CN106109556B - A kind of detection method of licorice root particles - Google Patents
A kind of detection method of licorice root particles Download PDFInfo
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- CN106109556B CN106109556B CN201610459103.3A CN201610459103A CN106109556B CN 106109556 B CN106109556 B CN 106109556B CN 201610459103 A CN201610459103 A CN 201610459103A CN 106109556 B CN106109556 B CN 106109556B
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- 244000303040 Glycyrrhiza glabra Species 0.000 title claims abstract description 134
- 235000006200 Glycyrrhiza glabra Nutrition 0.000 title claims abstract description 133
- 239000002245 particle Substances 0.000 title claims abstract description 127
- 235000017443 Hedysarum boreale Nutrition 0.000 title claims abstract description 120
- 235000007858 Hedysarum occidentale Nutrition 0.000 title claims abstract description 120
- 239000001947 glycyrrhiza glabra rhizome/root Substances 0.000 title claims abstract description 120
- 238000001514 detection method Methods 0.000 title claims abstract description 28
- 238000000034 method Methods 0.000 claims abstract description 66
- LPLVUJXQOOQHMX-QWBHMCJMSA-N glycyrrhizinic acid Chemical compound O([C@@H]1[C@@H](O)[C@H](O)[C@H](O[C@@H]1O[C@@H]1C([C@H]2[C@]([C@@H]3[C@@]([C@@]4(CC[C@@]5(C)CC[C@@](C)(C[C@H]5C4=CC3=O)C(O)=O)C)(C)CC2)(C)CC1)(C)C)C(O)=O)[C@@H]1O[C@H](C(O)=O)[C@@H](O)[C@H](O)[C@H]1O LPLVUJXQOOQHMX-QWBHMCJMSA-N 0.000 claims abstract description 41
- 239000003814 drug Substances 0.000 claims abstract description 32
- 239000000843 powder Substances 0.000 claims abstract description 27
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 19
- 235000011477 liquorice Nutrition 0.000 claims abstract description 13
- 239000007921 spray Substances 0.000 claims abstract description 12
- 239000000706 filtrate Substances 0.000 claims abstract description 10
- 239000006071 cream Substances 0.000 claims abstract description 9
- 238000010438 heat treatment Methods 0.000 claims abstract description 8
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- 239000003153 chemical reaction reagent Substances 0.000 claims abstract description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 57
- VTAJIXDZFCRWBR-UHFFFAOYSA-N Licoricesaponin B2 Natural products C1C(C2C(C3(CCC4(C)CCC(C)(CC4C3=CC2)C(O)=O)C)(C)CC2)(C)C2C(C)(C)CC1OC1OC(C(O)=O)C(O)C(O)C1OC1OC(C(O)=O)C(O)C(O)C1O VTAJIXDZFCRWBR-UHFFFAOYSA-N 0.000 claims description 29
- LPLVUJXQOOQHMX-UHFFFAOYSA-N glycyrrhetinic acid glycoside Natural products C1CC(C2C(C3(CCC4(C)CCC(C)(CC4C3=CC2=O)C(O)=O)C)(C)CC2)(C)C2C(C)(C)C1OC1OC(C(O)=O)C(O)C(O)C1OC1OC(C(O)=O)C(O)C(O)C1O LPLVUJXQOOQHMX-UHFFFAOYSA-N 0.000 claims description 29
- 239000001685 glycyrrhizic acid Substances 0.000 claims description 29
- 229960004949 glycyrrhizic acid Drugs 0.000 claims description 29
- UYRUBYNTXSDKQT-UHFFFAOYSA-N glycyrrhizic acid Natural products CC1(C)C(CCC2(C)C1CCC3(C)C2C(=O)C=C4C5CC(C)(CCC5(C)CCC34C)C(=O)O)OC6OC(C(O)C(O)C6OC7OC(O)C(O)C(O)C7C(=O)O)C(=O)O UYRUBYNTXSDKQT-UHFFFAOYSA-N 0.000 claims description 29
- 235000019410 glycyrrhizin Nutrition 0.000 claims description 29
- KSDSYIXRWHRPMN-UHFFFAOYSA-N 4'-O-beta-D-Galactopyranoside-6''-p-Coumaroylprunin-4',5,7-Trihydroxyflavanone Natural products OC1C(O)C(O)C(CO)OC1OC1=CC=C(C2OC3=CC(O)=CC(O)=C3C(=O)C2)C=C1 KSDSYIXRWHRPMN-UHFFFAOYSA-N 0.000 claims description 28
- DEMKZLAVQYISIA-ONJCETCRSA-N Liquiritin Natural products O([C@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1)c1ccc([C@@H]2Oc3c(C(=O)C2)ccc(O)c3)cc1 DEMKZLAVQYISIA-ONJCETCRSA-N 0.000 claims description 28
- DEMKZLAVQYISIA-UHFFFAOYSA-N Liquirtin Natural products OC1C(O)C(O)C(CO)OC1OC1=CC=C(C2OC3=CC(O)=CC=C3C(=O)C2)C=C1 DEMKZLAVQYISIA-UHFFFAOYSA-N 0.000 claims description 28
