CN106074700B - A kind of detection method of radix scutellariae particle - Google Patents
A kind of detection method of radix scutellariae particle Download PDFInfo
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- 239000002245 particle Substances 0.000 title claims abstract description 102
- 238000001514 detection method Methods 0.000 title claims abstract description 29
- 238000000034 method Methods 0.000 claims abstract description 74
- 239000000843 powder Substances 0.000 claims abstract description 27
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000007921 spray Substances 0.000 claims abstract description 11
- 239000000706 filtrate Substances 0.000 claims abstract description 10
- 239000006071 cream Substances 0.000 claims abstract description 9
- 240000004534 Scutellaria baicalensis Species 0.000 claims abstract description 7
- 235000017089 Scutellaria baicalensis Nutrition 0.000 claims abstract description 7
- 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 57
- 238000002329 infrared spectrum Methods 0.000 claims description 26
- 238000000605 extraction Methods 0.000 claims description 22
- XDQITMCFPPPMBC-TUANDBMESA-N scutelloside Natural products OC[C@H]1O[C@@H](O[C@@H]2O[C@@H]3C[C@H]4[C@H](O)[C@@H](O)[C@@](O)(CO3)[C@@H]24)[C@H](O)[C@@H](O)[C@@H]1O XDQITMCFPPPMBC-TUANDBMESA-N 0.000 claims description 19
- 238000001228 spectrum Methods 0.000 claims description 19
- 230000003595 spectral effect Effects 0.000 claims description 14
- 238000000862 absorption spectrum Methods 0.000 claims description 10
- 238000013210 evaluation model Methods 0.000 claims description 10
- 238000012360 testing method Methods 0.000 claims description 10
- IPQKDIRUZHOIOM-UHFFFAOYSA-N Oroxin A Natural products OC1C(O)C(O)C(CO)OC1OC(C(=C1O)O)=CC2=C1C(=O)C=C(C=1C=CC=CC=1)O2 IPQKDIRUZHOIOM-UHFFFAOYSA-N 0.000 claims description 8
- IKIIZLYTISPENI-ZFORQUDYSA-N baicalin Chemical compound O1[C@H](C(O)=O)[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1OC(C(=C1O)O)=CC2=C1C(=O)C=C(C=1C=CC=CC=1)O2 IKIIZLYTISPENI-ZFORQUDYSA-N 0.000 claims description 8
- 229960003321 baicalin Drugs 0.000 claims description 8
- AQHDANHUMGXSJZ-UHFFFAOYSA-N baicalin Natural products OC1C(O)C(C(O)CO)OC1OC(C(=C1O)O)=CC2=C1C(=O)C=C(C=1C=CC=CC=1)O2 AQHDANHUMGXSJZ-UHFFFAOYSA-N 0.000 claims description 8
- 239000000284 extract Substances 0.000 claims description 8
- 239000008188 pellet Substances 0.000 claims description 8
- 238000009826 distribution Methods 0.000 claims description 7
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- 238000012937 correction Methods 0.000 claims description 2
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- 239000000470 constituent Substances 0.000 claims 1
- 238000012546 transfer Methods 0.000 claims 1
- 239000003814 drug Substances 0.000 abstract description 25
- 238000002360 preparation method Methods 0.000 abstract description 17
- 239000008187 granular material Substances 0.000 abstract description 12
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- 241000207929 Scutellaria Species 0.000 description 4
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- 239000000463 material Substances 0.000 description 4
- 238000003908 quality control method Methods 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 230000002159 abnormal effect Effects 0.000 description 3
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- 235000014676 Phragmites communis Nutrition 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
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- 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
- 238000000643 oven drying Methods 0.000 description 2
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- 206010054949 Metaplasia Diseases 0.000 description 1
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- 206010044565 Tremor Diseases 0.000 description 1
- REDTZTIXXKUEIX-UHFFFAOYSA-N [P].O.CO Chemical compound [P].O.CO REDTZTIXXKUEIX-UHFFFAOYSA-N 0.000 description 1
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- 238000005469 granulation Methods 0.000 description 1
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- 230000023597 hemostasis Effects 0.000 description 1
- 238000004128 high performance liquid chromatography Methods 0.000 description 1
