CN106109696B - A kind of detection method of radix scrophulariae particle - Google Patents
A kind of detection method of radix scrophulariae particle Download PDFInfo
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- CN106109696B CN106109696B CN201610459105.2A CN201610459105A CN106109696B CN 106109696 B CN106109696 B CN 106109696B CN 201610459105 A CN201610459105 A CN 201610459105A CN 106109696 B CN106109696 B CN 106109696B
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- KVRQGMOSZKPBNS-FMHLWDFHSA-N Harpagoside Chemical compound O([C@@H]1OC=C[C@@]2(O)[C@H](O)C[C@]([C@@H]12)(C)OC(=O)\C=C\C=1C=CC=CC=1)[C@@H]1O[C@H](CO)[C@@H](O)[C@H](O)[C@H]1O KVRQGMOSZKPBNS-FMHLWDFHSA-N 0.000 claims description 25
- KVRQGMOSZKPBNS-BYYMOQGZSA-N Harpagoside Natural products C[C@@]1(C[C@@H](O)[C@@]2(O)C=CO[C@@H](O[C@@H]3O[C@H](CO)[C@@H](O)[C@H](O)[C@H]3O)[C@H]12)OC(=O)C=Cc4ccccc4 KVRQGMOSZKPBNS-BYYMOQGZSA-N 0.000 claims description 25
- XUWSHXDEJOOIND-YYDKPPGPSA-N (1s,4as,5r,7s,7ar)-7-methyl-1-[(2s,3r,4s,5s,6r)-3,4,5-trihydroxy-6-(hydroxymethyl)oxan-2-yl]oxy-1,5,6,7a-tetrahydrocyclopenta[c]pyran-4a,5,7-triol Chemical compound O([C@@H]1OC=C[C@@]2(O)[C@H](O)C[C@@]([C@@H]12)(O)C)[C@@H]1O[C@H](CO)[C@@H](O)[C@H](O)[C@H]1O XUWSHXDEJOOIND-YYDKPPGPSA-N 0.000 claims description 24
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- HQKMJHAJHXVSDF-UHFFFAOYSA-L magnesium stearate Chemical compound [Mg+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O HQKMJHAJHXVSDF-UHFFFAOYSA-L 0.000 description 2
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- YTJSFYQNRXLOIC-UHFFFAOYSA-N octadecylsilane Chemical compound CCCCCCCCCCCCCCCCCC[SiH3] YTJSFYQNRXLOIC-UHFFFAOYSA-N 0.000 description 1
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Classifications
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- 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)
- A61K36/80—Scrophulariaceae (Figwort family)
- A61K36/808—Scrophularia (figwort)
-
- 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
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K9/00—Medicinal preparations characterised by special physical form
- A61K9/20—Pills, tablets, discs, rods
- A61K9/2004—Excipients; Inactive ingredients
- A61K9/2022—Organic macromolecular compounds
- A61K9/205—Polysaccharides, e.g. alginate, gums; Cyclodextrin
- A61K9/2059—Starch, including chemically or physically modified derivatives; Amylose; Amylopectin; Dextrin
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N21/3563—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing solids; Preparation of samples therefor
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- 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
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- 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
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- 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
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Abstract
The invention discloses a kind of radix scrophulariae particle and its Chinese medicine preparation.The radix scrophulariae particle is prepared by the method comprised the following steps：Radix scrophulariae 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, radix scrophulariae particle of the granularity in 16 40 mesh is obtained.The radix scrophulariae 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 scrophulariae particle and its Chinese medicine preparation.
Background technology
Radix scrophulariae is goatweed radix scrophulariae Scrophularia ningpoensis Hemsl. dry root, sweet, bitter, salty,
It is slightly cold, return lung, stomach, kidney channel, with clearing heat and cooling blood, nourishing Yin and falling fire, effect of detoxicating and resolving a mass.
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 scrophulariae particle needs several hours, operation with reference to the method for pharmacopeia
Also it is more complicated.The main chemical compositions of radix scrophulariae particle are harpagide+harpagoside, and as quality control index, conventional method makes
With high performance liquid chromatography etc., numerous and diverse pretreatment need to be often carried out to sample, substantial amounts of reagent is expended, environmental pollution it is larger and
Inspector's body is damaged, feedback of the information is delayed, it is impossible to meet many product of instant analysis during particle enterprise large-scale production
The need for kind, many batch samples.