- DEMKZLAVQYISIA-ZRWXNEIDSA-N liquiritin Chemical compound O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@H]1OC1=CC=C([C@H]2OC3=CC(O)=CC=C3C(=O)C2)C=C1 DEMKZLAVQYISIA-ZRWXNEIDSA-N 0.000 claims description 28
- GSZUGBAEBARHAW-UHFFFAOYSA-N sophoraflavone B Natural products OC1C(O)C(O)C(CO)OC1OC1=CC=C(C=2OC3=CC(O)=CC=C3C(=O)C=2)C=C1 GSZUGBAEBARHAW-UHFFFAOYSA-N 0.000 claims description 28
- 238000002329 infrared spectrum Methods 0.000 claims description 25
- 238000000605 extraction Methods 0.000 claims description 21
- 238000001228 spectrum Methods 0.000 claims description 20
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- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 3
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- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 2
- 244000025254 Cannabis sativa Species 0.000 description 2
- 229920002774 Maltodextrin Polymers 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
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- 150000002338 glycosides Chemical class 0.000 description 2
- 238000004811 liquid chromatography Methods 0.000 description 2
- -1 liquorice glycosides Chemical class 0.000 description 2
- HQKMJHAJHXVSDF-UHFFFAOYSA-L magnesium stearate Chemical compound [Mg+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O HQKMJHAJHXVSDF-UHFFFAOYSA-L 0.000 description 2
- 238000002203 pretreatment Methods 0.000 description 2
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- 241001411320 Eriogonum inflatum Species 0.000 description 1
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- 241001278898 Glycyrrhiza inflata Species 0.000 description 1
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- 238000004128 high performance liquid chromatography Methods 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- LTINPJMVDKPJJI-UHFFFAOYSA-N iodinated glycerol Chemical compound CC(I)C1OCC(CO)O1 LTINPJMVDKPJJI-UHFFFAOYSA-N 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 235000021374 legumes Nutrition 0.000 description 1
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- YTJSFYQNRXLOIC-UHFFFAOYSA-N octadecylsilane Chemical compound CCCCCCCCCCCCCCCCCC[SiH3] YTJSFYQNRXLOIC-UHFFFAOYSA-N 0.000 description 1
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Classifications
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/48—Fabaceae or Leguminosae (Pea or Legume family); Caesalpiniaceae; Mimosaceae; Papilionaceae
- A61K36/484—Glycyrrhiza (licorice)
-
- 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
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N21/3563—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing solids; Preparation of samples therefor
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N21/359—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light using near infrared light
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
- A61K2236/331—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using water, e.g. cold water, infusion, tea, steam distillation, decoction
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/39—Complex extraction schemes, e.g. fractionation or repeated extraction steps
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/51—Concentration or drying of the extract, e.g. Lyophilisation, freeze-drying or spray-drying
Abstract
The invention discloses licorice root particles and its Chinese medicine preparation.The licorice root particles are prepared by the method comprised the following steps：Extracting liquorice medicine materical crude slice, is added water to cook 23 times, and 5 10 times of amount water are added every time, and 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, licorice root particles of the granularity in 16 40 mesh are obtained.The licorice root particles preparation technology 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 licorice root particles and its Chinese medicine preparation.
