CN106092958B - A kind of detection method of coptis particle - Google Patents
A kind of detection method of coptis particle Download PDFInfo
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- 235000002991 Coptis groenlandica Nutrition 0.000 title claims abstract description 151
- 239000002245 particle Substances 0.000 title claims abstract description 114
- 238000001514 detection method Methods 0.000 title claims abstract description 29
- 241000218202 Coptis Species 0.000 title claims abstract 41
- 238000000034 method Methods 0.000 claims abstract description 75
- 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 19
- 238000002360 preparation method Methods 0.000 claims abstract description 18
- 239000008187 granular material Substances 0.000 claims abstract description 14
- 239000007921 spray Substances 0.000 claims abstract description 11
- 239000000706 filtrate Substances 0.000 claims abstract description 10
- 230000008569 process Effects 0.000 claims abstract description 10
- 239000006071 cream Substances 0.000 claims abstract description 9
- 238000010438 heat treatment Methods 0.000 claims abstract description 7
- 238000007908 dry granulation Methods 0.000 claims abstract description 6
- 239000003153 chemical reaction reagent Substances 0.000 claims abstract description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 51
- WITLAWYGGVAFLU-UHFFFAOYSA-N 3-(6-methoxy-1,3-benzodioxol-5-yl)-8,8-dimethylpyrano[2,3-f]chromen-4-one Chemical compound C1=CC(C)(C)OC2=CC=C(C(C(C3=CC=4OCOC=4C=C3OC)=CO3)=O)C3=C21 WITLAWYGGVAFLU-UHFFFAOYSA-N 0.000 claims description 44
- 238000002329 infrared spectrum Methods 0.000 claims description 29
- XDVZNDLANFJOQR-UHFFFAOYSA-N Coptisine Natural products O=Cc1c2OCOc2ccc1C=C3/NCCc4cc5OCOc5cc34 XDVZNDLANFJOQR-UHFFFAOYSA-N 0.000 claims description 27
- XYHOBCMEDLZUMP-UHFFFAOYSA-N coptisine Chemical compound C1=C2C=C(C3=C(C=C4OCOC4=C3)CC3)[N+]3=CC2=C2OCOC2=C1 XYHOBCMEDLZUMP-UHFFFAOYSA-N 0.000 claims description 27
- PTPHDVKWAYIFRX-UHFFFAOYSA-N Palmatine Natural products C1C2=C(OC)C(OC)=CC=C2C=C2N1CCC1=C2C=C(OC)C(OC)=C1 PTPHDVKWAYIFRX-UHFFFAOYSA-N 0.000 claims description 26
- FPJQGFLUORYYPE-UHFFFAOYSA-N epiberberine Chemical compound C1=C2C=C(C3=C(C=C(C(=C3)OC)OC)CC3)[N+]3=CC2=C2OCOC2=C1 FPJQGFLUORYYPE-UHFFFAOYSA-N 0.000 claims description 26
- QUCQEUCGKKTEBI-UHFFFAOYSA-N palmatine Chemical compound COC1=CC=C2C=C(C3=C(C=C(C(=C3)OC)OC)CC3)[N+]3=CC2=C1OC QUCQEUCGKKTEBI-UHFFFAOYSA-N 0.000 claims description 26
- 238000001228 spectrum Methods 0.000 claims description 24
- 238000000605 extraction Methods 0.000 claims description 21
- 230000003595 spectral effect Effects 0.000 claims description 21
- 238000000862 absorption spectrum Methods 0.000 claims description 18
- 239000000047 product Substances 0.000 claims description 15
- 238000013210 evaluation model Methods 0.000 claims description 10
- 239000000284 extract Substances 0.000 claims description 10
- 238000010606 normalization Methods 0.000 claims description 9
- 238000012360 testing method Methods 0.000 claims description 9
- 238000009826 distribution Methods 0.000 claims description 7
- 238000002835 absorbance Methods 0.000 claims description 6
- 239000003513 alkali Substances 0.000 claims description 6
- YBHILYKTIRIUTE-UHFFFAOYSA-N berberine Chemical compound C1=C2CC[N+]3=CC4=C(OC)C(OC)=CC=C4C=C3C2=CC2=C1OCO2 YBHILYKTIRIUTE-UHFFFAOYSA-N 0.000 claims description 6
- 229940093265 berberine Drugs 0.000 claims description 6
- QISXPYZVZJBNDM-UHFFFAOYSA-N berberine Natural products COc1ccc2C=C3N(Cc2c1OC)C=Cc4cc5OCOc5cc34 QISXPYZVZJBNDM-UHFFFAOYSA-N 0.000 claims description 6
- 238000005259 measurement Methods 0.000 claims description 6
- 239000008188 pellet Substances 0.000 claims description 6
- 238000003705 background correction 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 description 2
- 238000012546 transfer Methods 0.000 claims 1
- 244000247747 Coptis groenlandica Species 0.000 description 110
- 238000002790 cross-validation Methods 0.000 description 12
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 9
- 238000010586 diagram Methods 0.000 description 9
- 238000005516 engineering process Methods 0.000 description 8
- 229940079593 drug Drugs 0.000 description 7
- 238000004519 manufacturing process Methods 0.000 description 7
- 238000011084 recovery Methods 0.000 description 6
- 239000000243 solution Substances 0.000 description 6
- 241001083847 Berberis Species 0.000 description 4
- 235000016068 Berberis vulgaris Nutrition 0.000 description 4
- 238000003556 assay Methods 0.000 description 4
- 238000011156 evaluation Methods 0.000 description 4
- 239000011521 glass Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 238000003908 quality control method Methods 0.000 description 4
- 239000013558 reference substance Substances 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
- 230000014759 maintenance of location Effects 0.000 description 3
- 239000003921 oil Substances 0.000 description 3
