CN106074722B - A kind of detection method of capsule of weeping forsythia particle - Google Patents
A kind of detection method of capsule of weeping forsythia particle Download PDFInfo
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- 241000576429 Forsythia suspensa Species 0.000 title claims abstract description 120
- 239000002775 capsule Substances 0.000 title claims abstract description 119
- 239000002245 particle Substances 0.000 title claims abstract description 91
- 238000001514 detection method Methods 0.000 title claims abstract description 27
- 238000000034 method Methods 0.000 claims abstract description 65
- 239000003814 drug Substances 0.000 claims abstract description 31
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- 238000002360 preparation method Methods 0.000 claims abstract description 18
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- 238000010438 heat treatment Methods 0.000 claims abstract description 12
- WHGYBXFWUBPSRW-FOUAGVGXSA-N beta-cyclodextrin Chemical compound OC[C@H]([C@H]([C@@H]([C@H]1O)O)O[C@H]2O[C@@H]([C@@H](O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O3)[C@H](O)[C@H]2O)CO)O[C@@H]1O[C@H]1[C@H](O)[C@@H](O)[C@@H]3O[C@@H]1CO WHGYBXFWUBPSRW-FOUAGVGXSA-N 0.000 claims abstract description 11
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- 239000000706 filtrate Substances 0.000 claims abstract description 8
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- 238000001914 filtration Methods 0.000 claims abstract description 7
- 239000000341 volatile oil Substances 0.000 claims abstract description 7
- 238000004821 distillation Methods 0.000 claims abstract description 6
- 239000003153 chemical reaction reagent Substances 0.000 claims abstract description 5
- KFFCKOBAHMGTMW-LGQRSHAYSA-N Forsythin Chemical compound C1=C(OC)C(OC)=CC=C1[C@H]1[C@@H](CO[C@@H]2C=3C=C(OC)C(O[C@H]4[C@@H]([C@@H](O)[C@H](O)[C@@H](CO)O4)O)=CC=3)[C@@H]2CO1 KFFCKOBAHMGTMW-LGQRSHAYSA-N 0.000 claims description 27
- 238000002329 infrared spectrum Methods 0.000 claims description 23
- 238000001228 spectrum Methods 0.000 claims description 15
- 239000000047 product Substances 0.000 claims description 13
- 230000003595 spectral effect Effects 0.000 claims description 12
- 238000013210 evaluation model Methods 0.000 claims description 10
- 229950005162 benexate Drugs 0.000 claims description 9
- IAXUQWSLRKIRFR-SAABIXHNSA-N chembl2104696 Chemical compound C1C[C@@H](CNC(=N)N)CC[C@@H]1C(=O)OC1=CC=CC=C1C(=O)OCC1=CC=CC=C1 IAXUQWSLRKIRFR-SAABIXHNSA-N 0.000 claims description 9
- 150000001875 compounds Chemical class 0.000 claims description 9
- 238000012360 testing method Methods 0.000 claims description 9
- 239000008188 pellet Substances 0.000 claims description 8
- 238000000862 absorption spectrum Methods 0.000 claims description 7
- 229940079593 drug Drugs 0.000 claims description 7
- 238000002835 absorbance Methods 0.000 claims description 5
- 238000009826 distribution Methods 0.000 claims description 5
- 239000003921 oil Substances 0.000 claims description 5
- 238000003705 background correction Methods 0.000 claims description 4
- 238000005259 measurement Methods 0.000 claims description 4
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- 230000008676 import Effects 0.000 claims 1
- HFHDHCJBZVLPGP-UHFFFAOYSA-N schardinger α-dextrin Chemical group O1C(C(C2O)O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC(C(O)C2O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC2C(O)C(O)C1OC2CO HFHDHCJBZVLPGP-UHFFFAOYSA-N 0.000 claims 1
- 239000002893 slag Substances 0.000 claims 1
- 208000011580 syndromic disease Diseases 0.000 claims 1
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- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 12
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 229920002774 Maltodextrin Polymers 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
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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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- 241000207834 Oleaceae Species 0.000 description 1
- 240000007164 Salvia officinalis Species 0.000 description 1
- 229920002472 Starch Polymers 0.000 description 1
- PBCJIPOGFJYBJE-UHFFFAOYSA-N acetonitrile;hydrate Chemical compound O.CC#N PBCJIPOGFJYBJE-UHFFFAOYSA-N 0.000 description 1
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- 230000003760 hair shine Effects 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 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
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- 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
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Classifications
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- 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)
- A61K36/63—Oleaceae (Olive family), e.g. jasmine, lilac or ash tree
- A61K36/634—Forsythia
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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
