CN106153574B - A kind of detection method of dandelion granule - Google Patents
A kind of detection method of dandelion granule Download PDFInfo
- Publication number
- CN106153574B CN106153574B CN201610454116.1A CN201610454116A CN106153574B CN 106153574 B CN106153574 B CN 106153574B CN 201610454116 A CN201610454116 A CN 201610454116A CN 106153574 B CN106153574 B CN 106153574B
- Authority
- CN
- China
- Prior art keywords
- dandelion
- granule
- dandelion granule
- sample
- spectrum
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- 235000005187 Taraxacum officinale ssp. officinale Nutrition 0.000 title claims abstract description 136
- 241000245665 Taraxacum Species 0.000 title claims abstract description 132
- 239000008187 granular material Substances 0.000 title claims abstract description 127
- 238000001514 detection method Methods 0.000 title claims abstract description 29
- 238000000034 method Methods 0.000 claims abstract description 68
- 239000003814 drug Substances 0.000 claims abstract description 31
- 239000000843 powder Substances 0.000 claims abstract description 27
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000007921 spray Substances 0.000 claims abstract description 11
- 239000006071 cream Substances 0.000 claims abstract description 9
- 239000000706 filtrate Substances 0.000 claims abstract description 9
- 238000010438 heat treatment Methods 0.000 claims abstract description 8
- 238000007908 dry granulation Methods 0.000 claims abstract description 7
- 239000003153 chemical reaction reagent Substances 0.000 claims abstract description 6
- 240000001949 Taraxacum officinale Species 0.000 claims abstract 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 52
- QAIPRVGONGVQAS-DUXPYHPUSA-N trans-caffeic acid Chemical compound OC(=O)\C=C\C1=CC=C(O)C(O)=C1 QAIPRVGONGVQAS-DUXPYHPUSA-N 0.000 claims description 30
- 238000002329 infrared spectrum Methods 0.000 claims description 29
- 238000000605 extraction Methods 0.000 claims description 24
- ACEAELOMUCBPJP-UHFFFAOYSA-N (E)-3,4,5-trihydroxycinnamic acid Natural products OC(=O)C=CC1=CC(O)=C(O)C(O)=C1 ACEAELOMUCBPJP-UHFFFAOYSA-N 0.000 claims description 15
- 229940074360 caffeic acid Drugs 0.000 claims description 15
- 235000004883 caffeic acid Nutrition 0.000 claims description 15
- QAIPRVGONGVQAS-UHFFFAOYSA-N cis-caffeic acid Natural products OC(=O)C=CC1=CC=C(O)C(O)=C1 QAIPRVGONGVQAS-UHFFFAOYSA-N 0.000 claims description 15
- 230000003595 spectral effect Effects 0.000 claims description 15
- 238000001228 spectrum Methods 0.000 claims description 15
- 239000002245 particle Substances 0.000 claims description 13
- 238000000862 absorption spectrum Methods 0.000 claims description 10
- 238000013210 evaluation model Methods 0.000 claims description 10
- 238000012360 testing method Methods 0.000 claims description 10
- 239000002253 acid Substances 0.000 claims description 8
- 239000000284 extract Substances 0.000 claims description 7
- 238000002835 absorbance Methods 0.000 claims description 6
- 238000009826 distribution Methods 0.000 claims description 6
- 238000010606 normalization Methods 0.000 claims description 6
- 238000003705 background correction Methods 0.000 claims description 5
- 239000000463 material Substances 0.000 claims description 5
- 238000005259 measurement Methods 0.000 claims description 5
- 238000004080 punching Methods 0.000 claims description 4
- 238000000227 grinding Methods 0.000 claims description 3
- 230000008676 import Effects 0.000 claims 1
- 238000005464 sample preparation method Methods 0.000 claims 1
- 238000005507 spraying Methods 0.000 claims 1
- 238000012546 transfer Methods 0.000 claims 1
- 238000002360 preparation method Methods 0.000 abstract description 19
- 238000005516 engineering process Methods 0.000 abstract description 8
- 239000000047 product Substances 0.000 description 13
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 9
- 239000000243 solution Substances 0.000 description 9
- 238000004519 manufacturing process Methods 0.000 description 8
- 238000003556 assay Methods 0.000 description 6
- 238000010586 diagram Methods 0.000 description 6
- 238000002790 cross-validation Methods 0.000 description 5
- 229940079593 drug Drugs 0.000 description 5
- 238000011156 evaluation Methods 0.000 description 5
- 239000011521 glass Substances 0.000 description 4
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 4
- 230000002159 abnormal effect Effects 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 230000000857 drug effect Effects 0.000 description 3
- 238000007689 inspection Methods 0.000 description 3
- 238000004811 liquid chromatography Methods 0.000 description 3
- 239000003921 oil Substances 0.000 description 3
- 238000003908 quality control method Methods 0.000 description 3
- 239000013558 reference substance Substances 0.000 description 3
- 238000010561 standard procedure Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 2
- 241000196324 Embryophyta Species 0.000 description 2
- 229920002774 Maltodextrin Polymers 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 239000004480 active ingredient Substances 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
- 230000003111 delayed effect Effects 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 235000019253 formic acid Nutrition 0.000 description 2
- HQKMJHAJHXVSDF-UHFFFAOYSA-L magnesium stearate Chemical compound [Mg+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O HQKMJHAJHXVSDF-UHFFFAOYSA-L 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000002203 pretreatment Methods 0.000 description 2
- 238000004445 quantitative analysis Methods 0.000 description 2
- 238000001694 spray drying Methods 0.000 description 2
- 235000008495 Chrysanthemum leucanthemum Nutrition 0.000 description 1
- 244000192528 Chrysanthemum parthenium Species 0.000 description 1
- 235000000604 Chrysanthemum parthenium Nutrition 0.000 description 1
- 239000005913 Maltodextrin Substances 0.000 description 1
- 206010054949 Metaplasia Diseases 0.000 description 1
- 208000004880 Polyuria Diseases 0.000 description 1
- 240000007164 Salvia officinalis Species 0.000 description 1
- 241000292546 Taraxacum mongolicum Species 0.000 description 1
- 206010044565 Tremor Diseases 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 208000035850 clinical syndrome Diseases 0.000 description 1