- 238000010561 standard procedure Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 229920002774 Maltodextrin Polymers 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
- 239000012141 concentrate Substances 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
- 238000004128 high performance liquid chromatography Methods 0.000 description 2
- 238000007689 inspection Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000004811 liquid chromatography Methods 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
- VKJGBAJNNALVAV-UHFFFAOYSA-M Berberine chloride (TN) Chemical compound [Cl-].C1=C2CC[N+]3=CC4=C(OC)C(OC)=CC=C4C=C3C2=CC2=C1OCO2 VKJGBAJNNALVAV-UHFFFAOYSA-M 0.000 description 1
- 241000037740 Coptis chinensis Species 0.000 description 1
- 241000037803 Coptis deltoidea Species 0.000 description 1
- 206010013786 Dry skin Diseases 0.000 description 1
- 241001411320 Eriogonum inflatum Species 0.000 description 1
- 239000005913 Maltodextrin Substances 0.000 description 1
- 206010054949 Metaplasia Diseases 0.000 description 1
- RCEAADKTGXTDOA-UHFFFAOYSA-N OS(O)(=O)=O.CCCCCCCCCCCC[Na] Chemical compound OS(O)(=O)=O.CCCCCCCCCCCC[Na] RCEAADKTGXTDOA-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 206010044565 Tremor Diseases 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 230000008859 change Effects 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
- 239000000470 constituent Substances 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
- 230000000694 effects Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 238000001914 filtration Methods 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
- 238000005469 granulation Methods 0.000 description 1
- 230000003179 granulation Effects 0.000 description 1
- FUKUFMFMCZIRNT-UHFFFAOYSA-N hydron;methanol;chloride Chemical compound Cl.OC FUKUFMFMCZIRNT-UHFFFAOYSA-N 0.000 description 1
- 210000002429 large intestine Anatomy 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 238000002386 leaching Methods 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
- 239000011259 mixed solution Substances 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 235000019796 monopotassium 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
- 230000000144 pharmacologic effect Effects 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- GNSKLFRGEWLPPA-UHFFFAOYSA-M potassium dihydrogen phosphate Chemical class [K+].OP(O)([O-])=O GNSKLFRGEWLPPA-UHFFFAOYSA-M 0.000 description 1
- 238000007781 pre-processing Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000010926 purge Methods 0.000 description 1
- 238000004451 qualitative analysis Methods 0.000 description 1
- 239000002994 raw material Substances 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
- 210000000952 spleen Anatomy 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
- 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)
- A61K36/71—Ranunculaceae (Buttercup family), e.g. larkspur, hepatica, hydrastis, columbine or goldenseal
- A61K36/718—Coptis (goldthread)
-
- 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
-
- 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
- A61K9/20—Pills, tablets, discs, rods
- A61K9/2004—Excipients; Inactive ingredients
- A61K9/2022—Organic macromolecular compounds
- A61K9/205—Polysaccharides, e.g. alginate, gums; Cyclodextrin
- A61K9/2059—Starch, including chemically or physically modified derivatives; Amylose; Amylopectin; Dextrin
-
- 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
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- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Physics & Mathematics (AREA)
- Chemical & Material Sciences (AREA)
- Natural Medicines & Medicinal Plants (AREA)
- General Health & Medical Sciences (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Epidemiology (AREA)
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- Engineering & Computer Science (AREA)
- Public Health (AREA)
- Veterinary Medicine (AREA)
- Pharmacology & Pharmacy (AREA)
- Animal Behavior & Ethology (AREA)
- Bioinformatics & Cheminformatics (AREA)
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- Biochemistry (AREA)
- General Physics & Mathematics (AREA)
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- Pathology (AREA)
- Botany (AREA)
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Abstract
The invention discloses a kind of coptis particle and its Chinese medicine preparation.Described coptis particle is prepared by the method comprised the following steps：Coptis medicine materical crude slice is taken, is added water to cook 23 times, 5 10 times of amount water are added every time, heating is decocted 12 hours；Decoction merges, and filtrate is concentrated into the clear cream that relative density is 1.02 1.10, is filtered while hot with 250 350 mesh sieves；Qinghuo reagent is spray-dried, and obtains spray powder；By spray powder dry granulation, coptis particle of the granularity in 16 40 mesh is obtained.The coptis granule preparing process 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 coptis particle and comprising in coptis particle
Medicine preparation.
