CN106074664B - A kind of detection method of Fructus Corni particle - Google Patents
A kind of detection method of Fructus Corni particle Download PDFInfo
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- CN106074664B CN106074664B CN201610454087.9A CN201610454087A CN106074664B CN 106074664 B CN106074664 B CN 106074664B CN 201610454087 A CN201610454087 A CN 201610454087A CN 106074664 B CN106074664 B CN 106074664B
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- 239000002245 particle Substances 0.000 title claims abstract description 91
- 238000001514 detection method Methods 0.000 title claims abstract description 26
- 241000209020 Cornus Species 0.000 claims abstract description 112
- 235000013399 edible fruits Nutrition 0.000 claims abstract description 111
- 238000000034 method Methods 0.000 claims abstract description 64
- 239000003814 drug Substances 0.000 claims abstract description 31
- 239000000843 powder Substances 0.000 claims abstract description 26
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000007921 spray Substances 0.000 claims abstract description 12
- 239000006071 cream Substances 0.000 claims abstract description 10
- 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
- 238000002329 infrared spectrum Methods 0.000 claims description 27
- AMBQHHVBBHTQBF-UHFFFAOYSA-N Loganin Natural products C12C(C)C(O)CC2C(C(=O)OC)=COC1OC1OC(CO)C(O)C(O)C1O AMBQHHVBBHTQBF-UHFFFAOYSA-N 0.000 claims description 25
- AMBQHHVBBHTQBF-UOUCRYGSSA-N loganin Chemical compound O([C@@H]1OC=C([C@H]2C[C@H](O)[C@H](C)[C@H]21)C(=O)OC)[C@@H]1O[C@H](CO)[C@@H](O)[C@H](O)[C@H]1O AMBQHHVBBHTQBF-UOUCRYGSSA-N 0.000 claims description 25
- 239000000047 product Substances 0.000 claims description 12
- 230000003595 spectral effect Effects 0.000 claims description 12
- 238000001228 spectrum Methods 0.000 claims description 12
- 238000012360 testing method Methods 0.000 claims description 11
- 238000013210 evaluation model Methods 0.000 claims description 10
- 239000008188 pellet Substances 0.000 claims description 8
- 238000000862 absorption spectrum Methods 0.000 claims description 6
- 238000002835 absorbance Methods 0.000 claims description 5
- 238000009826 distribution Methods 0.000 claims description 5
- 239000000463 material Substances 0.000 claims description 5
- 238000003705 background correction Methods 0.000 claims description 4
- 238000005259 measurement Methods 0.000 claims description 4
- 238000004080 punching Methods 0.000 claims description 4
- 238000000227 grinding Methods 0.000 claims description 2
- 238000005507 spraying Methods 0.000 claims description 2
- 238000005464 sample preparation method Methods 0.000 claims 1
- 238000012546 transfer Methods 0.000 claims 1
- 238000002360 preparation method Methods 0.000 abstract description 17
- 239000008187 granular material Substances 0.000 abstract description 12
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 9
- 238000005516 engineering process Methods 0.000 description 8
- 238000004519 manufacturing process Methods 0.000 description 7
- 229940079593 drug Drugs 0.000 description 5
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- 239000013558 reference substance Substances 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
- 238000003556 assay Methods 0.000 description 2
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- 238000000605 extraction Methods 0.000 description 2
- 238000004128 high performance liquid chromatography Methods 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
- 238000002203 pretreatment Methods 0.000 description 2
- 238000004445 quantitative analysis Methods 0.000 description 2
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- 238000010561 standard procedure Methods 0.000 description 2
- 241000846172 Cremastra appendiculata Species 0.000 description 1
- 206010062717 Increased upper airway secretion Diseases 0.000 description 1
- 239000005913 Maltodextrin Substances 0.000 description 1
- 206010054949 Metaplasia Diseases 0.000 description 1
- 241001250598 Pleione bulbocodioides Species 0.000 description 1
- 241001457446 Pleione yunnanensis Species 0.000 description 1
- 240000007164 Salvia officinalis Species 0.000 description 1
- PBCJIPOGFJYBJE-UHFFFAOYSA-N acetonitrile;hydrate Chemical compound O.CC#N PBCJIPOGFJYBJE-UHFFFAOYSA-N 0.000 description 1
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- 230000004069 differentiation Effects 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
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- 235000019634 flavors Nutrition 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 229930182470 glycoside Natural products 0.000 description 1
- 150000002338 glycosides Chemical class 0.000 description 1
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- 230000003179 granulation Effects 0.000 description 1
- 230000003760 hair shine Effects 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 239000007788 liquid Substances 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
- 235000013372 meat Nutrition 0.000 description 1
- 230000015689 metaplastic ossification Effects 0.000 description 1
- 238000012544 monitoring process Methods 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
- 208000026435 phlegm Diseases 0.000 description 1
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Classifications
-
- 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)
- A61K36/40—Cornaceae (Dogwood family)
-
- 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
-
- 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
- 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
Abstract
The invention discloses a kind of dogwood fruit particle and its Chinese medicine preparation.The dogwood fruit particle is prepared by the method comprised the following steps：Dogwood fruit 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, dogwood fruit particle of the granularity in 16 40 mesh is obtained.The dogwood fruit 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 dogwood fruit particle and the dogwood fruit is included
The Chinese medicine preparation of particle.