- 238000010960 commercial process Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 235000009508 confectionery Nutrition 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 230000004069 differentiation Effects 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 230000035619 diuresis Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 235000008384 feverfew Nutrition 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 239000000796 flavoring agent Substances 0.000 description 1
- 235000019634 flavors Nutrition 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 238000005469 granulation Methods 0.000 description 1
- 230000003179 granulation Effects 0.000 description 1
- 230000003760 hair shine Effects 0.000 description 1
- 238000004128 high performance liquid chromatography Methods 0.000 description 1
- 230000001939 inductive effect Effects 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 210000004185 liver Anatomy 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 235000019359 magnesium stearate Nutrition 0.000 description 1
- 229940035034 maltodextrin Drugs 0.000 description 1
- 230000015689 metaplastic ossification Effects 0.000 description 1
- CAAULPUQFIIOTL-UHFFFAOYSA-N methyl dihydrogen phosphate Chemical compound COP(O)(O)=O CAAULPUQFIIOTL-UHFFFAOYSA-N 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 229910000403 monosodium phosphate Inorganic materials 0.000 description 1
- 235000019799 monosodium phosphate Nutrition 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- YTJSFYQNRXLOIC-UHFFFAOYSA-N octadecylsilane Chemical compound CCCCCCCCCCCCCCCCCC[SiH3] YTJSFYQNRXLOIC-UHFFFAOYSA-N 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000000643 oven drying Methods 0.000 description 1
- 239000008188 pellet Substances 0.000 description 1
- 239000008055 phosphate buffer solution Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000004451 qualitative analysis Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 235000005412 red sage Nutrition 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- -1 sets moisture≤8.0% Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- AJPJDKMHJJGVTQ-UHFFFAOYSA-M sodium dihydrogen phosphate Chemical compound [Na+].OP(O)([O-])=O AJPJDKMHJJGVTQ-UHFFFAOYSA-M 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 210000002784 stomach Anatomy 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
- 230000010415 tropism Effects 0.000 description 1
- 238000012795 verification Methods 0.000 description 1
- 239000000341 volatile oil Substances 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N21/359—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light using near infrared light
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/28—Asteraceae or Compositae (Aster or Sunflower family), e.g. chamomile, feverfew, yarrow or echinacea
- A61K36/288—Taraxacum (dandelion)
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K9/00—Medicinal preparations characterised by special physical form
- A61K9/14—Particulate form, e.g. powders, Processes for size reducing of pure drugs or the resulting products, Pure drug nanoparticles
- A61K9/16—Agglomerates; Granulates; Microbeadlets ; Microspheres; Pellets; Solid products obtained by spray drying, spray freeze drying, spray congealing,(multiple) emulsion solvent evaporation or extraction
- A61K9/1605—Excipients; Inactive ingredients
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N21/3563—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing solids; Preparation of samples therefor
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
- A61K2236/331—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using water, e.g. cold water, infusion, tea, steam distillation, decoction
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/39—Complex extraction schemes, e.g. fractionation or repeated extraction steps
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/51—Concentration or drying of the extract, e.g. Lyophilisation, freeze-drying or spray-drying
Landscapes
- Health & Medical Sciences (AREA)
- Physics & Mathematics (AREA)
- Natural Medicines & Medicinal Plants (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Engineering & Computer Science (AREA)
- Analytical Chemistry (AREA)
- Immunology (AREA)
- Public Health (AREA)
- Veterinary Medicine (AREA)
- Epidemiology (AREA)
- Pharmacology & Pharmacy (AREA)
- Medicinal Chemistry (AREA)
- Biochemistry (AREA)
- General Physics & Mathematics (AREA)
- Animal Behavior & Ethology (AREA)
- Pathology (AREA)
- Bioinformatics & Cheminformatics (AREA)
- Alternative & Traditional Medicine (AREA)
- Biotechnology (AREA)
- Botany (AREA)
- Medical Informatics (AREA)
- Microbiology (AREA)
- Mycology (AREA)
- Investigating Or Analysing Materials By Optical Means (AREA)
- Medicines Containing Plant Substances (AREA)
Abstract
The invention discloses a kind of dandelion granule and its Chinese medicine preparation.The dandelion granule is prepared by the method comprised the following steps：Dandelion medicine materical crude slice is taken, is added water to cook 23 times, 5 10 times of amount water are added every time, heating every time is decocted 12 hours；Decoction merges, and filtrate is concentrated into the clear cream that relative density is 1.02 1.12, is filtered while hot with 250 350 mesh sieves；Qinghuo reagent is spray-dried, and obtains spray powder；By spray powder dry granulation, dandelion granule of the granularity in 16 40 mesh is obtained.The dandelion granule preparation technology of the present invention is simple, and technological parameter is easy to control, and with science, quick, workable detection method.
Description
Technical field
The invention belongs to technical field of traditional Chinese medicine preparation, more particularly to a kind of dandelion granule and the dandelion is included
The Chinese medicine preparation of particle.
Background technology
Dandelion is feverfew dandelion Taraxacum mongolicum Hand.-Mazz., alkali ground dandelion
Taraxacum borealisinense Kitam. or the drying herb for belonging to several plants together, it is bitter, sweet, tremble with fear, Return liver, stomach, tool
Have clearing heat and detoxicating, dispersing swelling and dissipating binds, effect of inducing diuresis for treating strangurtia.Dandelion agents area is herb, is not easy to storage, the appearance of particle
This problem is solved well.