Background technology
This product is ranunculaceae plant coptis Coptis chinensis Franch., triangle leaf coptis Coptis
Deltoidea C.Y.Cheng et Hsiao or cloud connect Coptis teeta wall. dry rhizome, bitter, tremble with fear, the thoughts of returning home, spleen,
Stomach, liver, courage, large intestine channel, with heat-clearing and damp-drying drug, effect of purging intense heat and detonicating.
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 coptis particle needs several hours, operation with reference to the method for pharmacopeia
Also it is more complicated.The main chemical compositions of coptis particle are palmatine, epiberberine, coptisine, jamaicin, are referred to as quality control
Mark, conventional method need to often carry out numerous and diverse pretreatment using high performance liquid chromatography etc. to sample, expend substantial amounts of reagent, right
Environmental pollution is larger and inspector's body has been damaged, and feedback of the information is delayed, it is impossible to meet particle enterprise large-scale production process
The need for middle instant analysis multi items, many batch samples.
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 Huang of production technology standardization
Connect particle, its preparation technology is simple, steady quality.Meanwhile, in order to better control over the quality of coptis particle, adapt to industrial metaplasia
Product batch is additionally provided a kind of fast and accurately fast based on near-infrared spectrum technique in the demand of X -ray inspection X during production
The method of speed detection coptis particle.
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 coptis particle, prepared by the method comprised the following steps：The coptis is taken to drink
Piece, is added water to cook 2-3 times, adds 5-10 times to measure water every time, heating is decocted 1-2 hours；Decoction merges, and filtrate is concentrated into relative density
For 1.02-1.10 clear cream, filtered while hot with 250-350 mesh sieves；Qinghuo reagent is spray-dried, and obtains spray powder；By spray powder
Dry granulation, obtains coptis particle of the granularity in 16-40 mesh.
Present inventor has found that the coptis adds water to cook 2-3 times by long term test, and adding 5-10 times every time measures water, plus
Heat is decocted and can more completely extracted active ingredient for 1-2 hours.And it is 1.02-1.10's to concentrate the filtrate to relative density
Clear cream, is filtered with 250-350 mesh sieves, can quickly be removed the moisture in clear cream by the method for spray drying while hot, and anti-
Only cause the loss of active ingredient because heated time is longer.
Preferably, coptis particle of the invention is prepared by the method comprised the following steps：Coptis medicine materical crude slice is taken, is added water pan-fried
Boil 3 times, 8 times of amount water are added every time, heating every time is decocted 1.5 hours；Decoction merge, filtrate be concentrated into relative density for 1.08 it is clear
Cream, is filtered with 350 mesh sieves while hot；In 170-185 DEG C of EAT, 400-700 revs/min of revolution speed, leaving air temp 85-95 are expected
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 frequency
Dry granulation under the conditions of rate 40HZ, feeding motor frequency 45HZ, oil cylinder working-pressure 20bar, obtains the coptis of the granularity in 16-40 mesh
Grain.
Moisture≤8.0% in the process for producing optimized by the present invention, gained coptis particle, ethanol soluble extraction >=
34.0%, palmatine >=26.0mg/g, epiberberine >=17.0mg/g, coptisine >=26.0mg/g, jamaicin >=104.0mg/
g。
The coptis particle of the present invention can be further applied in various Chinese medicine preparations, to realize the pharmacological activity of the coptis.Often
The Chinese medicine preparation comprising coptis particle seen is known in the art, those skilled in the art can be combined as needed and
Using.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 coptis particle of the present invention, and it is based on near-infrared spectrum technique quick detection, and wraps
Include following steps：
The collection of a.NIR spectrum：Coptis particulate samples about 3g is taken, fine powder is ground into, near infrared spectrum scanning is carried out, light is gathered
Spectrum, obtains the original absorbance spectrogram of coptis particulate samples, and each component content is measured, and measures coptis particulate samples each
The measured value of constituent content, determines that calibration set and checking collect according to sample number and sample each component content actual measurement Distribution value；
B. the foundation of coptis particle quantitative model：Coptis granule moisture level is determined, using subtracting straight line method to original
Beginning absorption spectrum is pre-processed, and the spectral region of modeling chooses 5451.7-4247.9cm-1Characteristic wave bands, dimension elects 9 as；Survey
Determine coptis particle ethanol soluble extraction content, original absorbance spectrum is pre-processed using without spectrum facture, the spectrum of modeling
Scope chooses 9401.7-6096.4cm-1Characteristic wave bands, dimension elects 5 as；Coptis particle palmatine content is determined, is led using single order
Number+vector normalization method is pre-processed to original absorbance spectrum, and the spectral region of modeling chooses 6100.5-4598.8cm-1It is special
Wave band is levied, dimension elects 7 as；Coptis particle epiberberine content is determined, using first derivative+vector normalization method to original absorbance
