ 2.5:1 ~ 2:0.6 ~ 1:0.3 ~ 1.
3. the preparation method of decoction made from radix adenophorea, tuber of dwarf lilyturf granule according to claim 1, it is characterized in that, described step 1) in, the mass ratio of Radix Glehniae, Rhizoma Polygonati Odorati, Radix Ophiopogonis, Radix Trichosanthis, Seem Lablab Album, Folium Mori and Radix Glycyrrhizae seven taste raw material is 1:1:1:1.5:1:0.6:0.3.
4. the preparation method of decoction made from radix adenophorea, tuber of dwarf lilyturf granule according to claim 1, is characterized in that, described step 4) in, described adjuvant is pharmaceutically acceptable carrier or excipient.
5. the preparation method of decoction made from radix adenophorea, tuber of dwarf lilyturf granule according to claim 1, is characterized in that, step 3) described in filtrate simmer down to 60 DEG C time relative density be the clear paste of 1.14.
6. the preparation method of decoction made from radix adenophorea, tuber of dwarf lilyturf granule according to claim 1, is characterized in that described simmer down to concentrating under reduced pressure; Described drying is spraying dry.
7. the preparation method of decoction made from radix adenophorea, tuber of dwarf lilyturf granule according to claim 6, is characterized in that, described spray-dired inlet temperature is 154 DEG C, and leaving air temp is 95 DEG C.
8. decoction made from radix adenophorea, tuber of dwarf lilyturf granule prepared by the method according to any one of claim 1-7.
9. a detection method for decoction made from radix adenophorea, tuber of dwarf lilyturf granule prepared by the method according to any one of claim 1-7, 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 decoction made from radix adenophorea, tuber of dwarf lilyturf granule, and control medicinal material is Radix Ophiopogonis;
B): qualitative detection licorice ingredient: described qualitative detection is undertaken by thin layer chromatography; Wherein, test sample is decoction made from radix adenophorea, tuber of dwarf lilyturf granule, and control medicinal material is Radix Glycyrrhizae;
C): measure the content of beary metal in described decoction made from radix adenophorea, tuber of dwarf lilyturf granule by Residue on ignition check method;
D): measure the Organochlorine Pesticide Residues content in described decoction made from radix adenophorea, tuber of dwarf lilyturf granule by persticide residue algoscopy;
E): detect extract content by ethanol-soluble extractives hot dipping algoscopy;
F): by the content of material in decoction made from radix adenophorea, tuber of dwarf lilyturf granule described in high effective liquid chromatography for measuring,
Wherein,
Step a) in, described test sample and control medicinal material are respectively by chloroform extraction process, residue is obtained by after chloroform evaporate to dryness, ethanol is added to dissolving in residue, with obtained need testing solution and control medicinal material solution, wherein, developing solvent is chloroform-acetone and developer is the ethanol solution of sulfuric acid of volume ratio 10%;
Step b) in, described test sample and control medicinal material are respectively by adding methanol, supersound process, filtration treatment, after filtrate water is dissolved, use n-butanol extraction, then wash with n-butyl alcohol saturation water, abandon water liquid and by after n-butyl alcohol evaporate to dryness, methanol is added to dissolving in residue, with obtained need testing solution and control medicinal material solution, wherein, developing solvent is acetic ether-methanoic acid-glacial acetic acid-water and developer is the ethanol solution of sulfuric acid of volume ratio 10%;
Step c) in, the content of beary metal≤25ppm recorded;
Steps d) in, 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) undertaken by the method comprised the following steps:
1) carrying out chromatographic condition and system suitability test, is wherein filler with octadecylsilane chemically bonded silica; Take methanol as mobile phase A, with 0.2mol/L ammonium acetate 2% acetic acid solution for Mobile phase B, the volume ratio of A:B is 58:42, and determined wavelength is 237nm, and number of theoretical plate calculates should be not less than 5000 by ammonium glycyrrhizinate peak;
2) prepare testing sample solution, by high effective liquid chromatography for measuring, described testing sample solution comprises reference substance solution and need testing solution;
3) measure, obtain result.
10. the detection method of decoction made from radix adenophorea, tuber of dwarf lilyturf granule according to claim 9, is characterized in that,
Step a) in, described need testing solution and control medicinal material solution are obtained by following steps: get test sample 1g, add water 15mL, adds hydrochloric acid 0.5ml, to put in water-bath reflux 10 minutes, let cool, extract with chloroform 20ml jolting, divide and get chloroform liquid, evaporate to dryness, residue adds ethanol 1ml makes dissolving, makes need testing solution; Separately get control medicinal material 1g Radix Ophiopogonis, add water 20ml, decocts 10 minutes, filters, filtrate adds hydrochloric acid 0.5ml, to put in water-bath reflux 10 minutes, lets cool, extract with chloroform 20ml jolting, divide and get chloroform liquid, evaporate to dryness, residue adds ethanol 1ml makes dissolving, makes control medicinal material solution;
Step b) in, described need testing solution and control medicinal material solution are obtained by following steps: get test sample 0.5g, add methanol 40ml, supersound process 30 minutes, filters, filtrate evaporate to dryness, the residue 20ml that adds water makes dissolving, extracts 2 times, each 25ml with water saturated n-butyl alcohol jolting, merge extractive liquid, wash with the water 30ml that n-butyl alcohol is saturated again, discard water liquid, n-butyl alcohol liquid evaporate to dryness, residue adds methanol 1ml makes dissolving, makes need testing solution; Another extracting liquorice control medicinal material 0.5g, adds methanol 40ml, supersound process 30 minutes, filter, filtrate evaporate to dryness, the residue 20ml that adds water makes dissolving, 2 times are extracted with water saturated n-butyl alcohol jolting, each 25ml, merge extractive liquid, then wash with the water 30ml that n-butyl alcohol is saturated, discard water liquid, n-butyl alcohol liquid evaporate to dryness, residue adds methanol 1ml makes dissolving, makes control medicinal material solution;
Step f) in, the method preparation of described reference substance solution by comprising the following steps: extracting liquorice acid ammonium reference substance is appropriate, accurately weighed, adds 70% ethanol and makes the solution of every 1ml containing ammonium glycyrrhizinate 10 μ g, to obtain final product; Wherein, the method preparation of described need testing solution by comprising the following steps: get test sample 2.0g, accurately weighed, put in tool plug conical flask, precision adds 70% alcoholic solution 100ml, close plug, weighed weight, supersound process 30 minutes, lets cool, weighed weight again, supply the weight of less loss with 70% ethanol, shake up, filter, get subsequent filtrate, to obtain final product.
The detection method of 11. decoction made from radix adenophorea, tuber of dwarf lilyturf granules according to claim 10, is characterized in that, described step f) in, the power of described supersound process is 240W, and frequency is 45kHZ.
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| 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 |
| CN115343383B (en) * | 2022-07-18 | 2024-03-22 | 神威药业集团有限公司 | Method for measuring content of 8 chemical components in adenophora root and ophiopogon root soup |
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