Chinese medicinal granule is, to meet the traditional Chinese medicine medicine materical crude slice of concocted specification as raw material, to extract, concentrate, do through modern industry
Dry, granulation and the Chinese medicine series of products that are made, its function, cure mainly, nature and flavor, channel tropism it is consistent with traditional Chinese medicine medicine materical crude slice, as new
Medicine materical crude slice form is controlled for clinical syndrome differentiation opinion instead of the prepared slices of Chinese crude drugs, adds and subtracts, uses with card." medicine materical crude slice is used as medicine, and faces use with traditional Chinese medicine decoction
Now decoct " application method compare, Chinese medicinal granule had both maintained the property of medicine drug effect of the former prepared slices of Chinese crude drugs, and when using without decocting,
It is easy to carry, safe and healthy, quality controllable, and can be added and subtracted with disease, meet the allegro life style of modern.
At present, Chinese medicinal granule is generally that traditional water is extracted, or extracts extraction after volatile oil, and different preparation technologies are led
The product quality that cause is produced by different manufacturers is inconsistent, and drug effect has difference.Accordingly, it would be desirable to the extraction process of research standard,
With the production process of specification Chinese medicinal granule, it is ensured that drug effect.In addition, the quality of Chinese medicinal granule also can be by detection means
Restriction, the measure of moisture and ethanol soluble extraction in traditional dandelion granule needs several hours, behaviour with reference to the method for pharmacopeia
Make also more complicated.The main chemical compositions of dandelion granule are caffeic acid, and as quality control index, conventional method uses efficient
Liquid chromatography etc., need to often carry out numerous and diverse pretreatment to sample, expend substantial amounts of reagent, and environmental pollution is larger and to examining
Member's body has been damaged, and feedback of the information is delayed, it is impossible to meet instant analysis multi items during particle enterprise large-scale production, many batches
The need for measuring sample.
With the development in epoch, near infrared spectrum (NIRS) analytical technology is further employed in Chemical Measurement polynary time
Return method and contemporary optics, microcomputer data processing so that near-infrared is developed rapidly, as in recent years point
Analyse the emerging analytical technology of one kind " green " of chemical field fast development, with applied widely, measurement it is convenient, pollution-free,
Without destruction, data it is accurate, it is reliable the advantages of, therefore be widely used in the quantitative analysis in the various fields of food, medicine and qualitative mirror
Not.
The content of the invention
In view of the above-mentioned problems of the prior art, it is an object of the invention to provide a kind of Pu of production technology standardization
Public English particle, its preparation technology is simple, steady quality.Meanwhile, in order to better control over the quality of dandelion granule, adapt to industry
Product batch is additionally provided a kind of fast and accurately based near infrared spectrum skill in the demand of X -ray inspection X during metaplasia production
The method of art quick detection dandelion granule.
In order to solve the technical problem of the present invention, the present invention is achieved by the following technical solutions：
On the one hand, the invention provides a kind of dandelion granule, it is prepared by the method comprised the following steps：Take Pu
Public English medicine materical crude slice, is added water to cook 2-3 times, and adding 5-10 times every time measures water, and heating every time is decocted 1-2 hours；Decoction merges, filtrate concentration
To the clear cream that relative density is 1.02-1.12, filtered while hot with 250-350 mesh sieves；Qinghuo reagent is spray-dried, and obtains spray drying
Powder；By spray powder dry granulation, dandelion granule of the granularity in 16-40 mesh is obtained.
Present inventor has found that dandelion adds water to cook 2-3 times by long term test, and adding 5-10 times every time measures water,
Heating is decocted and can more completely extracted active ingredient for 1-2 hours every time.And relative density is concentrated the filtrate to for 1.02-
1.12 clear cream, is filtered with 250-350 mesh sieves, can quickly be gone the moisture in clear cream by the method for spray drying while hot
Remove, and prevent from causing the loss of active ingredient because heated time is longer.
Preferably, dandelion granule of the invention is prepared by the method comprised the following steps：Dandelion medicine materical crude slice is taken, plus
Decocting is boiled 3 times, and 8 times of amount water are added every time, and heating every time is decocted 1.5 hours；Decoction merges, and it is 1.08 that filtrate, which is concentrated into relative density,
Clear cream, while hot with 350 mesh sieves filter；In 170-185 DEG C of EAT, 400-700 revs/min of revolution speed, leaving air temp 85- are expected
95 DEG C, wind is spray-dried under conditions of sending 35-45 DEG C of temperature, obtains spray powder；In punching panel aperture 1.50mm, roller motor
Dry granulation under the conditions of frequency 40HZ, feeding motor frequency 45HZ, oil cylinder working-pressure 20bar, obtains dandelion of the granularity in 16-40 mesh
Particle.
Moisture≤8.0% in the process for producing optimized by the present invention, gained dandelion granule, ethanol soluble extraction
>=20.0%, caffeic acid >=0.50mg/g.
The dandelion granule of the present invention can be further applied in various Chinese medicine preparations, lived with the pharmacology for realizing dandelion
Property.The common Chinese medicine preparation comprising dandelion granule is known in the art, and those skilled in the art can enter as needed
Row combination and application.It is preferred that, pharmaceutically acceptable auxiliary material, such as maltodextrin can be added in Chinese medicine preparation.
