CN106074679A - A kind of Radix Puerariae granule and Chinese medicine preparation thereof - Google Patents

A kind of Radix Puerariae granule and Chinese medicine preparation thereof Download PDF

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CN106074679A
CN106074679A CN201610454185.2A CN201610454185A CN106074679A CN 106074679 A CN106074679 A CN 106074679A CN 201610454185 A CN201610454185 A CN 201610454185A CN 106074679 A CN106074679 A CN 106074679A
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radix puerariae
granule
spectrum
sample
puerariae granule
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CN106074679B (en
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王闽予
朱德全
霍文杰
刘丽萍
陈向东
谭登平
程学仁
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Zhejiang Yifang Pharmaceutical Co Ltd
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Guangdong Yifang Pharmaceutical Co Ltd
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18Magnoliophyta (angiosperms)
    • A61K36/185Magnoliopsida (dicotyledons)
    • A61K36/48Fabaceae or Leguminosae (Pea or Legume family); Caesalpiniaceae; Mimosaceae; Papilionaceae
    • A61K36/488Pueraria (kudzu)
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K9/00Medicinal preparations characterised by special physical form
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    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
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    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation 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
    • A61K2236/30Extraction of the material
    • A61K2236/33Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
    • A61K2236/331Extraction 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
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
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    • A61K2236/00Isolation 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
    • A61K2236/30Extraction of the material
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    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
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    • A61K2236/50Methods involving additional extraction steps
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    • G01MEASURING; TESTING
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    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • G01N21/35Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
    • G01N21/3563Investigating 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
    • G01N2021/3572Preparation of samples, e.g. salt matrices

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Abstract

The invention discloses a kind of Radix Puerariae granule and Chinese medicine preparation thereof.Described Radix Puerariae granule is prepared by the method comprised the steps: take Radix Puerariae decoction pieces, boiling 23 times, adds 5 10 times amount water every time, and heating decocts 12 hours;Medicinal liquid merges, and filtrate is concentrated into the clear paste that relative density is 1.02 1.10, filters with 250 350 mesh sieves while hot;Qinghuo reagent is spray-dried, and obtains spray powder;By spray powder dry granulation, obtain the granularity Radix Puerariae granule at 16 40 mesh.The Radix Puerariae granule preparing process of the present invention is simple, and technological parameter is easy to control, and has science, quick, workable detection method.

Description

A kind of Radix Puerariae granule and Chinese medicine preparation thereof
Technical field
The invention belongs to technical field of traditional Chinese medicine preparation, particularly relate to a kind of Radix Puerariae granule and Chinese medicine preparation thereof.
Background technology
Radix Puerariae derives from the dry root of legume pueraria lobata Pueraria lobata (Willd.) Ohwi, sweet, pungent, cool, returns Spleen, stomach, lung meridian, have expelling pathogenic factors from muscles for reducing heat, promoting the production of body fluid to quench thirst, rash, yang invigorating antidiarrheal, dredge the meridian passage, deinebriating effect.
Chinese medicinal granule be the Chinese medicine decoction pieces to meet concocted specification as raw material, extract through modern industry, concentrate, dry Dry, pelletize and the Chinese medicine series of products made, its function, cure mainly, nature and flavor, return through consistent with Chinese medicine decoction pieces, as new Decoction pieces form replaces the prepared slices of Chinese crude drugs to control for clinical syndrome differentiation opinion, with card plus-minus, formula.With Chinese medicine decoction " decoction pieces is used as medicine, Face and decoct 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, easy to carry, safe and sanitary, quality controllable, and can add and subtract with disease, meet the allegro life style of modern.
At present, Chinese medicinal granule mostly is tradition water extraction, or extracts extraction after volatile oil, and different preparation technologies leads The product quality causing to be produced by different manufacturers is inconsistent, and drug effect exists difference.Accordingly, it would be desirable to the extraction process of research standard, Production process with specification Chinese medicinal granule, it is ensured that drug effect.It addition, the quality of Chinese medicinal granule also can be by detection means Restriction, the mensuration of moisture and ethanol soluble extraction in traditional Radix Puerariae granule, need several hours with reference to the method for pharmacopeia, operation The most complicated.The main chemical compositions of Radix Puerariae granule is puerarin, and as quality control index, traditional method uses efficient liquid phase Chromatographys etc., often need to carry out numerous and diverse pretreatment to sample, expend substantial amounts of reagent, and environmental pollution is relatively big and to coroner's body Body has damaged, and information feedback is delayed, it is impossible to meet instant analysis multi items, many batch samples during granule enterprise large-scale production The needs of product.