- A61K9/14—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
- A61K9/1682—Processes
-
- 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
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- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
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- 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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- 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
- G01N2021/3572—Preparation of samples, e.g. salt matrices
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Abstract
The invention discloses a kind of capsule of weeping forsythia particle and its Chinese medicine preparation.The capsule of weeping forsythia particle is prepared by the method comprised the following steps：Capsule of weeping forsythia medicine materical crude slice, plus 25 times of amount water, heating distillation 13 hours are taken, volatile oil and aqua aromatica is collected, is included with beta cyclodextrin, beta cyclodextrin clathrate is obtained, decoction filtration is standby；The dregs of a decoction are added water to cook 23 times, 5 10 times of amount water, heating decoction 12 hours every time, and decoction merges；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；Beta cyclodextrin clathrate is well mixed with spray powder, dry granulation, obtains capsule of weeping forsythia particle of the granularity in 16 40 mesh.The capsule of weeping forsythia 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 capsule of weeping forsythia particle and containing in capsule of weeping forsythia particle
Medicine preparation.
Background technology
The capsule of weeping forsythia is Oleaceae plants the capsule of weeping forsythia Forsythia suspensa (Thunb.) Vahl dry fruit.Hardship, is slightly cold,
Return lung, the heart, small intestinl channel, clearing heat and detoxicating, dispersing swelling and dissipating binds, effect of dispelling wind and heat from the body.
Chinese medicinal granule is, to meet the traditional Chinese medicine medicine materical crude slice of concocted specification as raw material, to extract, concentrate, do through modern industry
Dry, granulation and the Chinese medicine series of products that are made, its function, cure mainly, nature and flavor, channel tropism it is consistent with traditional Chinese medicine medicine materical crude slice, as new
Medicine materical crude slice form is controlled for clinical syndrome differentiation opinion instead of the prepared slices of Chinese crude drugs, adds and subtracts, uses with card." medicine materical crude slice is used as medicine, and faces use with traditional Chinese medicine decoction
Now decoct " application method compare, Chinese medicinal granule had both maintained the property of medicine drug effect of the former prepared slices of Chinese crude drugs, and when using without decocting,
It is easy to carry, safe and healthy, quality controllable, and can be added and subtracted with disease, meet the allegro life style of modern.
At present, Chinese medicinal granule is generally that traditional water is extracted, or extracts extraction after volatile oil, and different preparation technologies are led
The product quality that cause is produced by different manufacturers is inconsistent, and drug effect has difference.Accordingly, it would be desirable to the extraction process of research standard,
With the production process of specification Chinese medicinal granule, it is ensured that drug effect.In addition, the quality of Chinese medicinal granule also can be by detection means
Restriction, the measure of moisture in traditional capsule of weeping forsythia particle needs several hours with reference to the method for pharmacopeia, operates also more complicated.Even
The main chemical compositions for sticking up particle are forsythin, as quality control index, and conventional method uses high performance liquid chromatography etc., often
Numerous and diverse pretreatment need to be carried out to sample, substantial amounts of reagent is expended, environmental pollution is larger and inspector's body has been damaged,
Feedback of the information is delayed, it is impossible to meet during particle enterprise large-scale production the need for instant analysis multi items, many batch samples.
With the development in epoch, near infrared spectrum (NIRS) analytical technology is further employed in Chemical Measurement polynary time
Return method and contemporary optics, microcomputer data processing so that near-infrared is developed rapidly, as in recent years point
Analyse the emerging analytical technology of one kind " green " of chemical field fast development, with applied widely, measurement it is convenient, pollution-free,
Without destruction, data it is accurate, it is reliable the advantages of, therefore be widely used in the quantitative analysis in the various fields of food, medicine and qualitative mirror
Not.