On the other hand, in order to adapt in commercial process to product batch in the demand of X -ray inspection X, overcome traditional
High effective liquid chromatography for detecting pre-processes that numerous and diverse, reagent consumption is big, environmental pollution is larger, feedback of the information is delayed lacks
Point, additionally provides a kind of detection method for dandelion granule of the present invention, and it is based on near-infrared spectrum technique quick detection, and
Comprise the following steps：
A. the collection of near infrared spectrum：Dandelion granule sample about 3g is taken, fine powder is ground into, near infrared spectrum scanning is carried out,
Spectrum is gathered, the original absorbance spectrogram of dandelion granule sample is obtained, and each component content is measured, dandelion is measured
The measured value of particulate samples each component content, according to sample number and sample each component content actual measurement Distribution value determine calibration set and
Checking collection；
B. the foundation of dandelion granule quantitative model：The content of dandelion granule moisture is determined, using min-max normalizing
Change method is pre-processed to original absorbance spectrum, and the spectral region of modeling chooses 9401.7-6096.4cm-1And 4602.9-
4247.9cm-1Characteristic wave bands, dimension elects 8 as；Dandelion granule ethanol soluble extraction content is determined, is normalized using min-max
Method is pre-processed to original absorbance spectrum, and the spectral region of modeling is chosen for 7500.1-4247.9cm-1Characteristic wave bands, dimension
Elect 7 as；Dandelion granule coffee acid content is determined, original absorbance spectrum is pre-processed using vector normalization method, is modeled
Spectral region be chosen for 7500.1-5447.6cm-1Characteristic wave bands, dimension elects 8 as；With PLS to calibration set
Quantitative model is set up between near infrared spectrum and the measured value of its correspondence dandelion granule sample each component content；
C. near-infrared quantitative model is verified：Collection checking collection sample atlas of near infrared spectra, by step b set up it is each
Measured portions model, obtains the predicted value of dandelion granule sample each component content, predicted value is compared with measured value, tested
Demonstrate,prove the accuracy of quantitative model；
D. the measure of dandelion granule each component content：Dandelion granule to be detected is taken to be carried out according to step a method
In near infrared spectra collection, the quantitative model that specific band spectral information steps for importing b is set up, dandelion granule each group is determined
The content divided；The dandelion granule moisture built up, extract and caffeinic near-infrared quantitative determination model are passed through near red
Outer analysis software is integrated, and the multi-method evaluation model of dandelion granule is set up, by dandelion granule sample to be detected according to step
Rapid a method collection near infrared spectrum, is imported in dandelion granule multi-method evaluation model, while determining dandelion granule each group
Divide content.
Using above-mentioned detection method, the moisture, ethanol soluble extraction and coffee acid content of dandelion granule can be determined simultaneously, only
Need a few minutes just can complete the detection of each group divided data, substantially reduce detection time, adapt to modern enterprise quick, a large amount of
The demand of production.And traditional detection method, contained using high effective liquid chromatography for measuring coffee acid content, moisture analysis
Amount, ethanol soluble extractives determination method determine ethanol soluble extraction content, cumbersome, not only need a variety of instrument and equipments, also need each
Individual inspection post cooperates and can just smoothly completed, and data handling procedure is more complicated, time-consuming.In addition, the method for the present invention can
The each component assay of the material of 3 production links, including medicinal extract, spray dried powder, particle are applicable simultaneously.
In order to more accurately determine, in the assay method of the present invention, the sample system that dandelion granule near-infrared is determined
Preparation Method is：Same batch dandelion granule about 3g is taken, fine powder is ground into, 80 mesh sieves are crossed, near-infrared measure is transferred to
In tool plug vial.Preferably, grinding fine powder is shifted using funnel, makes it close by way of up-down vibration, used
Bottle closure of rubber is stoppered.It is highly preferred that under the conditions of 18-22 DEG C of temperature, humidity 40-50%, particle is ground and fast quick-mounting
Bottle.Sample bottle bottom after observation dress sample, it is ensured that the sample powder of test does not bond vial bottom, can just be carried out to sample
Near infrared spectrum scanning.
The inventive method carries out pre-treatment for particulate samples, is ground into fine powder, crosses 80 mesh sieves, is transferred to tool plug glass
In bottle, by way of up-down vibration, reduce the hole of sample powder, reducing near infrared light, irregularly operation causes in the optical path
Error；According to the method for the present invention, for the measure of extract of taraxacum, appropriate amount of auxiliary materials can be added by technological requirement, then use
Micro-wave oven rapid draing, dry extract can complete detection by particl method is determined, for spray dried powder, then directly by measure
Particl method, greatly reduces the workload of model foundation, realizes the quality to each key link material of dandelion granule
Control.
Preferably, in step a, the condition of scanning of described near infrared spectra collection is：Scanning range is 4000cm-1-
12000cm-1, scanning times are 32 times, and resolution ratio is 8cm-1, background correction, every part of sample collection 3 in real time in scanning process
Spectrum.
The inventive method has the function of quantitative detection and Qualitive test.Quantitatively surveyed in dandelion granule each component near-infrared
On the basis of cover half type, dandelion granule multi-method evaluation model is established, sample reclaimed water can be drawn by the collection of a spectrum
Point, the multicomponent content results such as ethanol soluble extraction and caffeic acid, while product can be distinguished again according to mahalanobis distance and density of fraction etc.
Plant the true and false.
The inventive method is particularly suitable for use in the products characteristics of Chinese medicinal granule, is processed and made through single medicine materical crude slice due to Chinese medicinal granule
Into, compared with Chinese native medicine compound prescription pellet or Chinese patent drug, component is relatively single, using this method interference less, accuracy it is high；In addition, in
Medicine particle series of products have kind more than 500, due to wide in variety, and conventional method is difficult to while realize qualitative, quantitative detection, the present invention
Under the premise of easy, free of contamination, while completing qualitative and quantitative analysis, product abnormal risk can be found in time, it is big to particle
The quality control of production intermediate link has great importance.
Therefore, the present invention compared with prior art, has the advantages that：(1) the specification preparation of dandelion granule
Technique, and preparation technology is simple, technological parameter is stable and easy to control, is adapted to the preparation of dandelion formulation particle.(2) base of the present invention
In near-infrared spectrum technique combination chemometrics method, in certain spectral region, establish dandelion granule near-infrared and determine
Model is measured, while for Qualitive test, without carrying out complicated pre-treatment to sample, fine powder can be ground into, do not related to
And any reagent, it is environmentally friendly, safe and nontoxic, it is the trend of Quality Control job development from now on, one kind is provided for detection dandelion granule
Fast and accurately new method.The online matter in Chinese medicinal granule enterprise production process can be promoted the use as a kind of practical approach
Abnormal products can be pointed out, it is ensured that the stabilization of production quality, feasible by amount monitoring in time.