Background technology
Dogwood fruit is orchid Cremastra appendiculata Cremastra appendiculata (D.Don) Makino, pleione bulbocodioides
Pleione bulbocodioides (Franch.) Rolfe's or Pleione yunnanensis Pleione yunnanensis Rolfe is dry
Dry pseudobulb, sweet, micro-pungent is cool, with clearing heat and detoxicating, effect of reducing phlegm and resolving masses.
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 in traditional dogwood fruit particle needs several hours with reference to the method for pharmacopeia, operates also more complicated.
The main chemical compositions of dogwood fruit particle are loganin, and as quality control index, conventional method uses high performance liquid chromatography
Deng, numerous and diverse pretreatment need to be often carried out to sample, substantial amounts of reagent is expended, environmental pollution it is larger and to inspector's body
Damage, feedback of the information is delayed, it is impossible to meet instant analysis multi items, the need of many batch samples during particle enterprise large-scale production
Will.
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 mountain of production technology standardization
Cornus particle, its preparation technology is simple, steady quality.Meanwhile, in order to better control over the quality of dogwood fruit particle, adapt to work
Product batch is additionally provided a kind of fast and accurately based near infrared spectrum in the demand of X -ray inspection X during the production of industry metaplasia
The method of technology quick detection dogwood fruit 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 dogwood fruit particle, it is characterised in that is prepared by the method comprised the following steps
Obtain：Dogwood fruit medicine materical crude slice is taken, is added water to cook 2-3 times, adding 5-10 times every time measures water, heating every time is decocted 1-2 hours；Decoction is closed
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；It is dry that qinghuo reagent carries out spraying
It is dry, obtain spray powder；By spray powder dry granulation, dogwood fruit particle of the granularity in 16-40 mesh is obtained.
Present inventor has found that dogwood fruit is added 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, dogwood fruit particle of the invention is prepared by the method comprised the following steps：Dogwood fruit 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 dogwood fruit of the granularity in 16-40 mesh
Particle.
Moisture≤8.0% in the process for producing optimized by the present invention, gained dogwood fruit particle, loganin >=
3.0mg/g。
The dogwood fruit particle of the present invention can be further applied in various Chinese medicine preparations, lived with the pharmacology for realizing dogwood fruit
Property.The common Chinese medicine preparation comprising dogwood fruit particle 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 dogwood fruit particle 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：Dogwood fruit 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 dogwood fruit particulate samples is obtained, and each component content is measured, dogwood fruit is measured
The measured value of particulate samples each component content, determines calibration set according to sample number and sample each component content actual measurement Distribution value and tests
Card collection；
B. the foundation of dogwood fruit particle quantitative model：The content of dogwood fruit pellet moisture is determined, using first derivative+MSC
Method is pre-processed to original absorbance spectrum, and the spectral region of modeling chooses 6100.5-5447.6cm-1And 4602.9-
4247.9cm-1Characteristic wave bands, dimension elects 5 as；Dogwood fruit particle Determination of Loganin is determined, is inhaled using First derivative spectrograply to original
Receive spectrum to be pre-processed, the spectral region of modeling chooses 9401.7-8446.8cm-1、6100.5-5447.6cm-1With
4602.9-4247.9cm-1Wave band is characterized, dimension elects 5 as；With PLS to the near infrared spectrum of calibration set and its
Quantitative model is set up between the measured value of correspondence dogwood fruit 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 dogwood fruit particulate samples each component content, predicted value is compared with measured value, tested
Demonstrate,prove the accuracy of quantitative model；
D. the measure of dogwood fruit particle each component content：Dogwood fruit particle 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, dogwood fruit particle each group is determined
The content divided；The near-infrared quantitative determination model of the dogwood fruit pellet moisture built up and loganin is soft by near-infrared analysis
Part is integrated, and the multi-method evaluation model of dogwood fruit particle is set up, by the method for dogwood fruit particulate samples to be detected according to step a
Near infrared spectrum is gathered, is imported in dogwood fruit particle multi-method evaluation model, while determining dogwood fruit particle each component content.