The content of the invention
In view of the above-mentioned problems of the prior art, it is an object of the invention to provide a kind of company of production technology standardization
Particle is stuck up, its preparation technology is simple, steady quality.Meanwhile, in order to better control over the quality of capsule of weeping forsythia 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 capsule of weeping forsythia 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 capsule of weeping forsythia particle, prepared by the method comprised the following steps：Take weeping forsythia drink
Piece, plus 2-5 times measured water, heating distillation 1-3 hour, collection volatile oil and aqua aromatica, with beta-cyclodextrin inclusion compound, obtains beta-schardinger dextrin bag
Compound, decoction filtration is standby；The dregs of a decoction are added water to cook 2-3 times, and each 5-10 times is measured water, and heating is decocted 1-2 hours, and decoction merges；
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,
Obtain spray powder；Benexate Hydrochloride is well mixed with spray powder, dry granulation, obtains capsule of weeping forsythia particle of the granularity in 16-40 mesh.
Preferably, capsule of weeping forsythia particle of the invention is prepared by the method comprised the following steps：Take capsule of weeping forsythia medicine materical crude slice, plus 3 times
Water is measured, volatile oil and aqua aromatica are collected in heating distillation 2 hours, with beta-cyclodextrin inclusion compound, obtain Benexate Hydrochloride, decoction filter
Cross, it is standby；The dregs of a decoction are added water to cook 3 times, 8 times of amount water, heating decoction 1.5 hours every time, and decoction merges；Filtrate is concentrated into relatively close
The clear cream for 1.09 is spent, is filtered while hot with 350 mesh sieves；In 170-185 DEG C of EAT, expect 400-700 revs/min of revolution speed, go out
85-95 DEG C of air temperature, wind is spray-dried under conditions of sending 35-45 DEG C of temperature, obtains spray powder；By spray powder and beta-schardinger dextrin
Inclusion compound is well mixed, 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 capsule of weeping forsythia particle of the granularity in 16-40 mesh.
Moisture≤8.0% in the process for producing optimized by the present invention, gained capsule of weeping forsythia particle, forsythin >=
8.6mg/g。
The capsule of weeping forsythia particle of the present invention can be further applied in various Chinese medicine preparations, to realize the pharmacological activity of the capsule of weeping forsythia.Often
The Chinese medicine preparation comprising capsule of weeping forsythia 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 capsule of weeping forsythia 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：Capsule of weeping forsythia 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 capsule of weeping forsythia particulate samples, and each component content is measured, measure capsule of weeping forsythia 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 capsule of weeping forsythia particle quantitative model：The content of capsule of weeping forsythia pellet moisture is determined, using subtracting straight line method pair
Original absorbance spectrum is pre-processed, and the spectral region of modeling chooses 9401.7-4247.9cm-1Characteristic wave bands, dimension elects 10 as；
Capsule of weeping forsythia particle Determination of forsythin is determined, original absorbance spectrum is pre-processed using first derivative+subtract straight line method, built
The spectral region of mould chooses 9401.7-4598.8cm-1Wave band is characterized, dimension elects 6 as；With PLS to calibration set
Near infrared spectrum and its correspondence capsule of weeping forsythia particulate samples each component content measured value between set up quantitative model；
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 capsule of weeping forsythia particulate samples each component content, predicted value is compared with measured value, verifies
The accuracy of quantitative model；
D. the measure of capsule of weeping forsythia particle each component content：Capsule of weeping forsythia 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 capsule of weeping forsythia particle each component
Amount；The near-infrared quantitative determination model of the capsule of weeping forsythia pellet moisture built up and forsythin is integrated by near-infrared analysis software,
The multi-method evaluation model of capsule of weeping forsythia particle is set up, capsule of weeping forsythia particulate samples to be detected are gathered into near-infrared according to step a method
Spectrum, is imported in capsule of weeping forsythia particle multi-method evaluation model, while determining capsule of weeping forsythia particle each component content.
Using above-mentioned detection method, the moisture and Determination of forsythin of capsule of weeping forsythia particle can be determined simultaneously, it is only necessary to which a few minutes just may be used
To complete the detection of each group divided data, detection time is substantially reduced, the demand that modern enterprise is quick, largely produce is adapted to.