Spectrum is pre-processed, and the spectral region of modeling chooses 9401.7-7496cm-1And 4602.9-4247.9cm-1Characteristic wave bands, dimension
Number elects 5 as；Coptis particle coptis alkali content is determined, original absorbance spectrum is carried out using first derivative+vector normalization method pre-
Processing, the spectral region of modeling chooses 7500.1-4598.8cm-1Characteristic wave bands, dimension elects 7 as；Determine coptis particle jamaicin
Content, is pre-processed using first derivative+subtract straight line method to original absorbance spectrum, and the spectral region of modeling is chosen
6100.5-4598.8cm-1Characteristic wave bands dimension elects 7 as；With PLS is to the near infrared spectrum of calibration set and its is right
Quantitative model is set up between the measured value for answering coptis particulate samples 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 coptis particulate samples each component content, predicted value is compared with measured value, verifies
The accuracy of quantitative model；
D. the measure of coptis particle each component content：Coptis particle 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 containing for coptis particle each component
Amount；The near-infrared of the coptis pellet moisture, extract and the palmatine that are built up, epiberberine, coptisine, jamaicin is quantitatively surveyed
Cover half type is integrated by near-infrared analysis software, sets up the multi-method evaluation model of coptis particle, by coptis particle to be detected
Sample gathers near infrared spectrum according to step a method, imports in coptis particle multi-method evaluation model, while determining the coptis
Grain each component content.
Using above-mentioned detection method, moisture, ethanol soluble extraction and palmatine, the table barberry of coptis particle can be determined simultaneously
Alkali, coptisine, content of berberine, it is only necessary to which a few minutes just can complete the detection of each group divided data, substantially reduce detection time,
Adapt to the demand that modern enterprise is quick, largely produce.And traditional detection method, using high effective liquid chromatography for measuring bar horse
Spit of fland, epiberberine, coptisine, content of berberine, moisture analysis content, ethanol soluble extractives determination method determine ethanol leaching
Apparent extract, it is cumbersome, a variety of instrument and equipments are not only needed, also needing each to examine post to cooperate can just smoothly complete,
Data handling procedure is more complicated, time-consuming.In addition, the method for the present invention can be applicable each group of the material of 3 production links simultaneously
Divide assay, including medicinal extract, spray dried powder, particle.
In order to more accurately determine, in the assay method of the present invention, the sample preparation that coptis particle near-infrared is determined
Method is：Same batch coptis particle about 3g is taken, fine powder is ground into, 80 mesh sieves are crossed, the tool plug of near-infrared measure is transferred to
In vial.Preferably, grinding fine powder is shifted using funnel, makes it close by way of up-down vibration, use rubber
Bottle stopper is stoppered.It is highly preferred that under the conditions of 18-22 DEG C of temperature, humidity 40-50%, particle is ground with quickly bottling.
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 near to sample
IR 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 coptis medicinal extract, appropriate amount of auxiliary materials can be added by technological requirement, then with micro-
Ripple stove rapid draing, dry extract can complete detection by particl method is determined, for spray dried powder, then directly by measure particle
Method, greatly reduces the workload of model foundation, realizes the quality control to each key link material of coptis particle.
Preferably, in step a, the condition of scanning of described NIR 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.In the quantitative determination of coptis particle each component near-infrared
On the basis of model, coptis particle multi-method evaluation model is established, moisture in sample, second can be drawn by the collection of a spectrum
The multicomponent content results such as alcohol extract and palmatine, epiberberine, coptisine, jamaicin, while according to mahalanobis distance and group
Point density etc. can distinguish the kind true and false again.
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 work of coptis particle
Skill, and preparation technology is simple, technological parameter is stable and easy to control, is adapted to the preparation of coptis root dispensing granule.(2) present invention is based near
Infrared spectrum technology combination chemometrics method, in certain spectral region, establishes coptis particle near-infrared quantitative model,
For Qualitive test, without carrying out complicated pre-treatment to sample, fine powder can be ground into, any examination is not related to simultaneously
Agent, it is environmentally friendly, safe and nontoxic, it is the trend of Quality Control job development from now on, is provided for detection coptis particle a kind of quick, accurate
New method.The online quality-monitoring in Chinese medicinal granule enterprise production process can be promoted the use as a kind of practical approach, it is right
Abnormal products can be pointed out in time, it is ensured that the stabilization of production quality, feasible.