With the development in epoch, near infrared spectrum (NIRS) analytical technology is further employed in Chemical Measurement polynary time
Return method and contemporary optics, microcomputer data processing so that near-infrared is developed rapidly, as in recent years point
Analyse the emerging analytical technology of one kind " green " of chemical field fast development, with applied widely, measurement it is convenient, pollution-free,
Without destruction, data it is accurate, it is reliable the advantages of, therefore be widely used in the quantitative analysis in the various fields of food, medicine and qualitative mirror
Not.
The content of the invention
In view of the above-mentioned problems of the prior art, it is an object of the invention to provide a kind of the profound of production technology standardization
Ginseng grains, its preparation technology is simple, steady quality.Meanwhile, in order to better control over the quality of radix scrophulariae 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 scrophulariae 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 scrophulariae particle, it is prepared by the method comprised the following steps：Take radix scrophulariae
Medicine materical crude slice, is added water to cook 2-3 times, and adding 5-10 times every time measures water, and heating every time is decocted 1-2 hours；Decoction merges, and filtrate is concentrated into phase
To the clear cream that density is 1.02-1.12, filtered while hot with 250-350 mesh sieves；Qinghuo reagent is spray-dried, and obtains spray powder；Will
Spray powder dry granulation, obtains radix scrophulariae particle of the granularity in 16-40 mesh.
Present inventor has found that radix scrophulariae is added water to cook 2-3 times by long term test, and adding 5-10 times every time measures water, often
Secondary heating is decocted and can more completely extracted active ingredient for 1-2 hours.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 because heated time is longer the loss of active ingredient
Preferably, radix scrophulariae particle of the invention is prepared by the method comprised the following steps：Radix scrophulariae medicine materical crude slice is taken, is added water pan-fried
Boil 3 times, 8 times of amount water are added every time, heating every time is decocted 1.5 hours；Decoction merge, filtrate be concentrated into relative density for 1.08 it is clear
Cream, is filtered with 350 mesh sieves while hot；In 170-185 DEG C of EAT, 400-700 revs/min of revolution speed, leaving air temp 85-95 are expected
DEG C, wind is spray-dried under conditions of sending 35-45 DEG C of temperature, obtains spray powder；In punching panel aperture 1.50mm, roller motor frequency
Dry granulation under the conditions of rate 40HZ, feeding motor frequency 45HZ, oil cylinder working-pressure 20bar, obtains radix scrophulariae of the granularity in 16-40 mesh
Grain.
Moisture≤8.0% in the process for producing optimized by the present invention, gained radix scrophulariae particle, ethanol soluble extraction >=
12.0%, harpagide+harpagoside >=2.0mg/g.
The radix scrophulariae particle of the present invention can be further applied in various Chinese medicine preparations, to realize the pharmacological activity of radix scrophulariae.Often
The Chinese medicine preparation comprising radix scrophulariae 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 scrophulariae 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 scrophulariae 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 scrophulariae particulate samples, and each component content is measured, measure radix scrophulariae 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 scrophulariae particle quantitative model：The content of radix scrophulariae pellet moisture is determined, using first derivative+MSC methods pair
Original absorbance spectrum is pre-processed, and the spectral region of modeling chooses 7500.1-4247.9cm-1Characteristic wave bands, dimension elects 8 as；
Radix scrophulariae particle ethanol soluble extraction content is determined, original absorbance spectrum is pre-processed using First derivative spectrograply, the spectrum of modeling
Scope is chosen for 7500.1-6096.4cm-1、5451.7-4247.9cm-1Characteristic wave bands, dimension elects 8 as；Radix scrophulariae particle is determined to breathe out
Bar glycosides+harpagoside content, is pre-processed using first derivative+MSC methods to original absorbance spectrum, the spectral region choosing of modeling
It is taken as 6100.5-4247.9cm-1Characteristic wave bands, dimension elects 9 as；With PLS to the near infrared spectrum of calibration set and
Quantitative model is set up between the measured value of its correspondence radix scrophulariae 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 radix scrophulariae particulate samples each component content, predicted value is compared with measured value, verifies
The accuracy of quantitative model；
D. the measure of radix scrophulariae particle each component content：Radix scrophulariae 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 scrophulariae particle each component
Amount；The near-infrared quantitative determination model of the radix scrophulariae pellet moisture built up, extract and harpagide+harpagoside is passed through near red
Outer analysis software is integrated, and the multi-method evaluation model of radix scrophulariae particle is set up, by radix scrophulariae particulate samples to be detected according to step a's
Method gathers near infrared spectrum, imports in radix scrophulariae particle multi-method evaluation model, while determining radix scrophulariae particle each component content.