- 210000002429 large intestine Anatomy 0.000 description 1
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- 239000007791 liquid phase Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 210000004072 lung Anatomy 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
- 235000019813 microcrystalline cellulose Nutrition 0.000 description 1
- 239000008108 microcrystalline cellulose Substances 0.000 description 1
- 229940016286 microcrystalline cellulose Drugs 0.000 description 1
- 239000000203 mixture Substances 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
- 230000000144 pharmacologic effect Effects 0.000 description 1
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- -1 sets moisture≤8.0% Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
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- 239000000341 volatile oil Substances 0.000 description 1
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)
- A61K36/53—Lamiaceae or Labiatae (Mint family), e.g. thyme, rosemary or lavender
- A61K36/539—Scutellaria (skullcap)
-
- 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
- A61K9/1629—Organic macromolecular compounds
- A61K9/1652—Polysaccharides, e.g. alginate, cellulose derivatives; Cyclodextrin
-
- 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 radix scutellariae particle and its Chinese medicine preparation.The radix scutellariae particle is prepared by the method comprised the following steps：Baikal skullcap root decoction pieces are taken, are 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, radix scutellariae particle of the granularity in 16 40 mesh is obtained.The radix scutellariae 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 radix scutellariae particle and comprising in radix scutellariae particle
Medicine preparation.
Background technology
Radix scutellariae derives from labiate radix scutellariae Scutellaria baicalensis Georgi dry root, bitter, trembles with fear,
Return lung, courage, spleen, large intestine, small intestinl channel, with heat-clearing and damp-drying drug, purging intense heat and detonicating, hemostasis, antiabortive effect.
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 radix scutellariae particle needs several hours, operation with reference to the method for pharmacopeia
Also it is more complicated.The main chemical compositions of radix scutellariae particle are scutelloside, and as quality control index, conventional method uses efficient liquid phase
Chromatography etc., numerous and diverse pretreatment need to be often carried out to sample, substantial amounts of reagent is expended, environmental pollution is larger and to inspector's body
Body has been damaged, and feedback of the information is delayed, it is impossible to meet instant analysis multi items, many batch samples during particle enterprise large-scale production
The need for product.
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
A kind of reed mentioned in ancient books particle, its preparation technology is simple, steady quality.Meanwhile, in order to better control over the quality of radix scutellariae 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 radix scutellariae 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 radix scutellariae particle, prepared by the method comprised the following steps：Radix scutellariae 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 radix scutellariae particle of the granularity in 16-40 mesh.
Present inventor has found that radix scutellariae is added 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, radix scutellariae particle of the invention is prepared by the method comprised the following steps：Baikal skullcap root decoction pieces are taken, are 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 150-190 DEG C of EAT, 400-700 revs/min of revolution speed, leaving air temp 80-95 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 40-50HZ, feeding motor frequency 30-50HZ, oil cylinder working-pressure 16-24bar, obtains granularity in 16-40 mesh
Radix scutellariae particle.
Moisture≤8.0% in the process for producing optimized by the present invention, gained radix scutellariae particle, ethanol soluble extraction >=
20.0%, scutelloside >=133.5mg/g.