Along with the development in epoch, near infrared spectrum (NIRS) analytical technology have employed in Chemical Measurement polynary time further Return method and contemporary optics, microcomputer data processing so that near-infrared is developed rapidly, become and dividing in recent years The emerging analytical technology of one " green " of analysis chemical field fast development, have applied widely, measurement is convenient, pollution-free, The advantages such as nothing is destroyed, data are accurate, reliable, are therefore widely used in food, the quantitative analysis in the various field of medicine and qualitative mirror Not.
Summary of the invention
The problem existed for above-mentioned prior art, it is an object of the invention to provide a kind of normalized Pueraria lobota of production technology Root granule, its preparation technology is simple, steady quality.Meanwhile, in order to better control over the quality of Radix Puerariae granule, adapt to industry metaplasia To product batch in the demand of X-ray inspection X during product, additionally provide one fast based on near-infrared spectrum technique fast and accurately The method of speed detection Radix Puerariae granule.
In order to solve the technical problem of the present invention, the present invention is achieved by the following technical solutions:
On the one hand, the invention provides a kind of Radix Puerariae granule, the method comprised the steps prepare: take kudzuvine root drink Sheet, boiling 2-3 time, add 5-10 times amount water every time, heating decocts 1-2 hour;Medicinal liquid merges, and filtrate is concentrated into relative density For the clear paste of 1.02-1.10, filter with 250-350 mesh sieve while hot;Qinghuo reagent is spray-dried, and obtains spray powder;By spray powder Dry granulation, obtains the granularity Radix Puerariae granule at 16-40 mesh.
Present inventor is found by long term test, Radix Puerariae boiling 2-3 time, adds 5-10 times amount water every time, adds Heat decocts and can be extracted more completely by effective ingredient for 1-2 hour.And concentrating the filtrate to relative density is 1.02-1.10's Clear paste, filters with 250-350 mesh sieve while hot, quickly can be removed by the moisture in clear paste by the method being spray-dried, and anti- The loss of effective ingredient is only caused because heated time is longer.
Preferably, the Radix Puerariae granule of the present invention is prepared by the method comprised the steps: takes Radix Puerariae decoction pieces, adds decocting Boiling 3 times, add 8 times amount water every time, heating decocts 1.5 hours every time;Medicinal liquid merge, filtrate be concentrated into relative density be 1.08 clear Cream, filters with 350 mesh sieves while hot;In inlet temperature 150-190 DEG C, expect revolution speed 400-700 rev/min, leaving air temp 80-95 DEG C, wind is spray-dried under conditions of sending temperature 35-45 DEG C, obtains spray powder;At punched-plate aperture 1.50mm, roller motor frequency Dry granulation under the conditions of rate 40-50HZ, feeding electric machine frequency 30-50HZ, oil cylinder working-pressure 16-24bar, obtains granularity at 16-40 mesh Radix Puerariae granule.
The process for producing optimized by the present invention, moisture≤8.0% in gained Radix Puerariae granule, ethanol soluble extraction >= 26.0%, puerarin >=52mg/g.
The Radix Puerariae granule of the present invention can further apply in various Chinese medicine preparation, to realize the pharmacologically active of Radix Puerariae.Often The Chinese medicine preparation comprising Radix Puerariae granule seen is known in the art, those skilled in the art can be combined as required and Application.Preferably, Chinese medicine preparation can add pharmaceutically acceptable adjuvant, such as maltodextrin.