Brief description of the drawings
The near-infrared original absorbance spectrogram of Fig. 1 coptis particulate samples；
Related figure between Fig. 2 coptiss pellet moisture near-infrared predicted value and measured value；
The comparison column diagram of Fig. 3 coptiss pellet moisture near-infrared predicted value and measured value；
Related figure between Fig. 4 coptis particle ethanol soluble extraction near-infrared predicted values and measured value；
The comparison column diagram of Fig. 5 coptis particle ethanol soluble extraction near-infrared predicted values and measured value；
Related figure between Fig. 6 coptis particle palmatine near-infrared predicted values and measured value；
The comparison column diagram of Fig. 7 coptis particle palmatine near-infrared predicted values and measured value；
Related figure between Fig. 8 coptis particle epiberberine near-infrared predicted values and measured value；
The comparison column diagram of Fig. 9 coptis particle epiberberine near-infrared predicted values and measured value；
Related figure between Figure 10 coptis particle coptisine near-infrared predicted values and measured value；
The comparison column diagram of Figure 11 coptis particle coptisine near-infrared predicted values and measured value；
Related figure between Figure 12 coptis particle jamaicin near-infrared predicted values and measured value；
The comparison column diagram of Figure 13 coptis particle jamaicin near-infrared predicted values 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 coptis particle：Coptis medicine materical crude slice is taken, is added water to cook 3 times, 8 times of amount water are added every time, it is small that each heating decocts 1.5
When；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；In EAT
175 DEG C, expect 500 revs/min of revolution speed, 90 DEG C of leaving air temp, wind is spray-dried under conditions of sending 40 DEG C of temperature, obtains spray drying
Powder；Done under the conditions of punching panel aperture 1.50mm, roller motor frequency 40HZ, feeding motor frequency 45HZ, oil cylinder working-pressure 20bar
Method is pelletized, and obtains coptis particle of the granularity in 40 mesh.
Embodiment 2：
The preparation of the Chinese medicine preparation of the particle containing the coptis：Coptis medicine materical crude slice is taken, is added water to cook 3 times, 8 times of amount water are added every time, every time
Heating is decocted 1.5 hours；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
Cross；In 175 DEG C of EAT, 500 revs/min of revolution speed is expected, 90 DEG C of leaving air temp, wind is sprayed under conditions of sending 40 DEG C of temperature
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 coptis particle of the granularity in 40 mesh；230g coptiss particle and 115g maltodextrins are mixed,
Appropriate magnesium stearate is added, mixes, is pressed into 1000.
Embodiment 3：
A kind of method based on near-infrared spectrum technique quick detection coptis granule moisture level, specifically includes following step
Suddenly：
A, coptis particulate samples are taken, totally 53 batches, respectively take about 3g, be ground into fine powder, be fitted into tool plug glass sample bottle, be placed near
It is scanned on infrared scanner, gathers spectrum, the condition of scanning：Scanning range 4000-12000cm-1, scanning times：32 times,
Resolution ratio 8cm-1, background correction in real time in scanning process, 3 spectrum of every part of sample collection obtain 53 batches of coptiss as shown in Figure 1
The near-infrared original absorbance spectrogram of particle；
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 coptis particle about 2g, is laid in and dries into the flat measuring cup of constant weight, accurately weighed, opens bottle cap in 100-
105 DEG C of dryings 5 hours, bottle cap is covered, in dislocation drier, is cooled down 30 minutes, accurately weighed, then dries 1 in said temperature
Hour, cooling is weighed, untill the double difference weighed is no more than 5mg；According to the weight of less loss, coptis particle is calculated
Water content (%), according to sample number and sample distribution determine calibration set and checking collect；
B, Distribution value surveyed according to sample number and sample moisture, it is calibration set to choose 43 batches, and it is checking to choose 10 batches
Collection.Analysis software, Automatic Optimal chooses preprocess method and spectral region, and optimum results are shown in Table 1.Using first derivative+
Subtract straight line method to pre-process near-infrared original absorbance spectrum, choose 7500.1-4247.9cm-1Under characteristic wave bands
Spectral information, the quantitative model set up with PLS (PLS) between near infrared spectrum and moisture measured value；Will
The sample of checking collection carries out near infrared spectrum scanning, using model, the predicted value of coptis particulate samples content is obtained, by predicted value
It is compared with measured value, verifies the accuracy and predictive ability of quantitative model, the model obtains cross validation phase through cross validation
Close coefficients R2=0.904, RMSECV=0.151, RPD=3.23, dimension elect 8, checking collection coefficient R as2=0.925,
RMSEP=0.093, the determination of moisture of 10 batches of coptis particles the results are shown in Table 2, related between moisture predicted value and measured value
Figure 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 10 batches of coptis particles of table
The deviation range of coptis granule moisture level is between 0.03-0.14% it can be seen from upper table 2, consensus forecast
The rate of recovery is 100.33%, illustrates that the model has preferable predictive ability and stability, available for the fast of coptis pellet moisture
Speed detection.