Using above-mentioned detection method, the moisture and Determination of Loganin of dogwood fruit particle can be determined simultaneously, it is only necessary to which a few minutes are just
The detection of each group divided data can be completed, detection time is substantially reduced, the need that modern enterprise is quick, largely produce are adapted to
Ask.And traditional detection method, using high effective liquid chromatography for measuring Determination of Loganin, moisture analysis content, operate numerous
It is trivial, a variety of instrument and equipments are not only needed, also needing each to examine post to cooperate can just smoothly complete, and data handling procedure compares
It is complicated, time-consuming.In addition, the method for the present invention can be applicable each component assay of the material of 3 production links, including leaching simultaneously
Cream, spray dried powder, particle.
In order to more accurately determine, in the assay method of the present invention, the sample system that dogwood fruit particle near-infrared is determined
Preparation Method is：Same batch dogwood fruit particle 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 dogwood fruit medicinal extract, 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
Grain method, greatly reduces the workload of model foundation, realizes the quality control to each key link material of dogwood fruit particle
System.
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 dogwood fruit particle each component near-infrared
On the basis of cover half type, dogwood fruit particle multi-method evaluation model is established, sample reclaimed water can be drawn by the collection of a spectrum
Point and the multicomponent content results such as loganin, while the kind true and false can be distinguished again according to mahalanobis distance and density of fraction etc..
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 dogwood fruit particle
Technique, and preparation technology is simple, technological parameter is stable and easy to control, is adapted to the preparation of dogwood fruit granule.(2) base of the present invention
In near-infrared spectrum technique combination chemometrics method, in certain spectral region, establish dogwood fruit particle 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 dogwood fruit particle
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 dogwood fruit particulate samples；
Related figure between Fig. 2 dogwood fruits pellet moisture near-infrared predicted value and measured value；
The comparison column diagram of Fig. 3 dogwood fruits pellet moisture near-infrared predicted value and measured value；
Related figure between Fig. 4 dogwood fruit particle loganin near-infrared predicted values and measured value；
The comparison column diagram of Fig. 5 dogwood fruit particle loganin 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 dogwood fruit particle：Dogwood fruit 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 dogwood fruit particle of the granularity in 40 mesh.
Embodiment 2：
The preparation of the Chinese medicine preparation of the particle containing dogwood fruit：Dogwood fruit medicine materical crude slice is taken, is added water to cook 3 times, 8 times of amount water are added every time,
Heating is decocted 1.5 hours every time；Decoction merges, and filtrate is concentrated into the clear cream that relative density is 1.08 (80 DEG C), and 350 mesh are used while hot
Sieving；In 175 DEG C of EAT, 500 revs/min of revolution speed, 90 DEG C of leaving air temp are expected, wind send progress under conditions of 40 DEG C of temperature
Spray drying, obtains spray powder；In punching panel aperture 1.50mm, roller motor frequency 40HZ, feeding motor frequency 45HZ, oil cylinder pressure
Dry granulation under the conditions of power 20bar, obtains dogwood fruit particle of the granularity in 40 mesh；By 200g dogwood fruits particle and 85g maltodextrins
Mix, add appropriate magnesium stearate, mix, be pressed into 1000.