Brief description of the drawings
The near-infrared original absorbance spectrogram of Fig. 1 dandelion granule samples；
Related figure between Fig. 2 dandelion granules moisture near-infrared predicted value and measured value；
The comparison column diagram of Fig. 3 dandelion granules moisture near-infrared predicted value and measured value；
Related figure between Fig. 4 dandelion granules ethanol soluble extraction near-infrared predicted value and measured value；
The comparison column diagram of Fig. 5 dandelion granules ethanol soluble extraction near-infrared predicted value and measured value；
Related figure between Fig. 6 dandelion granules caffeic acid near-infrared predicted value and measured value；
The comparison column diagram of Fig. 7 dandelion granules caffeic acid near-infrared predicted value and measured value.
Embodiment
The present invention is further illustrated below by embodiment, following examples are the specific embodiment party of the present invention
Formula, but embodiments of the present invention are not limited by following embodiments.
Embodiment 1：
The preparation of dandelion granule：Dandelion medicine materical crude slice is taken, is added water to cook 3 times, 8 times of amount water are added every time, heating every time is decocted
1.5 hour；Decoction merges, and filtrate is concentrated into the clear cream that relative density is 1.08 (80 DEG C), is filtered while hot with 350 mesh sieves；Entering
175 DEG C of air temperature, expects 500 revs/min of revolution speed, and 90 DEG C of leaving air temp, wind is spray-dried under conditions of sending 40 DEG C of temperature, obtained
Spray powder；In punching panel aperture 1.50mm, roller motor frequency 40HZ, feeding motor frequency 45HZ, oil cylinder working-pressure 20bar conditions
Lower dry granulation, obtains dandelion granule of the granularity in 40 mesh.
Embodiment 2：
The preparation of Chinese medicine preparation containing dandelion granule：The preparation of dandelion granule：Dandelion medicine materical crude slice is taken, 3 are added water to cook
It is secondary, 8 times of amount water are added every time, heating every time is decocted 1.5 hours；Decoction merges, and filtrate is concentrated into relative density for 1.08 (80 DEG C)
Clear cream, while hot with 350 mesh sieves filter；In 175 DEG C of EAT, 500 revs/min of revolution speed is expected, 90 DEG C of leaving air temp, wind send temperature
It is spray-dried under conditions of 40 DEG C of degree, obtains spray powder；In punching panel aperture 1.50mm, roller motor frequency 40HZ, feeding
Dry granulation under the conditions of electric machine frequency 45HZ, oil cylinder working-pressure 20bar, obtains dandelion granule of the granularity in 40 mesh；175g Pus is public
English particle and 65g maltodextrins are mixed, and add appropriate magnesium stearate, are mixed, are pressed into 1000.
Embodiment 3：
A kind of method based on near-infrared spectrum technique quick detection dandelion granule moisture, specifically includes following step
Suddenly：
A, dandelion granule sample is taken, totally 82 batches, respectively take about 3g, be ground into fine powder, be fitted into tool plug glass sample bottle, be placed in
It is scanned on infrared diaphanoscopy instrument, gathers spectrum, the condition of scanning：Scanning range 4000-12000cm-1, scanning times：32
It is secondary, resolution ratio 8cm-1, background correction in real time in scanning process, 3 spectrum of every part of sample collection obtain as shown in Figure 1 82 batches
The near-infrared original absorbance spectrogram of dandelion granule；
Meanwhile, the standard method according to specified in 2015 editions Chinese Pharmacopoeias, its moisture is determined using oven drying method, is taken and is ground
Finely disintegrated dandelion granule about 2g, is laid in and dries into the flat measuring cup of constant weight, accurately weighed, opens bottle cap and exists
100-105 DEG C of drying 5 hours, bottle cap is covered, in dislocation drier, is cooled down 30 minutes, accurately weighed, then dry in said temperature
Dry 1 hour, cooling was weighed, untill the double difference weighed is no more than 5mg；According to the weight of less loss, dandelion is calculated
The water content (%) of particle, determines that calibration set and checking collect according to sample number and sample distribution；
B, Distribution value surveyed according to sample number and sample moisture, it is calibration set to choose 64 batches, and it is checking to choose 18 batches
Collection.Analysis software, Automatic Optimal chooses preprocess method and spectral region, and optimum results are shown in Table 1.Using min-max
Normalization method is pre-processed to near-infrared original absorbance spectrum, chooses 9401.7-6096.4cm-1And 4602.9-4247.9cm-1Spectral information under characteristic wave bands, with PLS (PLS) set up near infrared spectrum and moisture measured value it
Between quantitative model；The sample for verifying collection is subjected near infrared spectrum scanning, using model, dandelion granule sample size is obtained
Predicted value, predicted value is compared with measured value, verify quantitative model accuracy and predictive ability, the model through intersect
Verify to obtain cross validation coefficient R2=0.881, RMSECV=0.163, RPD=2.9, dimension elect 8, checking collection phase relation as
Number R2The determination of moisture of=0.967, RMSEP=0.132,18 batch dandelion granule the results are shown in Table 2, moisture predicted value and reality
Related figure between measured value is shown in Fig. 2, and the comparison column diagram of moisture predicted value and measured value is shown in Fig. 3.
Model parameter of the water model of table 1 under different spectral regions and preprocess method
The determination of moisture result of 2 18 batches of dandelion granules of table
The deviation range of dandelion granule moisture is average pre- between 0.02-0.26% it can be seen from upper table 2
Survey time yield is 101.26%, illustrates that the model has preferable predictive ability and stability, available for dandelion granule moisture
Quick detection.