Using above-mentioned detection method, cocoa determines moisture, ethanol soluble extraction and the harpagide+Ha Bae of radix scrophulariae particle simultaneously
Glycosides 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
Quickly, the demand largely produced.And traditional detection method, using high effective liquid chromatography for measuring harpagide+harpagoside content,
Moisture analysis content, ethanol soluble extractives determination method determine ethanol soluble extraction content, cumbersome, not only need a variety of
Instrument and equipment, 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 simultaneously 3 production links material each component assay, including medicinal extract, spray dried powder,
Particle.
In order to more accurately determine, in the assay method of the present invention, the sample preparation that radix scrophulariae particle near-infrared is determined
Method is：Same batch radix scrophulariae 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 scrophulariae medicinal extract, appropriate amount of auxiliary materials can be added by technological requirement, then with micro-
Ripple stove rapid draing, dry extract can complete detection by particl method is determined, for spray dried powder, then directly by measure particle
Method, greatly reduces the workload of model foundation, realizes the quality control to each key link material of radix scrophulariae particle.
Preferably, in step a, the condition of scanning of described near infrared spectra collection is：Scanning range is 4000 cm-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 scrophulariae particle each component near-infrared
On the basis of model, radix scrophulariae 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 harpagide+harpagoside, while can be distinguished according to mahalanobis distance and density of fraction etc. again
The other kind true and false.
The inventive method is particularly suitable for use in the products characteristics of Chinese medicinal granule, is processed and made through single medicine materical crude slice due to Chinese medicinal granule
Into, compared with Chinese native medicine compound prescription pellet or Chinese patent drug, component is relatively single, using this method interference less, accuracy it is high；In addition, in
Medicine particle series of products have kind more than 500, due to wide in variety, and conventional method is difficult to while realize qualitative, quantitative detection, the present invention
Under the premise of easy, free of contamination, while completing qualitative and quantitative analysis, product abnormal risk can be found in time, it is big to particle
The quality control of production intermediate link has great importance.
Therefore, the present invention compared with prior art, has the advantages that：(1) the specification preparation work of radix scrophulariae particle
Skill, and preparation technology is simple, technological parameter is stable and easy to control, is adapted to the preparation of radix scrophulariae granule.(2) present invention is based near
Infrared spectrum technology combination chemometrics method, in certain spectral region, establishes radix scrophulariae 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 scrophulariae 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 scrophulariae particulate samples；
Related figure between Fig. 2 radix scrophulariaes pellet moisture near-infrared predicted value and measured value；
The comparison column diagram of Fig. 3 radix scrophulariaes pellet moisture near-infrared predicted value and measured value；
Related figure between Fig. 4 radix scrophulariae particle ethanol soluble extraction near-infrared predicted values and measured value；
The comparison column diagram of Fig. 5 radix scrophulariae particle ethanol soluble extraction near-infrared predicted values and measured value；
The related figure of Fig. 6 radix scrophulariaes particle harpagide+between harpagoside near-infrared predicted value and measured value；
The comparison column diagram of Fig. 7 radix scrophulariaes particle harpagide+harpagoside near-infrared predicted value and measured value.
Embodiment
The present invention is further illustrated below by embodiment, following examples are the specific embodiment party of the present invention
Formula, but embodiments of the present invention are not limited by following embodiments.
Embodiment 1：
The preparation of radix scrophulariae particle：Radix scrophulariae medicine materical crude slice is taken, is added water to cook 3 times, 8 times of amount water are added every time, it is small that each heating decocts 1.5
When；Decoction merges, and filtrate is concentrated into the clear cream that relative density is 1.08 (80 DEG C), is filtered while hot with 350 mesh sieves；In EAT
175 DEG C, expect 500 revs/min of revolution speed, 90 DEG C of leaving air temp, wind is spray-dried under conditions of sending 40 DEG C of temperature, obtains spray drying
Powder；Done under the conditions of punching panel aperture 1.50mm, roller motor frequency 40HZ, feeding motor frequency 45HZ, oil cylinder working-pressure 20bar
Method is pelletized, and obtains radix scrophulariae particle of the granularity in 40 mesh.