And traditional detection method, it is cumbersome using high effective liquid chromatography for measuring Determination of forsythin, moisture analysis content,
A variety of instrument and equipments are not only needed, also needing each to examine post to cooperate can just smoothly complete, and data handling procedure is more multiple
It is miscellaneous, time-consuming.In addition, the method for the present invention can be applicable each component assay of the material of 3 production links, including leaching simultaneously
Cream, spray dried powder, particle.
In order to more accurately determine, in the assay method of the present invention, the sample preparation that capsule of weeping forsythia particle near-infrared is determined
Method is：Same batch capsule of weeping forsythia 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 Fructus Forsythiae 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 capsule of weeping forsythia 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 capsule of weeping forsythia particle each component near-infrared
On the basis of model, establish capsule of weeping forsythia particle multi-method evaluation model, can be drawn by the collection of a spectrum in sample moisture and
The multicomponent content results such as forsythin, while the kind true and false can be distinguished again according to mahalanobis distance and density of fraction etc..
The inventive method is particularly suitable for use in the products characteristics of Chinese medicinal granule, is processed and made through single medicine materical crude slice due to Chinese medicinal granule
Into, compared with Chinese native medicine compound prescription pellet or Chinese patent drug, component is relatively single, using this method interference less, accuracy it is high；In addition, in
Medicine particle series of products have kind more than 500, due to wide in variety, and conventional method is difficult to while realize qualitative, quantitative detection, the present invention
Under the premise of easy, free of contamination, while completing qualitative and quantitative analysis, product abnormal risk can be found in time, it is big to particle
The quality control of production intermediate link has great importance.
Therefore, the present invention compared with prior art, has the advantages that：(1) the specification preparation work of capsule of weeping forsythia particle
Skill, and preparation technology is simple, technological parameter is stable and easy to control, is adapted to the preparation of Lianqiao Extracts.(2) present invention is based near
Infrared spectrum technology combination chemometrics method, in certain spectral region, establishes capsule of weeping forsythia 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 capsule of weeping forsythia 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 capsule of weeping forsythia particulate samples；
Related figure between Fig. 2 capsules of weeping forsythia pellet moisture near-infrared predicted value and measured value；
The comparison column diagram of Fig. 3 capsules of weeping forsythia pellet moisture near-infrared predicted value and measured value；
Related figure between Fig. 4 capsule of weeping forsythia particle forsythin near-infrared predicted values and measured value；
The comparison column diagram of Fig. 5 capsule of weeping forsythia particle forsythin 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 capsule of weeping forsythia particle：Capsule of weeping forsythia medicine materical crude slice, plus 3 times of amount water, heating distillation 2 hours are taken, volatile oil and aqua aromatica is collected,
With beta-cyclodextrin inclusion compound, Benexate Hydrochloride is obtained, decoction filtration is standby；The dregs of a decoction are added water to cook 3 times, measure water for 8 times every time, plus
Heat is decocted 1.5 hours, and decoction merges；Filtrate is concentrated into the clear cream that relative density is 1.09, is filtered while hot with 350 mesh sieves；Entering
175 DEG C of air temperature, 600 revs/min of revolution speed of material, 85 DEG C of leaving air temp, wind is spray-dried under conditions of sending temperature 45 C, is obtained
Spray powder；Spray powder is well mixed with Benexate Hydrochloride, in punching panel aperture 1.50mm, roller motor frequency 40HZ,
Dry granulation under the conditions of feeding motor frequency 45HZ, oil cylinder working-pressure 20bar, obtains capsule of weeping forsythia particle of the granularity in 40 mesh.
Embodiment 2：
The preparation of the Chinese medicine preparation of the particle containing the capsule of weeping forsythia：Capsule of weeping forsythia medicine materical crude slice, plus 3 times of amount water, heating distillation 2 hours are taken, collection is waved
Hair oil and aqua aromatica, with beta-cyclodextrin inclusion compound, obtain Benexate Hydrochloride, decoction filtration is standby；The dregs of a decoction add water to cook 3 times, often
Secondary 8 times of amounts water, heating is decocted 1.5 hours, and decoction merges；Filtrate is concentrated into the clear cream that relative density is 1.09, and 350 mesh are used while hot
Sieving；In 175 DEG C of EAT, 600 revs/min of revolution speed, 85 DEG C of leaving air temp are expected, wind send progress under conditions of temperature 45 C
Spray drying, obtains spray powder；Spray powder is well mixed with Benexate Hydrochloride, in punching panel aperture 1.50mm, roll electricity
Dry granulation under the conditions of unit frequency 40HZ, feeding motor frequency 45HZ, oil cylinder working-pressure 20bar, obtains the capsule of weeping forsythia of the granularity in 40 mesh
Grain；155g capsules of weeping forsythia particle, 58g starch, 22g maltodextrins, 6g essence are mixed, appropriate magnesium stearate is added, mixes, is pressed into
1000.