Embodiment 4：
A kind of method based on near-infrared spectrum technique quick detection dandelion granule ethanol soluble extraction content, is specifically included
Following steps：
A, dandelion granule sample is taken, totally 82 batches, respectively take about 3g, be ground into fine powder, be fitted into tool plug glass sample bottle, be placed in
It is scanned on infrared diaphanoscopy instrument, gathers spectrum, the condition of scanning：Scanning range 4000-12000cm-1, scanning times：32
It is secondary, resolution ratio 8cm-1, background correction in real time in scanning process, 3 spectrum of every part of sample collection obtain as shown in Figure 1 82 batches
The near-infrared original absorbance spectrogram of dandelion granule；
Meanwhile, the standard method according to specified in 2015 editions Chinese Pharmacopoeias, its ethanol soluble extraction content is surveyed using hot dipping
It is fixed, the dandelion granule about 2g for grinding to form fine powder is taken, it is accurately weighed, put in 100ml conical flask, precision plus ethanol 100ml are close
Plug, weighed weight after standing 1 hour, connects reflux condensing tube, is heated to boiling, and keep micro-boiling 1 hour；After letting cool, remove
Conical flask, close plug, then weighed weight, the weight of less loss is supplied with ethanol, is shaken up, and is filtered with filter is dried, precision measures filtrate
50ml, put dry into the evaporating dish of constant weight, be evaporated in water-bath after, in 105 DEG C dry 3 hours, put in drier cool down
30 minutes, the rapid close weighed weight of nationality；Unless otherwise specified, ethanol soluble extractives in dandelion granule is calculated with dry product to contain
Measure (%), determine that calibration set and checking collect according to sample number and sample distribution；
B, Distribution value surveyed according to sample number and sample ethanol soluble extraction content, it is calibration set to choose 67 batches, chooses 15 batches
For checking collection.Analysis software, Automatic Optimal chooses preprocess method and spectral region, and optimum results are shown in Table 3.Using most
Small-maximum normalization method is pre-processed to near-infrared original absorbance spectrum, chooses 7500.1-4247.9cm-1Under characteristic wave bands
Spectral information, set up determining between near infrared spectrum and ethanol soluble extraction content measured value with PLS (PLS)
Measure model；The sample for verifying collection is subjected near infrared spectrum scanning, using model, the prediction of dandelion granule sample size is obtained
Value, predicted value is compared with measured value, verifies the accuracy and predictive ability of quantitative model, and the model is obtained through cross validation
Cross validation coefficient R2=0.866, RMSECV=1.17, RPD=4.64, dimension elect 7, checking collection coefficient R as2=
The ethanol soluble extraction assay of 0.925, RMSEP=1.31,15 batches of dandelion granules the results are shown in Table 4, ethanol soluble extraction prediction
Related figure between value and measured value is shown in Fig. 4, and the comparison column diagram of ethanol soluble extraction predicted value and measured value is shown in Fig. 5
Model parameter of the ethanol soluble extraction model of table 3 under different spectral regions and preprocess method
The ethanol soluble extraction assay result of 4 15 batches of dandelion granules of table
The deviation range of dandelion granule ethanol soluble extraction content is between 0.02-2.25% it can be seen from upper table 4,
It is 100.60% to predict average recovery rate, illustrates that the model has preferable predictive ability and stability, available for dandelion
The quick detection of grain ethanol soluble extraction.
Embodiment 5：
A kind of method based on near-infrared spectrum technique quick detection Determination of Caffeic Acid in Pugongying Granules, specifically include as
Lower step：
A, dandelion granule sample is taken, totally 82 batches, respectively take about 3g, be ground into fine powder, be fitted into tool plug glass sample bottle, be placed in
It is scanned on infrared diaphanoscopy instrument, gathers spectrum, the condition of scanning：Scanning range 4000-12000cm-1, scanning times：32
It is secondary, resolution ratio 8cm-1, background correction in real time in scanning process, 3 spectrum of every part of sample collection obtain as shown in Figure 1 82 batches
The near-infrared original absorbance spectrogram of dandelion granule；
Meanwhile, the standard method according to specified in 2015 editions Chinese Pharmacopoeias, its coffee acid content shines high performance liquid chromatography
(《Chinese Pharmacopoeia》Four general rules 0512 of version in 2015) determine, comprise the following steps that：
Chromatographic condition and system suitability：Using octadecylsilane chemically bonded silica as filler；With methanol-phosphate
Buffer solution (sodium dihydrogen phosphate 1.56g is taken, adding water makes to be dissolved into 1000ml, then adjusts pH value to 3.8-4.0 with 1% phosphoric acid solution,
Produce) (23: 77) be mobile phase；Detection wavelength is 323nm；40 DEG C of column temperature.Number of theoretical plate is calculated by caffeic acid peak to be not less than
3000。
The preparation of reference substance solution：Take caffeic acid reference substance appropriate, it is accurately weighed, plus every 1ml is made containing 25 μ g in methanol
Solution, is produced.
The preparation of need testing solution：This product under content uniformity is taken, it is finely ground, about 1g is taken, it is accurately weighed, put tool plug taper
In bottle, precision adds 50% methanol solution 50ml of 5% formic acid, close plug, weighed weight, ultrasonically treated (power 300W, frequency
40kHz) 30 minutes, let cool, then weighed weight, the weight of less loss is supplied with 50% methanol solution of 5% formic acid, is shaken up, is centrifuged,
Supernatant is taken, is put in brown bottle, is produced.
Determination method：It is accurate respectively to draw reference substance solution and each 5-10 μ l of need testing solution, liquid chromatograph is injected, is surveyed
It is fixed, produce.