The radix scutellariae particle of the present invention can be further applied in various Chinese medicine preparations, to realize the pharmacological activity of radix scutellariae.Often
The Chinese medicine preparation comprising radix scutellariae 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 radix scutellariae particle of the present invention, and it is based on near-infrared spectrum technique quick detection, and wraps
Include following steps：
A. the collection of near infrared spectrum：Radix scutellariae particulate samples about 3g is taken, fine powder is ground into, near infrared spectrum scanning is carried out, adopts
Collect spectrum, obtain the original absorbance spectrogram of radix scutellariae particulate samples, and each component content is measured, measure radix scutellariae granular
The measured value of product each component 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 radix scutellariae particle quantitative model：The content of radix scutellariae pellet moisture is determined, using multiplicative scatter correction method pair
Original absorbance spectrum is pre-processed, and the spectral region of modeling chooses 7500.1-65447.6cm-1Characteristic wave bands, dimension elects 8 as；
Radix scutellariae particle ethanol soluble extraction content is determined, original absorbance spectrum is pre-processed using first derivative+MSC methods, modeling
Spectral region is chosen for 6100.5-5174.2cm-1Characteristic wave bands, dimension elects 5 as；Radix scutellariae particle content of baicalin is determined, is used
Vector normalization method is pre-processed to original absorbance spectrum, and the spectral region of modeling is chosen for 9401.7-4247.9cm-1Feature
Wave band, dimension elects 9 as；With PLS to the near infrared spectrum of calibration set and its correspondence radix scutellariae particulate samples each component
Quantitative model is set up between the measured value of 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 radix scutellariae particulate samples each component content, predicted value is compared with measured value, verifies
The accuracy of quantitative model；
D. the measure of radix scutellariae particle each component content：Radix scutellariae 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 radix scutellariae particle each component
Amount；The near-infrared quantitative determination model of the radix scutellariae pellet moisture, extract and the scutelloside that are built up is soft by near-infrared analysis
Part is integrated, and sets up the multi-method evaluation model of radix scutellariae particle, and radix scutellariae particulate samples to be detected are gathered according to step a method
Near infrared spectrum, is imported in radix scutellariae particle multi-method evaluation model, while determining radix scutellariae particle each component content.
Using the above-mentioned detection method of the present invention, the moisture, ethanol soluble extraction and scutelloside of radix scutellariae particle can be determined simultaneously
Content, it is only necessary to which a few minutes just can complete the detection of each group divided data, substantially reduces detection time, adapts to modern enterprise fast
Speed, the demand largely produced.And traditional detection method, determined using high effective liquid chromatography for measuring content of baicalin, oven drying method
Moisture, ethanol soluble extractives determination method determine ethanol soluble extraction content, cumbersome, not only need a variety of instrument and equipments,
Also needing each to examine post to cooperate can just smoothly complete, and data handling procedure is more complicated, time-consuming.In addition, the present invention
Method can be applicable each component assay of the material of 3 production links, including medicinal extract, spray dried powder, particle simultaneously.
In order to more accurately determine, in the assay method of the present invention, the sample preparation that radix scutellariae particle near-infrared is determined
Method is：Same batch radix scutellariae 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.See
Examine the sample bottle bottom after dress sample, it is ensured that the sample powder of test does not bond vial bottom, sample can just be carried out near red
External spectrum is scanned.
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 Radix Scutellariae extractum, 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 radix scutellariae 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 radix scutellariae particle each component near-infrared
On the basis of model, radix scutellariae 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 scutelloside, while can distinguish that kind is true again according to mahalanobis distance and density of fraction etc.
It is pseudo-.
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 radix scutellariae particle
Skill, and preparation technology is simple, technological parameter is stable and easy to control, is adapted to the preparation of scutellaria dispensing granule.(2) present invention is based near
Infrared spectrum technology combination chemometrics method, in certain spectral region, establishes radix scutellariae 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 radix scutellariae 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 radix scutellariae particulate samples；
Related figure between Fig. 2 radix scutellariaes pellet moisture near-infrared predicted value and measured value；
The comparison column diagram of Fig. 3 radix scutellariaes pellet moisture near-infrared predicted value and measured value；
Related figure between Fig. 4 radix scutellariae particle ethanol soluble extraction near-infrared predicted values and measured value；
The comparison column diagram of Fig. 5 radix scutellariae particle ethanol soluble extraction near-infrared predicted values and measured value；
Related figure between Fig. 6 radix scutellariae particle scutelloside near-infrared predicted values and measured value；
The comparison column diagram of Fig. 7 radix scutellariae particle scutelloside 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 radix scutellariae particle：Baikal skullcap root decoction pieces are taken, are 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
160 DEG C, expect 700 revs/min of revolution speed, 80 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 50HZ, oil cylinder working-pressure 20bar
Method is pelletized, and obtains radix scutellariae particle of the granularity in 40 mesh.