Embodiment 3：
A kind of method based on near-infrared spectrum technique quick detection capsule of weeping forsythia granule moisture level, specifically includes following step
Suddenly：
A, capsule of weeping forsythia particulate samples are taken, totally 75 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 75 batches of capsules of weeping forsythia 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 capsule of weeping forsythia 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, capsule of weeping forsythia 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 60 batches, and it is checking to choose 15 batches
Collection.Analysis software, Automatic Optimal chooses preprocess method and spectral region, and optimum results are shown in Table 1.Subtract straight line method
Near-infrared original absorbance spectrum is pre-processed, 9401.7-4247.9cm is chosen-1Spectral information under characteristic wave bands, is used
The quantitative model that PLS (PLS) is set up between near infrared spectrum and moisture measured value；The sample of collection will be verified
Near infrared spectrum scanning is carried out, using model, the predicted value of capsule of weeping forsythia particulate samples content is obtained, predicted value and measured value are carried out
Compare, verify the accuracy and predictive ability of quantitative model, the model obtains cross validation coefficient R through cross validation2=
0.907, RMSECV=0.129, RPD=3.28, dimension elect 10, checking collection coefficient R as2=0.926, RMSEP=0.13,
The determination of moisture of 15 batches of capsule of weeping forsythia particles the results are shown in Table 2, and the related figure between moisture predicted value and measured value is shown in Fig. 2, moisture
The comparison column diagram of 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 15 batches of capsule of weeping forsythia particles of table
The deviation range of capsule of weeping forsythia granule moisture level is between 0.-0.22% it can be seen from upper table 2, and consensus forecast is returned
Yield is 102.80%, illustrates that the model has preferable predictive ability and stability, available for the quick of capsule of weeping forsythia pellet moisture
Detection.
Embodiment 4：
The method of Determination of forsythin, is specifically included as follows in a kind of quick detection capsule of weeping forsythia particle based on near-infrared spectrum technique
Step：
A, capsule of weeping forsythia particulate samples are taken, totally 75 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 75 batches of capsules of weeping forsythia 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 Determination of forsythin shines high performance liquid chromatography
(《Chinese Pharmacopoeia》Four general rules 0512 of version in 2015) determine, comprise the following steps that：
Chromatographic condition and system suitability：Using octadecylsilane chemically bonded silica as filler；With acetonitrile-water (25:
75) it is mobile phase；Detection wavelength is 277nm.Number of theoretical plate is calculated by forsythin peak should be not less than 3000.
The preparation of reference substance solution：Take forsythin reference substance appropriate, it is accurately weighed, plus every 1ml is made containing 0.2mg's in methanol
Solution, is produced.
The preparation of need testing solution：Take this product appropriate, it is finely ground, about 0.5g is taken, it is accurately weighed, put in conical flask with cover, essence
Close addition methanol 15ml, close plug, weighed weight, ultrasonically treated (power 250W, frequency 40kHz) 25 minutes is let cool, then weighed heavy
Amount, the weight of less loss is supplied with methanol, is shaken up, and is filtered, and precision measures subsequent filtrate 5ml, is steamed near dry, is used neutral alumina 0.5g
Mix thoroughly, be added on neutral alumina column (100-200 mesh, 1g, internal diameter 1-1.5cm), eluted with 70% ethanol 80ml, collect elution
Liquid, is concentrated to dryness, and residue is dissolved with 50% methanol, is transferred in 5ml measuring bottles, and is diluted to scale, is shaken up, filtration, takes continuous filter
Liquid, is produced.