Embodiment 3：
A kind of method based on near-infrared spectrum technique quick detection dogwood fruit granule moisture level, specifically includes following step
Suddenly：
A, dogwood fruit particulate samples are taken, totally 83 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 83 batches
The near-infrared original absorbance spectrogram of dogwood fruit 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 dogwood fruit particle 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, dogwood fruit 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 67 batches, and it is checking to choose 16 batches
Collection.Analysis software, Automatic Optimal chooses preprocess method and spectral region, and optimum results are shown in Table 1.Using first derivative+
MSC methods are pre-processed to near-infrared original absorbance spectrum, choose 6100.5-5447.6cm-1, 4602.9-4247.9cm-1It is special
The spectral information under wave band is levied, is set up with PLS (PLS) between near infrared spectrum and moisture measured value
Quantitative model；The sample for verifying collection is subjected near infrared spectrum scanning, using model, the pre- of dogwood fruit particulate samples content is obtained
Measured value, predicted value is compared with measured value, verifies the accuracy and predictive ability of quantitative model, the model is through cross validation
Obtain cross validation coefficient R2=0.860, RMSECV=0.132, RPD=2.66, dimension elect 5, checking collection coefficient R as2
The determination of moisture of=0.952, RMSEP=0.058,16 batch dogwood fruit particle the results are shown in Table 2, and moisture predicted value is with surveying
Related figure between 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 16 batches of dogwood fruit particles of table
The deviation range of dogwood fruit granule moisture level is between 0-0.11% it can be seen from upper table 2, and consensus forecast is returned
Yield is 100.44%, illustrates that the model has preferable predictive ability and stability, available for the fast of dogwood fruit pellet moisture
Speed detection.
Embodiment 4：
A kind of method of Determination of Loganin in quick detection dogwood fruit particle based on near-infrared spectrum technique, specifically include as
Lower step：
A, dogwood fruit particulate samples are taken, totally 83 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 83 batches
The near-infrared original absorbance spectrogram of dogwood fruit particle；
Meanwhile, the standard method according to specified in 2015 editions Chinese Pharmacopoeias, its Determination of Loganin 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 acetonitrile-water (15:
85) it is mobile phase；Detection wavelength is 240nm.Number of theoretical plate is calculated by loganin peak should be not less than 3000.
The preparation of reference substance solution：Precision weighs loganin reference substance in right amount, plus 80% methanol is made every 1ml and contains 40 μ g's
Solution, is produced.
The preparation of need testing solution：This product powder about 0.25g is taken, it is accurately weighed, put in conical flask with cover, precision is added
80% methanol 25ml, weighed weight is heated to reflux 1 hour, let cool, then weighed weight, and the weight of less loss is supplied with 80% methanol,
Shake up, filter, take subsequent filtrate, produce.
Determination method：It is accurate respectively to draw reference substance solution and each 5 μ l of need testing solution, liquid chromatograph is injected, is determined, i.e.,
.
B, Distribution value surveyed according to sample number and sample Determination of Loganin, it is calibration set to choose 68 batches, chooses 15 batches to test
Card collection.Analysis software, Automatic Optimal chooses preprocess method and spectral region, and optimum results are shown in Table 3.Using first derivative
Method is pre-processed to near-infrared original absorbance spectrum, chooses 9401.7-8446.8cm-1、6100.5-5447.6cm-1With
4602.9-4247.9cm-1Spectral information under characteristic wave bands, near infrared spectrum and horse are set up with PLS (PLS)
Quantitative model between money glycosides standard content；The sample for verifying collection is subjected near infrared spectrum scanning, using model, mountain cornel is obtained
The predicted value of meat particulate samples content, predicted value is compared with measured value, verifies the accuracy and prediction energy of quantitative model
Power, the model obtains cross validation coefficient R through cross validation2=0.960, RMSECV=0.272, RPD=4.98, dimension choosing
For 5, checking collection coefficient R2The determination of loganin content result of=0.937, RMSECV=0.348,15 batch dogwood fruit particle
4 are shown in Table, the related figure between loganin predicted value and measured value is shown in Fig. 4, loganin predicted value and measured value comparison column diagram
See Fig. 5.