Embodiment 2：
The preparation of the Chinese medicine preparation of the particle containing radix scutellariae：Baikal skullcap root decoction pieces are taken, are 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 160 DEG C of EAT, 700 revs/min of revolution speed is expected, 80 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 50HZ, oil cylinder working-pressure
Dry granulation under the conditions of 20bar, obtains radix scutellariae particle of the granularity in 40 mesh；188g radix scutellariaes particle, 65g maltodextrins and 27g is micro-
Crystalline cellulose is mixed, and adds appropriate magnesium stearate, is mixed, is pressed into 1000.
Embodiment 3：
A kind of method based on near-infrared spectrum technique quick detection radix scutellariae granule moisture level, specifically includes following step
Suddenly：
A, radix scutellariae particulate samples are taken, totally 136 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 1 136 batches
The near-infrared original absorbance spectrogram of radix scutellariae 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 radix scutellariae 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, radix scutellariae 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 108 batches, chooses 28 batches of checkings
Collection.Analysis software, Automatic Optimal chooses preprocess method and spectral region, and optimum results are shown in Table 1.Using polynary scattering school
Execute and near-infrared original absorbance spectrum is pre-processed, choose 7500.1-5447.6cm-1Spectral information under characteristic wave bands,
The quantitative model set up with PLS (PLS) between near infrared spectrum and moisture measured value；Collection will be verified
Sample carries out near infrared spectrum scanning, using model, obtains the predicted value of radix scutellariae particulate samples content, by predicted value and actual measurement
Value is compared, and verifies the accuracy and predictive ability of quantitative model, and the model obtains cross validation coefficient correlation through cross validation
R2=0.904, RMSECV=0.123, RPD=3.22, dimension elect 8, checking collection coefficient R as2=0.871, RMSEP=
The determination of moisture of 0.148,28 batch of radix scutellariae particle the results are shown in Table 2, and the related figure between moisture predicted value and measured value is shown in figure
2, 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 28 batches of radix scutellariae particles of table
The deviation range of radix scutellariae granule moisture level is between 0.00-0.31% it can be seen from upper table 2, consensus forecast
The rate of recovery is 99.28%, illustrates that the model has preferable predictive ability and stability, available for the quick of radix scutellariae pellet moisture
Detection.
Embodiment 4：
A kind of method based on near-infrared spectrum technique quick detection radix scutellariae particle ethanol soluble extraction content, specifically include as
Lower step：
A, radix scutellariae particulate samples are taken, totally 136 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 1 136 batches
The near-infrared original absorbance spectrogram of radix scutellariae 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 radix scutellariae 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 radix scutellariae 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 108 batches, chooses 28 batches
For checking collection.Analysis software, Automatic Optimal chooses preprocess method and spectral region, and optimum results are shown in Table 3.Using single order
Derivative+MSC methods are pre-processed to near-infrared original absorbance spectrum, choose 6100.5-5174.2cm-1Spectrum under characteristic wave bands
Information, the quantitative model set up with PLS (PLS) between near infrared spectrum and ethanol soluble extraction content measured value；
The sample for verifying collection is subjected near infrared spectrum scanning, using model, the predicted value of radix scutellariae particulate samples content is obtained, will predict
Value is compared with measured value, verifies the accuracy and predictive ability of quantitative model, and the model obtains cross validation through cross validation
Coefficient R2=0.853, RMSECV=1.64, RPD=2.61, dimension elect 5, checking collection coefficient R as2=0.840,
RMSEP=1.35, the ethanol soluble extraction assay of 28 batches of radix scutellariae particles the results are shown in Table 4, and ethanol soluble extraction predicted value is with surveying
Related figure between value is shown in Fig. 4, and the comparison column diagram of ethanol soluble extraction predicted value and measured value is shown in Fig. 5.