Embodiment 4：
A kind of method based on near-infrared spectrum technique quick detection coptis particle ethanol soluble extraction content, specifically include as
Lower step：
A, coptis particulate samples are taken, totally 53 batches, respectively take about 3g, be ground into fine powder, be fitted into tool plug glass sample bottle, be placed near
It is scanned on infrared scanner, gathers spectrum, the condition of scanning：Scanning range 4000-12000cm-1, scanning times：32 times,
Resolution ratio 8cm-1, background correction in real time in scanning process, 3 spectrum of every part of sample collection obtain 53 batches of coptiss as shown in Figure 1
The near-infrared original absorbance spectrogram of particle；
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 coptis particle 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, the content of ethanol soluble extractives in coptis particle is calculated with dry product
(%), determines 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 44 batches, chooses 9 batches and is
Checking collection.Analysis software, Automatic Optimal chooses preprocess method and spectral region, and optimum results are shown in Table 3.Using without spectrum
Facture is pre-processed to near-infrared original absorbance spectrum, chooses 9401.7-6096.4cm-1Spectrum letter under characteristic wave bands
Breath, the quantitative model set up with PLS (PLS) between near infrared spectrum and ethanol soluble extraction content measured value；Will
The sample of checking collection carries out near infrared spectrum scanning, using model, the predicted value of coptis particulate samples content is obtained, by predicted value
It is compared with measured value, verifies the accuracy and predictive ability of quantitative model, the model obtains cross validation phase through cross validation
Close coefficients R2=0.96, RMSECV=1.2, RPD=5, dimension elect 5, checking collection coefficient R as2=0.936, RMSEP=
The ethanol soluble extraction assay of 1.2,9 batches of coptis particles the results are shown in Table 4, the phase between ethanol soluble extraction predicted value and measured value
Pass figure 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 49 batches of coptis particles of table
The deviation range of coptis particle ethanol soluble extraction content is between 0.19-1.96% it can be seen from upper table 4, in advance
It is 99.11% to survey average recovery rate, illustrates that the model has preferable predictive ability and stability, available for coptis particle ethanol
The quick detection of extract.
Embodiment 5：
One kind is based on palmatine, epiberberine, coptisine, jamaicin in near-infrared spectrum technique quick detection coptis particle
The method of content, specifically includes following steps：
A, coptis particulate samples are taken, totally 53 batches, respectively take about 3g, be ground into fine powder, be fitted into tool plug glass sample bottle, be placed near
It is scanned on infrared scanner, gathers spectrum, the condition of scanning：Scanning range 4000-12000cm-1, scanning times：32 times,
Resolution ratio 8cm-1, background correction in real time in scanning process, 3 spectrum of every part of sample collection obtain 53 batches of coptiss as shown in Figure 1
The near-infrared original absorbance spectrogram of particle；
Meanwhile, the standard method according to specified in 2015 editions Chinese Pharmacopoeias, its palmatine, epiberberine, coptisine, barberry
Alkali content according to 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 acetonitrile-
0.05mol/L potassium dihydrogen phosphates (50: 50) (add lauryl sodium sulfate 0.4g, then use phosphorus acid for adjusting pH value in per 100ml
4.0) to be mobile phase；Detection wavelength is 345nm.Number of theoretical plate is calculated by jamaicin peak should be not less than 5000.
The preparation of reference substance solution：Take Berberine hydrochloride reference substance appropriate, it is accurately weighed, plus every 1ml is made containing 45 μ in methanol
G solution, is produced.
The preparation of need testing solution：This product under content uniformity is taken, it is finely ground, about 0.1g is taken, it is accurately weighed, put tool plug cone
In shape bottle, precision adds the mixed solution 50ml of methanol-hydrochloric acid (100: 1), close plug, weighed weight, ultrasonically treated 30 minutes (work(
Rate 300W, frequency 40kHZ), let cool, then weighed weight, the weight of less loss is supplied with methanol, is shaken up, is filtered, precision measures continuous filter
Liquid 1ml, puts in 10ml measuring bottles, plus methanol is to scale, shakes up, filtration, takes subsequent filtrate, produces.
Determination method：It is accurate respectively to draw reference substance solution and each 10 μ l of need testing solution, liquid chromatograph is injected, is determined,
Using the peak area of jamaicin reference substance as control, the content of palmatine, epiberberine, coptisine and jamaicin is calculated respectively, is used
The relative retention time of composition chromatographic peak to be measured and jamaicin chromatographic peak is determined.