Background technology
Radix glycyrrhizae is glycyrrhizic legume Glycyrrhiza uralensis Fisch., swollen fruit Radix Glycyrrhiza
Inflata Bat. or glycyrrhiza glabra Glycyrrhiza glabra L. dry root and rhizome, it is sweet, put down, the thoughts of returning home, lung, spleen, stomach
Through clearing heat and detoxicating with invigorating the spleen and benefiting qi, expelling phlegm and arresting coughing, relieving spasm to stop pain, effect of coordinating the drug actions of a prescription.
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, used with card plus-minus, formula.With traditional Chinese medicine decoction " medicine materical crude slice is used as medicine,
Face and decocted with existing " 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 without decocting when using
Boil, 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 licorice root particles needs several hours, operation with reference to the method for pharmacopeia
Also it is more complicated.The main chemical compositions of licorice root particles are liquiritin, glycyrrhizic acid, and as quality control index, conventional method is used
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 is larger and right
Inspector's body has been damaged, and feedback of the information is delayed, it is impossible to meet instant analysis multi items during particle enterprise large-scale production,
The need for 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 sweet of production technology standardization
Grass particle, its preparation technology is simple, steady quality.Meanwhile, in order to better control over the quality of licorice root particles, 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 licorice root particles.
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 licorice root particles, it is prepared by the method comprised the following steps：Extracting liquorice
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 licorice root particles of the granularity in 16-40 mesh.
Present inventor has found that radix glycyrrhizae adds 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, licorice root particles of the invention are prepared by the method comprised the following steps：Extracting liquorice medicine materical crude slice, adds 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 glycyrrhizae of the granularity in 16-40 mesh
Grain.
Moisture≤8.0% in the process for producing optimized by the present invention, gained licorice root particles, ethanol soluble extraction >=
25.0%, liquiritin >=8.5mg/g, glycyrrhizic acid >=29.0mg/g.
The licorice root particles of the present invention can be further applied in various Chinese medicine preparations, to realize the pharmacological activity of radix glycyrrhizae.Often
The Chinese medicine preparation comprising licorice root particles 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 licorice root particles 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：Extracting liquorice particulate samples about 3g, is ground into fine powder, carries out near infrared spectrum scanning, adopts
Collect spectrum, obtain the original absorbance spectrogram of licorice root particles sample, and each component content is measured, measure licorice root particles sample
The predicted value of product each component content, determines that calibration set and checking collect according to sample number and sample each component content prediction Distribution value；
B. the foundation of licorice root particles quantitative model：The content of licorice root particles moisture is determined, using first derivative+vector normalizing
Change method is pre-processed to original absorbance spectrum, and the spectral region of modeling chooses 7500.2-6096.5cm-1、4603-4248cm-1Characteristic wave bands, dimension elects 6 as；Licorice root particles ethanol soluble extraction content is determined, using vector normalization method to original absorbance spectrum
Pre-processed, the spectral region of modeling is chosen for 9401.8-7496.2cm-1、5774.1-5447.7cm-1、4603-4248cm-1Characteristic wave bands, dimension elects 10 as；The content of licorice root particles liquiritin is determined, using vector normalization method to original absorbance spectrum
Pre-processed, the spectral region of modeling is chosen for 9401.8-5447.7cm-1、4603-4248cm-1Characteristic wave bands, dimension choosing
For 8；The content of licorice root particles glycyrrhizic acid is determined, original absorbance spectrum is pre-processed using vector normalization method, modeling
Spectral region is chosen for 6100.6-4248cm-1Characteristic wave bands, dimension elects 9 as；With PLS to the near red of calibration set
Quantitative model is set up between the predicted value of external spectrum and its correspondence licorice root particles sample 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 licorice root particles sample each component content, predicted value is compared with predicted value, verifies
The accuracy of quantitative model；
D. the measure of licorice root particles each component content：Licorice root particles to be detected are 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 licorice root particles each component
Amount；The near-infrared quantitative determination model of the licorice root particles moisture, extract and the liquiritin that are built up, glycyrrhizic acid is passed through into near-infrared
Analysis software is integrated, and the multi-method evaluation model of licorice root particles is set up, by the side of licorice root particles sample to be detected according to step a
Method gathers near infrared spectrum, imports in licorice root particles multi-method evaluation model, while determining licorice root particles each component content.