On the other hand, in order to adapt in commercial process product batch in the demand of X-ray inspection X, overcome traditional High effective liquid chromatography for detecting pretreatment is numerous and diverse, reagent consumption big, environmental pollution is relatively big, delayed the lacking of information feedback Point, additionally provides a kind of detection method for Radix Puerariae granule of the present invention, and it quickly detects based on near-infrared spectrum technique, and wraps Include following steps:
A. the collection of near infrared spectrum: take Radix Puerariae particulate samples about 3g, be ground into fine powder, carry out near infrared spectrum scanning, adopt Collection spectrum, obtains the original absorbance spectrogram of Radix Puerariae particulate samples, and is measured each constituent content, measure Radix Puerariae granular The measured value of each constituent content of product, determines calibration set and checking collection according to the distribution of sample number and sample each constituent content measured value;
B. the foundation of Radix Puerariae particle quantitative model: measure the content of Radix Puerariae pellet moisture, uses first derivative+MSC method pair Original absorbance spectrum carries out pretreatment, and the spectral region of modeling chooses 5451.7-4598.8cm-1Characteristic wave bands, dimension elects 7 as; Measure Radix Puerariae granule ethanol soluble extraction content, use first derivative+MSC method that original absorbance spectrum is carried out pretreatment, modeling Spectral region is chosen for 6100.5-4247.9cm-1Characteristic wave bands, dimension elects 9 as;Measure Radix Puerariae granule puerarin content, use First derivative+vector normalization method carries out pretreatment to original absorbance spectrum, and the spectral region of modeling is chosen for 6100.5- 4598.8cm-1Characteristic wave bands, dimension elects 9 as;Use partial least square method to the near infrared spectrum of calibration set and its corresponding Radix Puerariae Quantitative model is set up between the measured value of each constituent content of particulate samples;
C. checking near-infrared quantitative model: gather checking collection sample near infrared light spectrogram, by step b set up each Measured portions model, it is thus achieved that the predictive value of each constituent content of Radix Puerariae particulate samples, compares predictive value with measured value, checking The accuracy of quantitative model;
D. the mensuration of each constituent content of Radix Puerariae granule: take Radix Puerariae granule to be detected and carry out the reddest according to the method for step a External spectrum gathers, and in the quantitative model set up specific band spectral information steps for importing b, measures containing of each component of Radix Puerariae granule Amount;By soft by near-infrared analysis for the near-infrared quantitative determination model of the Radix Puerariae pellet moisture, extractum and the puerarin that are built up Part is integrated, and sets up the multi-method evaluation model of Radix Puerariae granule, by Radix Puerariae particulate samples to be detected according to the method collection of step a Near infrared spectrum, imports in Radix Puerariae granule multi-method evaluation model, measures each constituent content of Radix Puerariae granule simultaneously.
Utilize above-mentioned detection method, the moisture of Radix Puerariae granule, ethanol soluble extraction and puerarin content can be measured simultaneously, it is only necessary to A few minutes just can complete the detection of each component data, substantially reduces the detection time, and adaptation modern enterprise is quick, great Liang Sheng The demand produced.And traditional detection method, use high effective liquid chromatography for measuring puerarin content, moisture analysis content, Ethanol-soluble extractives algoscopy measures ethanol soluble extraction content, complex operation, not only needs multiple instrument and equipment, also needs each to examine Testing post to cooperate and just can smoothly complete, data handling procedure is more complicated, time-consuming.Meanwhile, the method for the present invention can be simultaneously Each constituent content of the material being suitable for 3 production links measures, including extractum, spray drying powder, granule.
In order to more accurately measure, in the assay method of the present invention, prepared by the sample that Radix Puerariae granule near-infrared measures Method is: take same batch Radix Puerariae granule about 3g, is ground into fine powder, crosses 80 mesh sieves, transfers to the tool plug that near-infrared measures In vial.Preferably, grinding fine powder use funnel is shifted, makes it tight by the way of up-down vibration, use rubber Bottle stopper stoppers.It is highly preferred that under the conditions of temperature 18-22 DEG C, humidity 40-50%, granule is ground and quickly bottles.See Examine bottom the sample bottle after dress sample, it is ensured that the sample powder of test does not bond bottom vial, just can carry out the reddest to sample External spectrum scans.
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 Ping, by the way of up-down vibration, reducing the hole of sample powder, minimizing near infrared light the most irregularly runs and causes Error;According to the method for the present invention, for the mensuration of Radix Puerariae 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 measuring particl method, for spray drying powder, the most directly by measuring granule Method, greatly reduces the workload that model is set up, it is achieved the quality control of key link material each to Radix Puerariae granule.