B, it is distributed according to sample number and sample coffee acid content measured value, it is calibration set to choose 66 batches, chooses 16 batches to test
Card collection.Analysis software, Automatic Optimal chooses preprocess method and spectral region, and optimum results are shown in Table 5.Using vector normalizing
Change method is pre-processed to near-infrared original absorbance spectrum, chooses 7500.1-5447.6cm-1Spectral information under characteristic wave bands,
The quantitative model set up with PLS (PLS) between near infrared spectrum and caffeic acid standard content；Collection will be verified
Sample carries out near infrared spectrum scanning, using model, obtains the predicted value of dandelion granule sample size, by predicted value and actual measurement
Value is compared, and verifies the accuracy and predictive ability of quantitative model, and the model obtains cross validation coefficient correlation through cross validation
R2=0.849, RMSECV=0.094, RPD=2.57, dimension elect 8, checking collection coefficient R as2=0.915, RMSEP=
The caffeic acid assay of 0.061,16 batch of dandelion granule the results are shown in Table 6, related between caffeic acid predicted value and measured value
Figure is shown in Fig. 6, and the comparison column diagram of caffeic acid predicted value and measured value is shown in Fig. 7.
Model parameter of the coffee acid profile of table 5 under different spectral regions and preprocess method
6 16 batches of dandelion granule caffeic acid assay results of table
The caffeinic deviation range of dandelion granule is between 0-0.12mg/g it can be seen from upper table 6, and prediction is average to return
Yield is 99.66%.Illustrate that the model has preferable predictive ability and stability, it is caffeinic fast available for dandelion granule
Speed detection.
Embodiment 6：
A kind of method based on near-infrared spectrum technique Fast Evaluation dandelion granule quality, specifically includes following steps：
A. software is used, the dandelion granule caffeic acid built, moisture and extract quantitative model are imported, and sets each
The content limit of component, according to the quality standard of dandelion granule, sets moisture≤8.0%, ethanol soluble extraction >=20.0%, coffee
Coffee acid >=0.50mg/g, sets up the multi-method evaluation model of dandelion granule；
B. sample near-infrared absorption spectrum figure is gathered, spectrogram is imported in multi-method evaluation model, sample each group is read
The content and evaluation information divided.
To verify the predictive ability and accuracy of this model, the present invention is using mono blind method experiment, to dandelion, red sage root etc. 10
Criticize particulate samples to be evaluated, sample message table is shown in Table 7.The spectrogram of the sample of numbering 1~10 is gathered respectively, and spectrogram is imported
In dandelion granule multi-method evaluation model, the content and evaluation information of sample each component are read, 8 are the results are shown in Table.
The multi-method evaluation model verification sample information table of table 7
The dandelion granule multi-method evaluation result of table 8
- represent to survey sample passes, * represents that institute's test sample product are abnormal (different samples or content are undesirable)
As can be seen from Table 8, the multi-method evaluation model can according to sample spectra information, analyze draw mahalanobis distance,
Whether density of fraction, by the size of its value, can be dandelion granule with principium identification institute test sample product, be identified as dandelion
The sample of grain can draw the accurate predictor of each component simultaneously.Illustrate that the model has preferable predictive ability and accuracy, can
The quality of Fast Evaluation dandelion granule.
Claims (6)
1. a kind of detection method of dandelion granule, it is characterised in that be the detection method based on near-infrared spectrum technique, and wrap
Include following steps：
A. the collection of near infrared spectrum：Dandelion granule sample about 3g is taken, fine powder is ground into, near infrared spectrum scanning, collection is carried out
Spectrum, obtains the original absorbance spectrogram of dandelion granule sample, and each component content is measured, and measures dandelion granule
The measured value of sample each component content, calibration set and checking are determined according to sample number and sample each component content actual measurement Distribution value
Collection；The condition of scanning of described near infrared spectra collection is：Scanning range is 4000cm-1-12000cm-1, scanning times are 32
Secondary, resolution ratio is 8cm-1, background correction, 3 spectrum of every part of sample collection in real time in scanning process；
B. the foundation of dandelion granule quantitative model：The content of dandelion granule moisture is determined, using min-max normalization method
Original absorbance spectrum is pre-processed, the spectral region of modeling chooses 9401.7-6096.4cm-1And 4602.9-4247.9cm-1Characteristic wave bands, dimension elects 8 as；Dandelion granule ethanol soluble extraction content is determined, using min-max normalization method to original
Absorption spectrum is pre-processed, and the spectral region of modeling is chosen for 7500.1-4247.9cm-1Characteristic wave bands, dimension elects 7 as；Survey
Determine dandelion granule coffee acid content, original absorbance spectrum is pre-processed using vector normalization method, the spectrum model of modeling
Enclose and be chosen for 7500.1-5447.6cm-1Characteristic wave bands, dimension elects 8 as；With near infrared light of the PLS to calibration set
Quantitative model is set up between the measured value of spectrum and its correspondence dandelion granule sample each component content；
C. near-infrared quantitative model is verified：The atlas of near infrared spectra of collection checking collection sample, each component set up by step b
Quantitative model, obtains the predicted value of dandelion granule sample each component content, predicted value is compared with measured value, and checking is fixed
Measure the accuracy of model；
D. the measure of dandelion granule each component content：Dandelion granule to be detected is taken to be carried out according to step a method near red
External spectrum is gathered, in the quantitative model that specific band spectral information steps for importing b is set up, and determines dandelion granule each component
Content；The dandelion granule moisture built up, extract and caffeinic near-infrared are quantitative determined into model and pass through near-infrared point
Analyse software to integrate, the multi-method evaluation model of dandelion granule is set up, by dandelion granule sample to be detected according to step a's
Method gathers near infrared spectrum, imports in dandelion granule multi-method evaluation model, contains while determining dandelion granule each component
Amount；
Described dandelion granule is prepared by the method comprised the following steps：Dandelion medicine materical crude slice is taken, is added water to cook 2-3 times,
Add 5-10 times every time and measure water, heating every time is decocted 1-2 hours；Decoction merges, and it is 1.02-1.12's that filtrate, which is concentrated into relative density,
Clear cream, is filtered with 250-350 mesh sieves while hot；Qinghuo reagent is spray-dried, and obtains spray powder；By spray powder dry granulation, grain is obtained
Spend the dandelion granule in 16-40 mesh；Moisture≤8.0% in dandelion granule, ethanol soluble extraction >=20.0%, caffeic acid >=
0.50mg/g。
2. the detection method of dandelion granule as claimed in claim 1, it is characterised in that described dandelion granule by including
The method of following steps is prepared：Dandelion medicine materical crude slice is taken, is added water to cook 3 times, 8 times of amount water are added every time, heating every time decocts 1.5
Hour；Decoction merges, and filtrate is concentrated into the clear cream that relative density is 1.08, is filtered while hot with 350 mesh sieves；In EAT 170-
185 DEG C, 400-700 revs/min of revolution speed of material, 85-95 DEG C of leaving air temp, progress spraying is dry under conditions of wind send 35-45 DEG C of temperature
It is dry, obtain spray powder；In punching panel aperture 1.50mm, roller motor frequency 40HZ, feeding motor frequency 45HZ, oil cylinder working-pressure
Dry granulation under the conditions of 20bar, obtains dandelion granule of the granularity in 16-40 mesh.