Using above-mentioned detection method, moisture, ethanol soluble extraction and liquiritin, the glycyrrhizic acid that licorice root particles can be determined simultaneously contain
Amount, it is only necessary to which a few minutes just can complete the detection of each group divided data, substantially reduces detection time, adapts to modern enterprise fast
Speed, the demand largely produced.And traditional detection method, using high effective liquid chromatography for measuring liquiritin, glycyrrhizic acid content, drying
Method determines moisture, ethanol soluble extractives determination method and determines ethanol soluble extraction content, cumbersome, not only needs a variety of instruments
Equipment, also needing each to examine post to cooperate can just smoothly complete, and data handling procedure is more complicated, time-consuming.Meanwhile, this hair
Bright method can be applicable each component assay of the material of 3 production links, including medicinal extract, spray dried powder, particle simultaneously.
In order to more accurately determine, in the assay method of the present invention, the sample preparation that licorice root particles near-infrared is determined
Method is：Same batch licorice root particles 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 extract of licorice root, 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
Grain method, greatly reduces the workload of model foundation, realizes the quality control to each key link material of licorice root particles.
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 licorice root particles each component near-infrared
On the basis of model, licorice root particles 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 liquiritin, glycyrrhizic acid, while can be distinguished according to mahalanobis distance and density of fraction etc. again
The 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 licorice root particles
Skill, and preparation technology is simple, technological parameter is stable and easy to control, is adapted to the preparation of glycyrrhiza dispensing granule.(2) present invention is based near
Infrared spectrum technology combination chemometrics method, in certain spectral region, establishes licorice root particles 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 licorice root particles 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 licorice root particles samples；
Related figure between Fig. 2 licorice root particles moisture near-infrared predicted value and predicted value；
The comparison column diagram of Fig. 3 licorice root particles moisture near-infrared predicted value and predicted value；
Related figure between Fig. 4 licorice root particles ethanol soluble extraction near-infrared predicted value and predicted value；
The comparison column diagram of Fig. 5 licorice root particles ethanol soluble extraction near-infrared predicted value and predicted value；
Related figure between Fig. 6 licorice root particles liquiritin near-infrared predicted value and predicted value；
The comparison column diagram of Fig. 7 licorice root particles liquiritin near-infrared predicted value and predicted value；
Related figure between Fig. 8 licorice root particles glycyrrhizic acid near-infrared predicted value and predicted value；
The comparison column diagram of Fig. 9 licorice root particles glycyrrhizic acid near-infrared predicted value and predicted 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 licorice root particles：Extracting liquorice medicine materical crude slice, is added water to cook 3 times, 8 times of amount water is 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, is filtered while hot with 350 mesh sieves；In 185 DEG C of EAT,
Expect 400 revs/min of revolution speed, 95 DEG C of leaving air temp, wind is spray-dried under conditions of sending 40 DEG C of temperature, obtains spray powder；In punching
Dry granulation under the conditions of orifice plate aperture 1.50mm, roller motor frequency 40HZ, feeding motor frequency 45HZ, oil cylinder working-pressure 20bar,
Obtain licorice root particles of the granularity in 40 mesh.
Embodiment 2：
The preparation of Chinese medicine preparation containing licorice root particles：Extracting liquorice medicine materical crude slice, is added water to cook 3 times, 8 times of amount water is 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, is filtered while hot with 350 mesh sieves；
185 DEG C of EAT, expects 400 revs/min of revolution speed, and 95 DEG C of leaving air temp, wind is spray-dried under conditions of sending 40 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 licorice root particles of the granularity in 40 mesh；200g licorice root particles and 85g maltodextrins are mixed, added appropriate
Magnesium stearate, mixes, is pressed into 1000.