Embodiment 2：
The preparation of the Chinese medicine preparation of the particle containing radix scrophulariae：Radix scrophulariae medicine materical crude slice is taken, is added water to cook 3 times, 8 times of amount water are added every time, every time
Heating is decocted 1.5 hours；Decoction merges, and filtrate is concentrated into the clear cream that relative density is 1.08 (80 DEG C), is filtered while hot with 350 mesh sieves
Cross；In 175 DEG C of EAT, 500 revs/min of revolution speed is expected, 90 DEG C of leaving air temp, wind is sprayed under conditions of sending 40 DEG C of temperature
Dry, obtain spray powder；In punching panel aperture 1.50mm, roller motor frequency 40HZ, feeding motor frequency 45HZ, oil cylinder working-pressure
Dry granulation under the conditions of 20bar, obtains radix scrophulariae particle of the granularity in 40 mesh；160g radix scrophulariaes particle and 80g maltodextrins are mixed, plus
Enter appropriate magnesium stearate, mix, be pressed into 1000.
Embodiment 3：
A kind of method based on near-infrared spectrum technique quick detection radix scrophulariae granule moisture level, specifically includes following step
Suddenly：
A, radix scrophulariae particulate samples are taken, totally 88 batches, respectively take about 3g, be ground into fine powder, be fitted into tool plug glass sample bottle, be placed near
It is scanned on infrared scanner, gathers spectrum, the condition of scanning：Scanning range 4000-12000cm-1, scanning times：32 times,
Resolution ratio 8cm-1, background correction in real time in scanning process, 3 spectrum of every part of sample collection obtain 88 batches of radix scrophulariaes as shown in Figure 1
The near-infrared original absorbance spectrogram of particle；
Meanwhile, the standard method according to specified in 2015 editions Chinese Pharmacopoeias, its moisture is determined using oven drying method, is taken and is ground
Finely disintegrated radix scrophulariae 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 scrophulariae 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 71 batches, and it is checking to choose 17 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 7500.1-4247.9cm-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, the predicted value of radix scrophulariae 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
=0.917, RMSECV=0.146, RPD=3.48, dimension elect 8, checking collection coefficient R as2=0.924, RMSEP=
The determination of moisture of 0.135,17 batch of radix scrophulariae 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 17 batches of radix scrophulariae particles of table
The deviation range of radix scrophulariae granule moisture level is between 0.01-0.21% it can be seen from upper table 2, consensus forecast
The rate of recovery is 100.64%, illustrates that the model has preferable predictive ability and stability, available for the fast of radix scrophulariae pellet moisture
Speed detection.
Embodiment 4：
A kind of method based on near-infrared spectrum technique quick detection radix scrophulariae particle ethanol soluble extraction content, specifically include as
Lower step：
A, radix scrophulariae particulate samples are taken, totally 88 batches, respectively take about 3g, be ground into fine powder, be fitted into tool plug glass sample bottle, be placed near
It is scanned on infrared scanner, gathers spectrum, the condition of scanning：Scanning range 4000-12000cm-1, scanning times：32 times,
Resolution ratio 8cm-1, background correction in real time in scanning process, 3 spectrum of every part of sample collection obtain 88 batches of radix scrophulariaes as shown in Figure 1
The near-infrared original absorbance spectrogram of particle；
Meanwhile, the standard method according to specified in 2015 editions Chinese Pharmacopoeias, its ethanol soluble extraction content is surveyed using hot dipping
It is fixed, the radix scrophulariae 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 scrophulariae 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 71 batches, chooses 17 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 method is pre-processed to near-infrared original absorbance spectrum, chooses 7500.1-6096.4cm-1、5451.7-4247.9cm-1It is special
The spectral information under wave band is levied, near infrared spectrum and ethanol soluble extraction content measured value are set up with PLS (PLS)
Between quantitative model；The sample for verifying collection is subjected near infrared spectrum scanning, using model, radix scrophulariae particulate samples content is obtained
Predicted value, predicted value is compared with measured value, verify quantitative model accuracy and predictive ability, the model through intersect
Verify to obtain cross validation coefficient R2=0.891, RMSECV=0.168, RPD=3.03, dimension elect 8 as, and checking collection is related
It is R2The ethanol soluble extraction assay of=0.950, RMSEP=0.988,17 batch radix scrophulariae particle the results are shown in Table 4, ethanol soluble extraction
Related figure between predicted value and measured value is shown in Fig. 4, and the comparison column diagram of ethanol soluble extraction predicted value and measured value is shown in Fig. 5
Model parameter of the ethanol soluble extraction model of table 3 under different spectral regions and preprocess method
The ethanol soluble extraction assay result of 4 17 batches of radix scrophulariae particles of table
The deviation range of radix scrophulariae particle ethanol soluble extraction content is between 0.03-2.43% it can be seen from upper table 4, in advance
It is 99.13% to survey average recovery rate, illustrates that the model has preferable predictive ability and stability, available for radix scrophulariae particle ethanol
The quick detection of extract.