Model parameter of the loganin model of table 3 under different spectral regions and preprocess method
4 15 batches of dogwood fruit particle determination of loganin content results of table
The deviation range of dogwood fruit particle loganin is between 0-0.70mg/g it can be seen from upper table 4, and prediction is average to return
Yield is 101.88%.Illustrate that the model has preferable predictive ability and stability, the quick inspection available for dogwood fruit particle
Survey.
Embodiment 5：
A kind of method based on near-infrared spectrum technique Fast Evaluation dogwood fruit granular mass, specifically includes following steps：
A. software is used, the dogwood fruit particle loganin built, water and basis weight model are imported, and set containing for each component
Limit is measured, according to the quality standard of dogwood fruit particle, loganin >=3.0mg/g is set, dogwood fruit particle is set up in moisture≤8.0
Multi-method evaluation model；
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 dogwood fruit, red sage root etc. 10
Criticize particulate samples to be evaluated, sample message table is shown in Table 5.The spectrogram of the sample of numbering 1~10 is gathered respectively, and spectrogram is imported
In dogwood fruit particle multi-method evaluation model, the content and evaluation information of sample each component are read, 6 are the results are shown in Table.
The multi-method evaluation model verification sample information table of table 5
The dogwood fruit particle multi-method evaluation result of table 6
- 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 6, 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 dogwood fruit particle with principium identification institute test sample product, be identified as dogwood fruit
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 dogwood fruit particle.
Claims (6)
1. a kind of detection method of Fructus Corni particle, 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：Dogwood fruit particulate samples about 3g is taken, fine powder is ground into, near infrared spectrum scanning, collection is carried out
Spectrum, obtains the original absorbance spectrogram of dogwood fruit particulate samples, and each component content is measured, and measures dogwood fruit particle
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 dogwood fruit particle quantitative model：The content of dogwood fruit pellet moisture is determined, using first derivative+MSC methods pair
Original absorbance spectrum is pre-processed, and the spectral region of modeling chooses 6100.5-5447.6cm-1And 4602.9-4247.9cm-1
Characteristic wave bands, dimension elects 5 as；Dogwood fruit particle Determination of Loganin is determined, original absorbance spectrum is carried out using First derivative spectrograply
Pretreatment, the spectral region of modeling chooses 9401.7-8446.8cm-1、6100.5-5447.6cm-1And 4602.9-4247.9cm-1
Wave band is characterized, dimension elects 5 as；With PLS to the near infrared spectrum of calibration set and its correspondence dogwood fruit granular
Quantitative model is set up between the measured value of product 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 dogwood fruit particulate samples each component content, predicted value is compared with measured value, and checking is fixed
Measure the accuracy of model；
D. the measure of dogwood fruit particle each component content：Dogwood fruit 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 dogwood fruit particle each component
Content；The near-infrared quantitative determination model of the dogwood fruit pellet moisture built up and loganin is whole by near-infrared analysis software
Close, set up the multi-method evaluation model of dogwood fruit particle, dogwood fruit particulate samples to be detected are gathered according to step a method
Near infrared spectrum, is imported in dogwood fruit particle multi-method evaluation model, while determining dogwood fruit particle each component content；
Described Fructus Corni particle is prepared by the method comprised the following steps：Dogwood fruit 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 dogwood fruit particle in 16-40 mesh；Moisture≤8.0% in dogwood fruit particle in Fructus Corni particle, loganin >=
3.0mg/g。
2. the detection method of Fructus Corni particle as claimed in claim 1, it is characterised in that described Fructus Corni particle by including
The method of following steps is prepared：Dogwood fruit 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 dogwood fruit particle of the granularity in 16-40 mesh.
3. the detection method of Fructus Corni particle as claimed in claim 1 or 2, it is characterised in that Fructus Corni particle near-infrared is determined
Sample preparation methods be：Same batch Fructus Corni particle 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 Fructus Corni particle 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 Fructus Corni particle 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 Fructus Corni 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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| CN104568813A (en) * | 2014-12-19 | 2015-04-29 | 浙江大学 | Multi-index fast detection method of dogwood medicinal materials |
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Denomination of invention: A detection method for Cornus officinalis granules Effective date of registration: 20231225 Granted publication date: 20170926 Pledgee: Bank of China Limited by Share Ltd. Foshan branch Pledgor: GUANGDONG YIFANG PHARMACEUTICAL Co.,Ltd. Registration number: Y2023980073969 |