Epiberberine, coptisine, palmatine, the peak position of jamaicin, its relative retention time should setting ± 5% model
Within enclosing, produce.Relative retention time see the table below：
B, Distribution value surveyed according to sample number and sample epiberberine, coptisine, palmatine, content of berberine, choose 43
It is calibration set to criticize, and chooses 10 batches and collects for checking.Analysis software, Automatic Optimal chooses preprocess method and spectral region, excellent
Change the results are shown in Table 5.Original absorbance spectrum is pre-processed using first derivative+vector normalization method, 6100.5- is chosen
4598.8cm-1Spectral information under characteristic wave bands, near infrared spectrum and palmatine standard are set up with PLS (PLS)
Quantitative model between content；Original absorbance spectrum is pre-processed using first derivative+vector normalization method, chosen
9401.7-7496cm-1And 4602.9-4247.9cm-1Spectral information under characteristic wave bands, builds with PLS (PLS)
Vertical quantitative model between near infrared spectrum and epiberberine standard content；Using first derivative+vector normalization method to original
Absorption spectrum is pre-processed, and chooses 7500.1-4598.8cm-1Spectral information under characteristic wave bands, with PLS
(PLS) quantitative model set up between near infrared spectrum and coptisine standard content；Using first derivative+subtract straight line method
Original absorbance spectrum is pre-processed, 6100.5-4598.8cm is chosen-1Information under characteristic wave bands spectrum, with partially minimum
The quantitative model that square law (PLS) is set up between near infrared spectrum and coptisine standard content.The sample for verifying collection is carried out near
IR spectrum scanning, using model, obtains the predicted value of coptis particulate samples content, predicted value is compared with measured value,
The accuracy and predictive ability of quantitative model are verified, palmatine quantitative model obtains cross validation coefficient R through cross validation2=
0.924, RMSECV=0.994, RPD=3.63, dimension elect 7, checking collection coefficient R as2=0.941, RMSEP=0.946；
Epiberberine quantitative model obtains cross validation coefficient R through cross validation2=0.928, RMSECV=0.072, RPD=
3.74, dimension elects 5, checking collection coefficient R as2=0.980, RMSEP=0.372；Coptisine quantitative model is through cross validation
Obtain cross validation coefficient R2=0.937, RMSECV=1.09, RPD=3.99, dimension elect 7, checking collection coefficient R as2
=0.929, RMSEP=1.17；Jamaicin quantitative model obtains cross validation coefficient R through cross validation2=0.922,
RMSECV=3.36, RPD=3.58, dimension elect 7, checking collection coefficient R as2=0.943, RMSEP=3.64.10 batches of coptiss
Palmatine, epiberberine, coptisine and the content of berberine measurement result of particle are shown in Table 6, palmatine, epiberberine, coptisine
Related figure between jamaicin predicted value and measured value is shown in Fig. 6,8,10,12, palmatine, epiberberine, coptisine and barberry
The comparison column diagram of alkali predicted value and measured value is shown in Fig. 7,9,11,13.
The palmatine of table 5, the mould of epiberberine, coptisine, jamaicin model under different spectral regions and preprocess method
Shape parameter
Table 6 10 batches of coptis particle palmatines, epiberberine, coptisine, content of berberine measurement results
The deviation range of coptis particle palmatine is between 0.01-1.76mg/g it can be seen from upper table 6, and prediction is average
The rate of recovery is 100.47%；The deviation range of epiberberine is between 0.02-0.51mg/g, and prediction average recovery rate is
100.47%；The deviation range of coptisine is between 0.15-0.96mg/g, and prediction average recovery rate is 100.41%；Jamaicin
Deviation range between 0.17-5.17mg/g, prediction average recovery rate be 99.93%.Illustrate that the model has preferably pre-
Survey ability and stability, available for coptis particle palmatine, epiberberine, coptisine, jamaicin quick detection.
Embodiment 6:
A kind of method based on near-infrared spectrum technique Fast Evaluation coptis granular mass, specifically includes following steps：
A. software is used, by coptis particle palmatine, epiberberine, coptisine, jamaicin, moisture and the extract built
Quantitative model is imported, and sets the content limit of each component, according to the quality standard of coptis particle, sets moisture≤8.0%,
Ethanol soluble extraction >=34.0%, palmatine >=26.0mg/g, epiberberine >=17.0mg/g, coptisine >=26.0mg/g, barberry
Alkali >=104.0mg/g, sets up the multi-method evaluation model of coptis particle；
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 the coptis, radix bupleuri etc. 10 batches
Particulate samples are evaluated, and sample message table is shown in Table 7.The spectrogram of the sample of numbering 1~10 is gathered respectively, spectrogram is imported yellow
Even in particle 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 coptis particle 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 coptis particle with principium identification institute test sample product, be identified as coptis particle
Sample can draw the accurate predictor of each component simultaneously.Illustrate that the model has preferable predictive ability and accuracy, can be quick
Evaluate the quality of coptis particle.
Claims (6)
1. a kind of detection method of coptis particle, it is characterised in that be the detection method based on near-infrared spectrum technique, and including
Following steps：
The collection of a.NIR spectrum：Coptis particulate samples about 3g is taken, fine powder is ground into, near infrared spectrum scanning is carried out, spectrum is gathered,
The original absorbance spectrogram of coptis particulate samples is obtained, and each component content is measured, coptis particulate samples each group is measured
Divide the measured value of content, determine that calibration set and checking collect according to sample number and sample each component content actual measurement Distribution value；Described
The condition of scanning of near infrared spectra collection is：Scanning range is 4000cm-1-12000cm-1, scanning times are 32 times, resolution ratio
For 8cm-1, background correction, 3 spectrum of every part of sample collection in real time in scanning process.