Embodiment 5：
A kind of method of harpagide+harpagoside content in quick detection radix scrophulariae particle based on near-infrared spectrum technique, tool
Body comprises the following steps：
A, radix scrophulariae particulate samples are taken, totally 88 batches, respectively take about 3g, be ground into fine powder, be fitted into tool plug glass sample bottle, be placed near
It is scanned on infrared scanner, gathers spectrum, the condition of scanning：Scanning range 4000-12000cm-1, scanning times：32 times,
Resolution ratio 8cm-1, background correction in real time in scanning process, 3 spectrum of every part of sample collection obtain 88 batches of radix scrophulariaes as shown in Figure 1
The near-infrared original absorbance spectrogram of particle；
Meanwhile, the standard method according to specified in 2015 editions Chinese Pharmacopoeias, its harpagide+harpagoside content shines efficient liquid
Phase 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；Using acetonitrile as flowing
Phase A, using 0.03% phosphoric acid solution as Mobile phase B, the regulation according to the form below is eluted；Detection wavelength 210nm.Number of theoretical plate is pressed
Harpagide is calculated with harpagoside peak all should be not less than 5000.
The preparation of reference substance solution：Take harpagide reference substance, harpagoside reference substance appropriate, it is accurately weighed, plus 30% first
Mixed solutions of every 1ml containing the μ g of harpagide 60, the μ g of harpagoside 20 is made in alcohol, produces.
The preparation of need testing solution：This product under content uniformity is taken, it is finely ground, about 1g is taken, it is accurately weighed, put tool plug taper
In bottle, precision 50% methanol 50ml of addition, close plug, weighed weight, ultrasonically treated (power 250W, frequency 40kHz) 30 minutes is put
It is cold, then weighed weight, the weight of less loss is supplied with 50% methanol, is shaken up, filters, 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 harpagide+harpagoside content, it is calibration set to choose 71 batches, is chosen
17 batches are checking collection.Analysis software, Automatic Optimal chooses preprocess method and spectral region, and optimum results are shown in Table 5.Using
First derivative+MSC methods are pre-processed to near-infrared original absorbance spectrum, choose 6100.5-4247.9cm-1Under characteristic wave bands
Spectral information, determining between near infrared spectrum and harpagide+harpagoside standard content is set up with PLS (PLS)
Measure model；The sample for verifying collection is subjected near infrared spectrum scanning, using model, the prediction of radix scrophulariae particulate samples content is obtained
Value, predicted value is compared with measured value, verifies the accuracy and predictive ability of quantitative model, and the model is obtained through cross validation
Cross validation coefficient R2=0.947, RMSECV=0.366, RPD=4.33, dimension elect 9, checking collection coefficient R as2=
The harpagide of 0.950, RMSEP=0.435,17 batches of radix scrophulariae particles+harpagoside assay the results are shown in Table 6, harpagide+Ha Ba
Related figure between Russia's glycosides predicted value and measured value is shown in Fig. 6, harpagide+harpagoside predicted value and measured value comparison column diagram
See Fig. 7.
Model parameter of 5 harpagides of the table+harpagoside model under different spectral regions and preprocess method
6 17 batches of radix scrophulariae particle harpagides of table are right+harpagoside assay result
The deviation range of radix scrophulariae particle harpagide+harpagoside is between 0-0.78mg/g it can be seen from upper table 6, in advance
It is 100.32% to survey average recovery rate.Illustrate that the model has preferable predictive ability and stability, breathed out available for radix scrophulariae particle
The quick detection of bar glycosides+harpagoside.