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 Determination of forsythin, it is calibration set to choose 61 batches, chooses 14 batches to test
Card collection.Analysis software, Automatic Optimal chooses preprocess method and spectral region, and optimum results are shown in Table 3.Using first derivative
+ subtract straight line method near-infrared original absorbance spectrum is pre-processed, choose 9401.7-4598.8cm-1Under characteristic wave bands
Spectral information, the quantitative model set up with PLS (PLS) between near infrared spectrum and forsythin standard content；
The sample for verifying collection is subjected near infrared spectrum scanning, using model, the predicted value of capsule of weeping forsythia 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=0.892, RMSECV=0.99, RPD=3.04, dimension elect 6, checking collection coefficient R as2=0.981,
RMSEP=0.485, the forsythin of 14 batches of capsule of weeping forsythia particles the results are shown in Table 4, between forsythin predicted value and measured value
Related figure is shown in Fig. 4, and the comparison column diagram of forsythin predicted value and measured value is shown in Fig. 5.
Model parameter of the forsythin model of table 3 under different spectral regions and preprocess method
4 14 batches of capsule of weeping forsythia particle forsythin results of table
The deviation range of capsule of weeping forsythia particle forsythin is between 0.02-1.04mg/g it can be seen from upper table 4, and prediction is average
The rate of recovery is 97.89%.Illustrate that the model has preferable predictive ability and stability, available for the fast of capsule of weeping forsythia particle forsythin
Speed detection.
Embodiment 5：
A kind of method based on near-infrared spectrum technique Fast Evaluation capsule of weeping forsythia granular mass, specifically includes following steps：
A. software is used, the capsule of weeping forsythia particle forsythin built, water and basis weight model are imported, and set the content of each component
Limit, according to the quality standard of capsule of weeping forsythia particle, sets forsythin >=8.6mg/g, the multi-party of capsule of weeping forsythia particle is set up in moisture≤8.0
Method evaluation model；
B. sample near-infrared absorption spectrum figure is gathered, spectrogram is imported in multi-method evaluation model, sample each group is read
The content and evaluation information divided.
To verify the predictive ability and accuracy of this model, the present invention is using mono blind method experiment, to the capsule of weeping forsythia, red sage root etc. 10 batches
Particulate samples are evaluated, and sample message table is shown in Table 5.The spectrogram of the sample of numbering 1~10 is gathered respectively, and spectrogram is imported and connected
Stick up in particle multi-method evaluation model, read the content and evaluation information of sample each component, the results are shown in Table 6.
The multi-method evaluation model verification sample information table of table 5
The capsule of weeping forsythia particle multi-method evaluation result of table 6
- represent to survey sample passes, * represents that institute's test sample product are abnormal (different samples or content are undesirable)
As can be seen from Table 6, the multi-method evaluation model can according to sample spectra information, analyze draw mahalanobis distance,
Whether density of fraction, by the size of its value, can be capsule of weeping forsythia particle with principium identification institute test sample product, be identified as capsule of weeping forsythia 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 capsule of weeping forsythia particle.
Claims (6)
1. a kind of detection method of capsule of weeping forsythia particle, it is characterised in that be the detection method based on near-infrared spectrum technique, and including
Following steps：
A. the collection of the collection of near infrared spectrum：Capsule of weeping forsythia particulate samples about 3g is taken, fine powder is ground into, near infrared spectrum scanning is carried out,
Spectrum is gathered, the original absorbance spectrogram of capsule of weeping forsythia particulate samples is obtained, and each component content is measured, capsule of weeping forsythia particle is measured
The measured value of sample each component content, calibration set and checking are determined according to sample number and sample each component content actual measurement Distribution value
Collection；The condition of scanning of described near infrared spectra collection is：Scanning range is 4000cm-1-12000cm-1, scanning times are 32
Secondary, resolution ratio is 8cm-1, background correction, 3 spectrum of every part of sample collection in real time in scanning process；
B. the foundation of capsule of weeping forsythia particle quantitative model：The content of capsule of weeping forsythia pellet moisture is determined, using subtracting straight line method to original
Absorption spectrum is pre-processed, and the spectral region of modeling chooses 9401.7-4247.9cm-1Characteristic wave bands, dimension elects 10 as；Determine