Model parameter of the ethanol soluble extraction model of table 3 under different spectral regions and preprocess method
The ethanol soluble extraction assay result of 4 28 batches of radix scutellariae particles of table
The deviation range of radix scutellariae particle ethanol soluble extraction content is between 0.01-2.29% it can be seen from upper table 4, in advance
It is 99.57% to survey average recovery rate, illustrates that the model has preferable predictive ability and stability, available for radix scutellariae particle ethanol
The quick detection of extract.
Embodiment 5：
The method of content of baicalin, is specifically included as follows in a kind of quick detection radix scutellariae particle based on near-infrared spectrum technique
Step：
A, radix scutellariae particulate samples are taken, totally 136 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 1 136 batches
The near-infrared original absorbance spectrogram of radix scutellariae particle；
Meanwhile, the standard method according to specified in 2015 editions Chinese Pharmacopoeias, its content of baicalin shines high performance liquid chromatography
(《Chinese Pharmacopoeia》Four general rules 0512 of version in 2015) determine, comprise the following steps that：
Chromatographic condition and system suitability：Using octadecylsilane chemically bonded silica as filler；With methanol-water-phosphorus
Sour (47: 53: 0.2) are mobile phase；Detection wavelength is 280nm.Number of theoretical plate is calculated by scutelloside peak should be not less than 2500.
The preparation of reference substance solution：Take scutelloside reference substance appropriate, it is accurately weighed, plus every 1ml is made containing 15 μ g in methanol
Solution, is produced.
The preparation of need testing solution：This product under content uniformity is taken, it is finely ground, about 0.1g is taken, it is accurately weighed, put tool plug cone
In shape bottle, precision 70% ethanol 100ml of addition, weighed weight, ultrasonically treated (power 250W, frequency 33kHz) 30 minutes is put
It is cold, then weighed weight, the weight of less loss is supplied with 70% ethanol, is shaken up, is filtered, precision measures subsequent filtrate 2ml, puts 25ml measuring bottles
In, plus 70% ethanol shakes up to scale, 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,
Produce.
B, Distribution value surveyed according to sample number and sample content of baicalin, it is calibration set to choose 108 batches, chooses 28 batches to test
Card collection.Analysis software, Automatic Optimal chooses preprocess method and spectral region, and optimum results are shown in Table 5.Using vector normalizing
Change method is pre-processed to near-infrared original absorbance spectrum, chooses 9401.7-4247.9cm-1Spectral information under characteristic wave bands,
The quantitative model set up with PLS (PLS) between near infrared spectrum and scutelloside standard content；Collection will be verified
Sample carries out near infrared spectrum scanning, using model, the predicted value of radix scutellariae particulate samples content is obtained, by predicted value and measured value
It is compared, verifies the accuracy and predictive ability of quantitative model, the model obtains cross validation coefficient R through cross validation2
=0.847, RMSECV=8.3, RPD=2.56, dimension elect 9, checking collection coefficient R as2=0.902, RMSEP=6.85,
The content determination of Baicalin of 28 batches of radix scutellariae particles the results are shown in Table 6, and the related figure between scutelloside predicted value and measured value is shown in Fig. 6,
The comparison column diagram of scutelloside predicted value and measured value is shown in Fig. 7.
Model parameter of the scutelloside model of table 5 under different spectral regions and preprocess method
6 28 batches of radix scutellariae particle content determination of Baicalin results of table
The deviation range of radix scutellariae particle scutelloside is between 0.10-13.37mg/g it can be seen from upper table 6, and prediction is average
The rate of recovery is 100.09%.Illustrate that the model has preferable predictive ability and stability, available for radix scutellariae particle scutelloside
Quick detection.
Embodiment 6:
A kind of method based on near-infrared spectrum technique Fast Evaluation radix scutellariae granular mass, specifically includes following steps：
A. software is used, the radix scutellariae particle scutelloside built, moisture and extract quantitative model are imported, and set each group
The content limit divided, according to the quality standard of radix scutellariae particle, sets moisture≤8.0%, ethanol soluble extraction >=20.0%, scutelloside
>=133.5mg/g, sets up the multi-method evaluation model of radix scutellariae 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 radix scutellariae, red sage root 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
In a kind of reed mentioned in ancient books 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 radix scutellariae 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 radix scutellariae particle with principium identification institute test sample product, be identified as radix scutellariae 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 radix scutellariae particle.