3. the detection method of dandelion granule as claimed in claim 1 or 2, it is characterised in that dandelion granule near-infrared is determined
Sample preparation methods be：Same batch dandelion granule about 3g is taken, fine powder is ground into, 80 mesh sieves are crossed, is transferred near red
In the tool plug vial of outer measure.
4. the detection method of dandelion granule as claimed in claim 1 or 2, it is characterised in that enter grinding fine powder using funnel
Row transfer, is made it close by way of up-down vibration, is stoppered with bottle closure of rubber.
5. the detection method of dandelion granule as claimed in claim 1 or 2, it is characterised in that in 18-22 DEG C of temperature, humidity
Under the conditions of 40-50%, particle is ground with quickly bottling.
6. the detection method of dandelion granule as claimed in claim 1 or 2, it is characterised in that the sample bottle bottom after observation dress sample
Portion, it is ensured that the sample powder of test does not bond vial bottom, just can carry out near infrared spectrum scanning to sample.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610454116.1A CN106153574B (en) | 2016-06-20 | 2016-06-20 | A kind of detection method of dandelion granule |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610454116.1A CN106153574B (en) | 2016-06-20 | 2016-06-20 | A kind of detection method of dandelion granule |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106153574A CN106153574A (en) | 2016-11-23 |
| CN106153574B true CN106153574B (en) | 2017-08-25 |
Family
ID=57353046
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610454116.1A Active CN106153574B (en) | 2016-06-20 | 2016-06-20 | A kind of detection method of dandelion granule |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106153574B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110057771A (en) * | 2019-06-13 | 2019-07-26 | 四川德成动物保健品有限公司 | A kind of discrimination method of viola mandshurica and dandelion |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101396423B (en) * | 2007-09-28 | 2012-05-30 | 北京康仁堂药业有限公司 | Kudzu root dispensing granule and preparation method and quality control method thereof |
-
2016
- 2016-06-20 CN CN201610454116.1A patent/CN106153574B/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| CN106153574A (en) | 2016-11-23 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106138131B (en) | A kind of bupleurum particles and its Chinese medicine preparation | |
| CN106074695B (en) | A kind of DANSHEN KELI and its Chinese medicine preparation | |
| CN106074700B (en) | A kind of detection method of radix scutellariae particle | |
| CN106074742B (en) | A kind of root of herbaceous peony particle and its Chinese medicine preparation | |
| CN106074664B (en) | A kind of detection method of Fructus Corni particle | |
| Huang et al. | Qualitative discrimination of Chinese dianhong black tea grades based on a handheld spectroscopy system coupled with chemometrics | |
| CN103033486A (en) | Method for near infrared spectrum monitoring of quality of pericarpium citri reticulatae and citrus chachiensis hortorum medicinal materials | |
| CN104568813A (en) | Multi-index fast detection method of dogwood medicinal materials | |
| Peng et al. | Discrimination of heat-damaged tomato seeds based on near infrared spectroscopy and PCA-SVM method | |
| CN106074679B (en) | A kind of root of kudzu vine particle and its Chinese medicine preparation | |
| CN102028710B (en) | Method for measuring contents of indole alkaloids in cinobufagin alcohol precipitation liquid | |
| CN106153574B (en) | A kind of detection method of dandelion granule | |
| CN108051396A (en) | A kind of rapid detection method of Xin Ke Shu ' tablet for treating coronary heart disease active constituent content | |
| CN106092958B (en) | A kind of detection method of coptis particle | |
| CN106706555A (en) | Milk powder determination method and system based on near infrared spectroscopy technology | |
| CN106109556B (en) | A kind of detection method of licorice root particles | |
| CN106074743B (en) | A kind of detection method of moutan bark particle | |
| CN106109696B (en) | A kind of detection method of radix scrophulariae particle | |
| CN106420925B (en) | A kind of cassia twig particle and its Chinese medicine preparation | |
| CN106074722B (en) | A kind of detection method of capsule of weeping forsythia particle | |
| CN104819955B (en) | Ligusticum wallichii method and application are detected based on population least square method supporting vector machine algorithm | |
| CN106074797B (en) | A kind of detection method of stir-baked FRUCTUS AURANTII in bran particle | |
| CN106109605B (en) | A kind of radix paeoniae rubrathe particle and its Chinese medicine preparation | |
| CN106074806B (en) | A kind of golden cypress particle and its Chinese medicine preparation | |
| CN114813627B (en) | Dendrobium nobile mannose content detection method based on near infrared spectrum |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| PE01 | Entry into force of the registration of the contract for pledge of patent right | ||
| PE01 | Entry into force of the registration of the contract for pledge of patent right |
Denomination of invention: A detection method for dandelion particles Effective date of registration: 20231225 Granted publication date: 20170825 Pledgee: Bank of China Limited by Share Ltd. Foshan branch Pledgor: GUANGDONG YIFANG PHARMACEUTICAL Co.,Ltd. Registration number: Y2023980073969 |