Embodiment 6:
A kind of method based on near-infrared spectrum technique Fast Evaluation radix scrophulariae granular mass, specifically includes following steps：
A. software is used, the radix scrophulariae particle harpagide+harpagoside built, moisture and extract quantitative model are imported,
And set the content limit of each component, according to the quality standard of radix scrophulariae particle, set moisture≤8.0%, ethanol soluble extraction >=
12.0%, harpagide+harpagoside >=2.0mg/g sets up the multi-method evaluation model of radix scrophulariae 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 scrophulariae, red sage root etc. 10 batches
Particulate samples are evaluated, and sample message table is shown in Table 7.The spectrogram of numbering 1-10 samples is gathered respectively, spectrogram is imported profound
In ginseng grains 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 scrophulariae 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 scrophulariae particle with principium identification institute test sample product, be identified as radix scrophulariae particle
Sample can draw the accurate predictor of each component simultaneously.Illustrate that the model has preferable predictive ability and accuracy, can be fast
Speed evaluates the quality of radix scrophulariae particle.
Claims (6)
1. a kind of detection method of radix scrophulariae 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 scrophulariae 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 scrophulariae particulate samples, and each component content is measured, and measures radix scrophulariae 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, described
The condition of scanning of near infrared spectra collection be：Scanning range is 4000cm-1-12000cm-1, scanning times are 32 times, are differentiated
Rate is 8cm-1, background correction, 3 spectrum of every part of sample collection in real time in scanning process；
B. the foundation of radix scrophulariae particle quantitative model：The content of radix scrophulariae pellet moisture is determined, using first derivative+MSC methods to original
Absorption spectrum is pre-processed, and the spectral region of modeling chooses 7500.1-4247.9cm-1Characteristic wave bands, dimension elects 8 as；Determine
Radix scrophulariae particle ethanol soluble extraction content, is pre-processed, the spectral region of modeling using First derivative spectrograply to original absorbance spectrum
It is chosen for 7500.1-6096.4cm-1、5451.7-4247.9cm-1Characteristic wave bands, dimension elects 8 as；Determine radix scrophulariae particle harpagide
+ harpagoside content, is pre-processed using first derivative+MSC methods to original absorbance spectrum, and the spectral region of modeling is chosen for
6100.5-4247.9cm-1Characteristic wave bands, dimension elects 9 as；With PLS is to the near infrared spectrum of calibration set and its is right
Quantitative model is set up between the measured value for answering radix scrophulariae particulate samples 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 radix scrophulariae 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 scrophulariae particle each component content：Radix scrophulariae 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 scrophulariae particle each component is determined；
The near-infrared quantitative determination model of the radix scrophulariae pellet moisture built up, extract and harpagide+harpagoside is passed through into near-infrared
Analysis software is integrated, and the multi-method evaluation model of radix scrophulariae particle is set up, by the side of radix scrophulariae particulate samples to be detected according to step a
Method gathers near infrared spectrum, imports in radix scrophulariae particle multi-method evaluation model, while determining radix scrophulariae particle each component content；
Described radix scrophulariae particle is prepared by the method comprised the following steps：Radix scrophulariae medicine materical crude slice is taken, is added water to cook 2-3 times, every time
Plus 5-10 times measured water, heating every time is decocted 1-2 hours；Decoction merges, and it is the clear of 1.02-1.12 that filtrate, which is concentrated into relative density,
Cream, is filtered with 250-350 mesh sieves while hot；Qinghuo reagent is spray-dried, and obtains spray powder；By spray powder dry granulation, granularity is obtained
In the radix scrophulariae particle of 16-40 mesh；Moisture≤8.0% in radix scrophulariae particle, ethanol soluble extraction >=12.0%, harpagide+Ha Bae
Glycosides >=2.0mg/g.
2. the detection method of radix scrophulariae particle as claimed in claim 1, it is characterised in that described radix scrophulariae particle is by including as follows
The method of step is prepared：Radix scrophulariae medicine materical crude slice is taken, is added water to cook 3 times, 8 times of amount water are added every time, heating every time is decocted 1.5 hours；
Decoction merges, and filtrate is concentrated into the clear cream that relative density is 1.08, is filtered while hot with 350 mesh sieves；In EAT 170-185
DEG C, expect 400-700 revs/min of revolution speed, 85-95 DEG C of leaving air temp, wind is spray-dried under conditions of sending 35-45 DEG C of temperature,
Obtain spray powder；In punching panel aperture 1.50mm, roller motor frequency 40HZ, feeding motor frequency 45HZ, oil cylinder working-pressure 20bar bars
Dry granulation under part, obtains radix scrophulariae particle of the granularity in 16-40 mesh.
3. the detection method of radix scrophulariae particle as claimed in claim 1 or 2, it is characterised in that：Take same batch radix scrophulariae 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 scrophulariae 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 scrophulariae 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 scrophulariae 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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