Claims (6)
1. a kind of detection method of radix scutellariae particle, it is characterised in that based on near-infrared spectrum technique quick detection, and including as follows
Step：
A. the collection of near infrared spectrum：Radix scutellariae 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 radix scutellariae particulate samples, and each component content is measured, and measures radix scutellariae 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；It is described
NIR spectra collection the condition of scanning be：Scanning range is 4000cm-1-12000cm-1, scanning times are 32 times, and 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 radix scutellariae particle quantitative model：The content of radix scutellariae pellet moisture is determined, using multiplicative scatter correction method to original
Absorption spectrum is pre-processed, and the spectral region of modeling chooses 7500.1-65447.6cm-1Characteristic wave bands, dimension elects 8 as；Determine
Radix scutellariae particle ethanol soluble extraction content, is pre-processed, the spectrum of modeling using first derivative+MSC methods to original absorbance spectrum
Scope is chosen for 6100.5-5174.2cm-1Characteristic wave bands, dimension elects 5 as；Radix scutellariae particle content of baicalin is determined, using vector
Normalization method is pre-processed to original absorbance spectrum, and the spectral region of modeling is chosen for 9401.7-4247.9cm-1Characteristic wave
Section, dimension elects 9 as；The near infrared spectrum of calibration set and its correspondence radix scutellariae particulate samples each component are contained with PLS
Quantitative model is set up between the measured value of amount；
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 radix scutellariae particulate samples each component content, predicted value is compared with measured value, and checking is quantitative
The accuracy of model；
D. the measure of radix scutellariae particle each component content：Radix scutellariae 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 radix scutellariae particle each component is determined；
The near-infrared quantitative determination model of the radix scutellariae pellet moisture, extract and the scutelloside that are built up is passed through into near-infrared analysis software
Integrate, set up the multi-method evaluation model of radix scutellariae particle, radix scutellariae particulate samples to be detected are gathered near according to step a method
Infrared spectrum, is imported in radix scutellariae particle multi-method evaluation model, while determining radix scutellariae particle each component content；
Described radix scutellariae particle is prepared by the method comprised the following steps：Baikal skullcap root decoction pieces are taken, are 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 radix scutellariae particle of 40 mesh；Moisture≤8.0% in radix scutellariae particle, ethanol soluble extraction >=20.0%, scutelloside >=133.5mg/g.
2. the detection method of radix scutellariae particle as claimed in claim 1, it is characterised in that described radix scutellariae particle is by including as follows
The method of step is prepared：Baikal skullcap root decoction pieces are taken, are 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 150-190
DEG C, expect 400-700 revs/min of revolution speed, 80-95 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 40-50HZ, feeding motor frequency 30-50HZ, oil cylinder working-pressure
Dry granulation under the conditions of 16-24bar, obtains radix scutellariae particle of the granularity in 16-40 mesh.
3. the detection method of radix scutellariae particle as claimed in claim 1 or 2, it is characterised in that：Take same batch radix scutellariae particle about
3g, is ground into fine powder, crosses 80 mesh sieves, in the tool plug vial for being transferred to near-infrared measure.
4. the detection method of radix scutellariae particle as claimed in claim 1 or 2, it is characterised in that：Grinding fine powder is entered 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 radix scutellariae 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 radix scutellariae particle as claimed in claim 1 or 2, it is characterised in that：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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Denomination of invention: A detection method for Huangqin granules Effective date of registration: 20231225 Granted publication date: 20170822 Pledgee: Bank of China Limited by Share Ltd. Foshan branch Pledgor: GUANGDONG YIFANG PHARMACEUTICAL Co.,Ltd. Registration number: Y2023980073969 |