B. the foundation of coptis particle quantitative model：Coptis granule moisture level is determined, is inhaled using straight line method is subtracted to original
Receive spectrum to be pre-processed, the spectral region of modeling chooses 5451.7-4247.9cm-1Characteristic wave bands, dimension elects 9 as；Determine yellow
Even particle ethanol soluble extraction content, is pre-processed, the spectral region of modeling using without spectrum facture to original absorbance spectrum
Choose 9401.7-6096.4cm-1Characteristic wave bands, dimension elects 5 as；Coptis particle palmatine content is determined, using first derivative+arrow
Amount normalization method is pre-processed to original absorbance spectrum, and the spectral region of modeling chooses 6100.5-4598.8cm-1Characteristic wave
Section, dimension elects 7 as；Coptis particle epiberberine content is determined, using first derivative+vector normalization method to original absorbance spectrum
Pre-processed, the spectral region of modeling chooses 9401.7-7496cm-1And 4602.9-4247.9cm-1Characteristic wave bands, dimension choosing
For 5；Coptis particle coptis alkali content is determined, original absorbance spectrum is pre-processed using first derivative+vector normalization method,
The spectral region of modeling chooses 7500.1-4598.8cm-1Characteristic wave bands, dimension elects 7 as；Coptis particle content of berberine is determined,
Original absorbance spectrum is pre-processed using first derivative+subtract straight line method, the spectral region of modeling chooses 6100.5-
4598.8cm-1Characteristic wave bands dimension elects 7 as；With PLS to the near infrared spectrum of calibration set and its correspondence coptis
Quantitative model is set up between the measured value of grain 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 coptis particulate samples each component content, predicted value is compared with measured value, and checking is quantitative
The accuracy of model；
D. the measure of coptis particle each component content：Coptis particle to be detected is taken to carry out near infrared light according to step a method
In spectrum collection, the quantitative model that specific band spectral information steps for importing b is set up, the content of coptis particle each component is determined；
The near-infrared of the coptis pellet moisture, extract and the palmatine that are built up, epiberberine, coptisine, jamaicin is quantitative determined
Model is integrated by near-infrared analysis software, sets up the multi-method evaluation model of coptis particle, by coptis granular to be detected
Product gather near infrared spectrum according to step a method, import in coptis particle multi-method evaluation model, while determining coptis particle
Each component content；
Described coptis particle is prepared by the method comprised the following steps：Coptis medicine materical crude slice is taken, is added water to cook 2-3 times, every time
Plus 5-10 times measured water, heating is decocted 1-2 hours；Decoction merges, and filtrate is concentrated into the clear cream that relative density is 1.02-1.10, takes advantage of
Heat is filtered with 250-350 mesh sieves；Qinghuo reagent is spray-dried, and obtains spray powder；By spray powder dry granulation, granularity is obtained in 16-
The coptis particle of 40 mesh；Moisture≤8.0% in coptis particle, ethanol soluble extraction >=34.0%, palmatine >=26.0mg/g, table
Jamaicin >=17.0mg/g, coptisine >=26.0mg/g, jamaicin >=104.0mg/g.
2. the detection method of coptis particle as claimed in claim 1, it is characterised in that described coptis particle is by including as follows
The method of step is prepared：Coptis 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 hours；
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, expect 400-700 revs/min of revolution speed, 85-95 DEG C of leaving air temp, wind is spray-dried under conditions of sending 35-45 DEG C of temperature,
Obtain spray powder；In punching panel aperture 1.50mm, roller motor frequency 40HZ, feeding motor frequency 45HZ, oil cylinder working-pressure 20bar bars
Dry granulation under part, obtains coptis particle of the granularity in 16-40 mesh.
3. the detection method of coptis particle as claimed in claim 1 or 2, it is characterised in that the sample that coptis particle near-infrared is determined
Product preparation method is：Same batch coptis particle about 3g is taken, fine powder is ground into, 80 mesh sieves are crossed, near-infrared measure is transferred to
Tool plug vial in.
4. the detection method of coptis particle as claimed in claim 1 or 2, it is characterised in that carry out grinding fine powder using funnel
Transfer, is made it close by way of up-down vibration, is stoppered with bottle closure of rubber.
5. the detection method of coptis particle as claimed in claim 1 or 2, it is characterised in that in 18-22 DEG C of temperature, humidity 40-
Under the conditions of 50%, particle is ground with quickly bottling.
6. the detection method of coptis particle 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.
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| 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 |
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Denomination of invention: A detection method for Huanglian granules 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 |
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