Embodiment 3
A kind of method based on near-infrared spectrum technique quick detection licorice root particles moisture, specifically includes following step
Suddenly：
A, extracting liquorice particulate samples, respectively take about 3g, are ground into fine powder by totally 101 batches, are fitted into tool plug glass sample bottle, are placed in
It is scanned on infrared diaphanoscopy instrument, gathers spectrum, the condition of scanning：Scanning range 4000-12000cm-1, scanning times：32
It is secondary, resolution ratio 8cm-1, background correction in real time in scanning process, 3 spectrum of every part of sample collection obtain as shown in Figure 1 101 batches
The near-infrared original absorbance spectrogram of licorice root particles；
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 licorice root particles 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, licorice root particles are 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 70 batches, and it is checking to choose 31 batches
Collection.Analysis software, Automatic Optimal chooses preprocess method and spectral region, and optimum results are shown in Table 1.Using first derivative+
Vector normalization method is pre-processed to near-infrared original absorbance spectrum, chooses 7500.2-6096.5cm-1、4603-4248cm-1
Spectral information under characteristic wave bands, sets up between near infrared spectrum and moisture predicted value with PLS (PLS)
Quantitative model；The sample for verifying collection is subjected near infrared spectrum scanning, using model, the pre- of licorice root particles sample size is obtained
Measured value, predicted value is compared with predicted value, verifies the accuracy and predictive ability of quantitative model, the model is through cross validation
Obtain cross validation coefficient R2=0.902, RMSECV=0.364, RPD=3.2, dimension elect 6, checking collection coefficient R as2
The determination of moisture of=0.838, RMSEP=0.419,31 batch licorice root particles the results are shown in Table 2, moisture predicted value and predicted value it
Between related figure see Fig. 2, the comparison column diagram of moisture predicted value and predicted 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 31 batches of licorice root particles of table
The deviation range of licorice root particles moisture is between 0.03-0.87% it can be seen from upper table 2, consensus forecast
The rate of recovery is 97.56%, illustrates that the model has preferable predictive ability and stability, available for the quick of licorice root particles moisture
Detection.
Embodiment 4：
A kind of method based on near-infrared spectrum technique quick detection licorice root particles ethanol soluble extraction content, specifically include as
Lower step：
A, extracting liquorice particulate samples, respectively take about 3g, are ground into fine powder by totally 101 batches, are fitted into tool plug glass sample bottle, are placed in
It is scanned on infrared diaphanoscopy instrument, gathers spectrum, the condition of scanning：Scanning range 4000-12000cm-1, scanning times：32
It is secondary, resolution ratio 8cm-1, background correction in real time in scanning process, 3 spectrum of every part of sample collection obtain as shown in Figure 1 101 batches
The near-infrared original absorbance spectrogram of licorice root particles；
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 licorice root particles 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 licorice root particles 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 70 batches, chooses 31 batches
For checking collection.Analysis software, Automatic Optimal chooses preprocess method and spectral region, and optimum results are shown in Table 3.Using vector
Normalization method is pre-processed to near-infrared original absorbance spectrum, chooses 9401.8-7496.2cm-1、5774.1-5447.7cm-1、4603-4248cm-1Spectral information under characteristic wave bands, near infrared spectrum and ethanol are set up with PLS (PLS)
Quantitative model between extract content predicted value；The sample for verifying collection is subjected near infrared spectrum scanning, using model, obtained
The predicted value of licorice root particles sample size, predicted value is compared with predicted value, verifies accuracy and the prediction of quantitative model
Ability, the model obtains cross validation coefficient R through cross validation2=0.923, RMSECV=1.98, RPD=3.61, dimension
Elect 10, checking collection coefficient R as2The ethanol soluble extraction assay knot of=0.835, RMSEP=2.71,31 batch licorice root particles
Fruit is shown in Table 4, and the related figure between ethanol soluble extraction predicted value and predicted value is shown in Fig. 4, ethanol soluble extraction predicted value and predicted value
Compare column diagram and see 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 31 batches of licorice root particles of table
The deviation range of licorice root particles ethanol soluble extraction content is between 0.04-4.88% it can be seen from upper table 4, in advance
It is 97.85% to survey average recovery rate, illustrates that the model has preferable predictive ability and stability, available for licorice root particles ethanol
The quick detection of extract.
Embodiment 5：
Liquiritin, the method for glycyrrhizic acid content in a kind of quick detection licorice root particles based on near-infrared spectrum technique, specifically
Comprise the following steps：
A, extracting liquorice particulate samples, respectively take about 3g, are ground into fine powder by totally 101 batches, are fitted into tool plug glass sample bottle, are placed in
It is scanned on infrared diaphanoscopy instrument, gathers spectrum, the condition of scanning：Scanning range 4000-12000cm-1, scanning times：32
It is secondary, resolution ratio 8cm-1, background correction in real time in scanning process, 3 spectrum of every part of sample collection obtain as shown in Figure 1 101 batches
The near-infrared original absorbance spectrogram of licorice root particles；
Meanwhile, the standard method according to specified in 2015 editions Chinese Pharmacopoeias, its liquiritin, glycyrrhizic acid content shine 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 0.05% phosphoric acid solution as Mobile phase B, the regulation according to the form below carries out gradient elution；Detection wavelength 237nm.Theoretical plate
Number is calculated by liquiritin peak should be not less than 5000.