Capsule of weeping forsythia particle Determination of forsythin, is pre-processed using first derivative+subtract straight line method to original absorbance spectrum, modeling
Spectral region chooses 9401.7-4598.8cm-1Wave band is characterized, dimension elects 6 as；With PLS to the near of calibration set
Quantitative model is set up between infrared spectrum and the measured value of its correspondence capsule of weeping forsythia 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 capsule of weeping forsythia particulate samples each component content, predicted value is compared with measured value, and checking is quantitative
The accuracy of model；
D. the measure of capsule of weeping forsythia particle each component content：Capsule of weeping forsythia 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 capsule of weeping forsythia particle each component is determined；
The near-infrared quantitative determination model of the capsule of weeping forsythia pellet moisture built up and forsythin is integrated by near-infrared analysis software, set up
Capsule of weeping forsythia particulate samples to be detected are gathered near infrared spectrum by the multi-method evaluation model of capsule of weeping forsythia particle according to step a method,
Import in capsule of weeping forsythia particle multi-method evaluation model, while determining capsule of weeping forsythia particle each component content；
Described capsule of weeping forsythia particle is prepared by the method comprised the following steps：Capsule of weeping forsythia medicine materical crude slice is taken, plus 2-5 times is measured water, heating is steamed
Evaporate 1-3 hours, collect volatile oil and aqua aromatica, with beta-cyclodextrin inclusion compound, obtain Benexate Hydrochloride, decoction filtration is standby；Medicine
Slag is added water to cook 2-3 times, and each 5-10 times is measured water, and heating is decocted 1-2 hours, and decoction merges；Filtrate is concentrated into relative density
1.02-1.12 clear cream, is filtered with 250-350 mesh sieves while hot；Qinghuo reagent is spray-dried, and obtains spray powder；By beta-schardinger dextrin
Inclusion compound is well mixed with spray powder, dry granulation, obtains capsule of weeping forsythia particle of the granularity in 16-40 mesh；Moisture in capsule of weeping forsythia particle≤
8.0%, forsythin >=8.6mg/g.
2. the detection method of capsule of weeping forsythia particle as claimed in claim 1, it is characterised in that described capsule of weeping forsythia particle is by including as follows
The method of step is prepared：Take capsule of weeping forsythia medicine materical crude slice, plus 3 times of amount water, heating distillation 2 hours, collect volatile oil and aqua aromatica, with β-
It is cyclodextrin encapsulated, Benexate Hydrochloride is obtained, decoction filtration is standby；The dregs of a decoction are added water to cook 3 times, and 8 times of amount water, heats and decoct every time
Boil 1.5 hours, decoction merges；Filtrate is concentrated into the clear cream that relative density is 1.09, is filtered while hot with 350 mesh sieves；Entering wind-warm syndrome
170-185 DEG C of degree, expects 400-700 revs/min of revolution speed, 85-95 DEG C of leaving air temp, and wind send progress under conditions of 35-45 DEG C of temperature
Spray drying, obtains spray powder；Spray powder is well mixed with Benexate Hydrochloride, in punching panel aperture 1.50mm, roll electricity
Dry granulation under the conditions of unit frequency 40HZ, feeding motor frequency 45HZ, oil cylinder working-pressure 20bar, obtains the capsule of weeping forsythia of the granularity in 16-40 mesh
Particle.
3. the detection method of capsule of weeping forsythia particle as claimed in claim 1 or 2, it is characterised in that the sample that capsule of weeping forsythia particle near-infrared is determined
Product preparation method is：Same batch capsule of weeping forsythia particle about 3g is taken, fine powder is ground into, 80 mesh sieves are crossed, near-infrared measure is transferred to
Tool plug vial in.
4. the detection method of capsule of weeping forsythia particle as claimed in claim 1 or 2, it is characterised in that carry out grinding fine powder using funnel
Transfer, is made it close by way of up-down vibration, is stoppered with bottle closure of rubber.
5. the detection method of capsule of weeping forsythia 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 capsule of weeping forsythia particle as claimed in claim 1 or 2, it is characterised in that the sample bottle bottom after observation dress sample
Portion, it is ensured that the sample powder of test does not bond vial bottom, just can carry out near infrared spectrum scanning to sample.
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Denomination of invention: A detection method for Forsythia suspensa particles Effective date of registration: 20231225 Granted publication date: 20170825 Pledgee: Bank of China Limited by Share Ltd. Foshan branch Pledgor: GUANGDONG YIFANG PHARMACEUTICAL Co.,Ltd. Registration number: Y2023980073969 |