The preparation of reference substance solution：Extracting liquorice glycosides reference substance, glycyrrhizic acid reference substance are appropriate, accurately weighed, plus 70% ethanol
Mixed solutions of every 1ml containing the μ g of liquiritin 12, the μ g of ammonium glycyrrhetate 60 is made, produce (glycyrrhizic acid weight=ammonium glycyrrhetate weight/
1.0207)。
The preparation of need testing solution takes this product under content uniformity, finely ground, takes about 0.1g, accurately weighed, puts tool plug cone
In shape bottle, precision 70% ethanol 100ml of addition, weighed weight, ultrasonically treated (power 300W, frequency 35kHz) 30 minutes is put
It is cold, then weighed weight, the weight of less loss is supplied with 70% ethanol, is shaken up, is filtered, is taken subsequent filtrate, produce.
Determination method is accurate respectively to draw reference substance solution and each 10 μ l of need testing solution, injects liquid chromatograph, determines, i.e.,
.
B, Distribution value surveyed according to sample number and sample liquiritin, glycyrrhizic acid content, it is calibration set to choose 70 batches, chooses 31
Criticize as checking collection.Analysis software, Automatic Optimal chooses preprocess method and spectral region, and optimum results are shown in Table 5.Using one
Order derivative+vector normalization method is pre-processed to near-infrared original absorbance spectrum, chooses 9401.8-5447.7cm-1、4603-
4248cm-1Spectral information under characteristic wave bands, sets up near infrared spectrum with PLS (PLS) and liquiritin standard contains
Quantitative model between amount；Near-infrared original absorbance spectrum is pre-processed using first derivative+vector normalization method, chosen
6100.6-4248cm-1Spectral information under characteristic wave bands, near infrared spectrum and radix glycyrrhizae are set up with PLS (PLS)
Quantitative model between sour standard content；The sample for verifying collection is subjected near infrared spectrum scanning, using model, radix glycyrrhizae is obtained
The predicted value of grain sample liquiritin and glycyrrhizic acid content, predicted value is compared with predicted value, verifies the accurate of quantitative model
Property and predictive ability, liquiritin quantitative model obtain cross validation coefficient R through cross validation2=0.922, RMSECV=
1.96, RPD=3.58, dimension elects 8, checking collection coefficient R as2=0.862, RMSEP=2.6；Glycyrrhizic acid quantitative model is passed through
Cross validation obtains cross validation coefficient R2=0.922, RMSECV=1.96, RPD=3.58, dimension elect 9, checking collection phase as
Close coefficients R2=0.870, RMSEP=4.32.The liquiritin of 31 batches of licorice root particles, glycyrrhizic acid content measurement result are shown in Table 6, radix glycyrrhizae
Related figure between glycosides, glycyrrhizic acid predicted value and predicted value is shown in Fig. 6,8, the comparison of liquiritin, glycyrrhizic acid predicted value and predicted value
Column diagram is shown in Fig. 7,9.
The liquiritin of table 5, model parameter of the radix glycyrrhizae acid profile under different spectral regions and preprocess method
6 31 batches of licorice root particles liquiritins of table, glycyrrhizic acid content measurement result
Deviation of the deviation range of licorice root particles liquiritin in 0.47-12.03mg/g, glycyrrhizic acid it can be seen from upper table 6
Scope is between 0.05-5.66mg/g, and liquiritin prediction average recovery rate is that 102.55%, glycyrrhizic acid prediction average recovery rate is
98.8%.Liquiritin is except 2,3,15, No. 17 sample variations are larger, and remaining sample variation is smaller；Glycyrrhizic acid is inclined except No. 12 samples
Difference is larger, and remaining sample variation is smaller；Illustrate that model has preferable predictive ability and stability, it is sweet available for licorice root particles
The quick inspection of careless glycosides, glycyrrhizic acid.
Embodiment 6:
A kind of method based on near-infrared spectrum technique Fast Evaluation licorice root particles quality, specifically includes following steps：
A. software is used, the licorice root particles liquiritin built, glycyrrhizic acid, moisture and extract quantitative model are imported, and
The content limit of each component is set, according to the quality standard of licorice root particles, moisture≤8.0% is set, ethanol soluble extraction >=
25.0%, liquiritin >=8.5mg/g, glycyrrhizic acid >=29.0mg/g sets up the multi-method evaluation model of licorice root particles；
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 glycyrrhizae, red sage root etc. 10 batches
Particulate samples are evaluated, and sample message table is shown in Table 7.The spectrogram of the sample of numbering 1~10 is gathered respectively, spectrogram is imported sweet
In grass particle multi-method evaluation model, the content and evaluation information of sample each component are read, 8 are the results are shown in Table.
The multi-method evaluation model verification sample information table of table 7
The licorice root particles 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 licorice root particles with principium identification institute test sample product, be identified as licorice root particles
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 licorice root particles.
Claims (6)
1. a kind of detection method of licorice root particles, 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：Extracting liquorice particulate samples about 3g, is ground into fine powder, carries out near infrared spectrum scanning, gathers light
Spectrum, obtains the original absorbance spectrogram of licorice root particles sample, and each component content is measured, and measures licorice root particles sample each
The predicted value of constituent content, determines that calibration set and checking collect according to sample number and sample each component content prediction Distribution value, described
NIR spectra collection the condition of scanning be：Scanning range is 4000cm-1-12000cm-1, scanning times are 32 times, and resolution ratio is
8cm-1, background correction, 3 spectrum of every part of sample collection in real time in scanning process；
B. the foundation of licorice root particles quantitative model：The content of licorice root particles moisture is determined, using first derivative+vector normalization method
Original absorbance spectrum is pre-processed, the spectral region of modeling chooses 7500.2-6096.5cm-1、4603-4248cm-1Feature
Wave band, dimension elects 6 as；Licorice root particles ethanol soluble extraction content is determined, original absorbance spectrum is carried out using vector normalization method
Pretreatment, the spectral region of modeling is chosen for 9401.8-7496.2cm-1、5774.1-5447.7cm-1、4603-4248cm-1It is special
Wave band is levied, dimension elects 10 as；The content of licorice root particles liquiritin is determined, original absorbance spectrum is carried out using vector normalization method
Pretreatment, the spectral region of modeling is chosen for 9401.8-5447.7cm-1、4603-4248cm-1Characteristic wave bands, dimension elects 8 as；
The content of licorice root particles glycyrrhizic acid is determined, original absorbance spectrum is pre-processed using vector normalization method, the spectrum of modeling
Scope is chosen for 6100.6-4248cm-1Characteristic wave bands, dimension elects 9 as；With near infrared light of the PLS to calibration set
Quantitative model is set up between the predicted value of spectrum and its correspondence licorice root particles sample each component content；
C. near-infrared quantitative model is verified：The atlas of near infrared spectra of collection checking collection sample, each component set up by step b
Quantitative model, obtains the predicted value of licorice root particles sample each component content, predicted value is compared with predicted value, and checking is quantitative
The accuracy of model；
D. the measure of licorice root particles each component content：Licorice root particles to be detected are 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 licorice root particles each component is determined；
The near-infrared quantitative determination model of the licorice root particles moisture, extract and the liquiritin that are built up, glycyrrhizic acid is passed through into near-infrared point
Analyse software to integrate, the multi-method evaluation model of licorice root particles is set up, by the method for licorice root particles sample to be detected according to step a
Near infrared spectrum is gathered, is imported in licorice root particles multi-method evaluation model, while determining licorice root particles each component content；
Described licorice root particles are prepared by the method comprised the following steps：Extracting liquorice medicine materical crude slice, 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 licorice root particles of 16-40 mesh；Moisture≤8.0% in licorice root particles, ethanol soluble extraction >=25.0%, liquiritin >=8.5mg/
G, glycyrrhizic acid >=29.0mg/g.
2. the detection method of licorice root particles as claimed in claim 1, it is characterised in that described licorice root particles are by including as follows
The method of step is prepared：Extracting liquorice medicine materical crude slice, is added water to cook 3 times, and 8 times of amount water are added every time, and 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 licorice root particles of the granularity in 16-40 mesh.
3. the detection method of licorice root particles as claimed in claim 1 or 2, it is characterised in that：Take same batch licorice root particles 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 licorice root particles 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 licorice root particles 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 licorice root particles 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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