Preferably, in step a, the condition of scanning of described NIR spectra collection is: sweep limits is 4000cm-1- 12000cm-1, scanning times is 32 times, and resolution is 8cm-1, real-time background correction in scanning process, every part of sample collecting 3 Spectrum.
The inventive method has the function of detection by quantitative and qualitative identification.Quantitative determine at Radix Puerariae granule each component near-infrared On the basis of model, establish Radix Puerariae granule multi-method evaluation model, moisture in sample, second can be drawn by the collection of a spectrum The multicomponent content results such as alcohol extract and puerarin, can distinguish again the kind true and false according to mahalanobis distance with density of fraction etc. simultaneously
The inventive method is particularly suited for the products characteristics of Chinese medicinal granule, owing to Chinese medicinal granule is through single decoction pieces processing system Becoming, compare with Chinese native medicine compound prescription pellet or Chinese patent medicine, component is the most single, and employing this method is disturbed less, accuracy is high;In it addition, Medicine granule series of products have kind more than 500, and due to wide in variety, conventional method is difficult to realize qualitative, quantitative detection, the present invention simultaneously Qualitative and quantitative analysis can be completed on the premise of easy, pollution-free simultaneously, find product abnormal risk in time, big to granule The quality control producing intermediate link has great importance.
Therefore, the present invention compared with prior art, has the advantages that the preparation work of (1) specification Radix Puerariae granule Skill, and preparation technology is simple, technological parameter is stable and easy to control, is suitable for the preparation of kudzu root dispensing granule.(2) present invention is based on closely Infrared spectrum technology combines chemometrics method, in certain spectral region, establishes Radix Puerariae granule near-infrared quantitative model, Can be used to qualitative identification, it is not necessary to sample is carried out the pre-treatment of complexity, is ground into fine powder, is not related to any examination simultaneously Agent, environmental protection, safe and nontoxic, be the trend of Quality Control job development from now on, for detection Radix Puerariae granule provide a kind of quickly, accurately New method.The online quality-monitoring that can promote the use in Chinese medicinal granule enterprise production process as a kind of practical approach, right Abnormal products can be pointed out in time, it is ensured that production quality stable, feasible.
Accompanying drawing explanation
The near-infrared original absorbance spectrogram of Fig. 1 Radix Puerariae particulate samples;
Relevant figure between Fig. 2 Radix Puerariae pellet moisture near-infrared predictive value and measured value;
Fig. 3 Radix Puerariae pellet moisture near-infrared predictive value and the comparison bar diagram of measured value;
Relevant figure between Fig. 4 Radix Puerariae granule ethanol soluble extraction near-infrared predictive value and measured value;
Fig. 5 Radix Puerariae granule ethanol soluble extraction near-infrared predictive value and the comparison bar diagram of measured value;
Relevant figure between Fig. 6 Radix Puerariae granule puerarin near-infrared predictive value and measured value;
Fig. 7 Radix Puerariae granule puerarin near-infrared predictive value and the comparison bar diagram of measured value.
Detailed description of the invention
Further illustrating the present invention below by detailed description of the invention, following example are the embodiment party that the present invention is concrete Formula, but embodiments of the present invention are not limited by following embodiment.
Embodiment 1:
The preparation of Radix Puerariae granule: take Radix Puerariae decoction pieces, boiling 3 times, add 8 times amount water every time, heating decoction 1.5 is little every time Time;Medicinal liquid merges, and filtrate is concentrated into the clear paste that relative density is 1.08 (80 DEG C), filters with 350 mesh sieves while hot;In inlet temperature 160 DEG C, expecting revolution speed 400 revs/min, leaving air temp 90 DEG C, wind is spray-dried under conditions of sending temperature 45 C, obtains spray drying Powder;Do under the conditions of punched-plate aperture 1.50mm, roller motor frequency 40HZ, feeding electric machine frequency 50HZ, oil cylinder working-pressure 18bar Method is pelletized, and obtains the granularity Radix Puerariae granule at 40 mesh.
Embodiment 2:
Preparation containing the Chinese medicine preparation of Radix Puerariae granule: take Radix Puerariae decoction pieces, boiling 3 times, adds 8 times amount water, every time every time Heating decocts 1.5 hours;Medicinal liquid merges, and filtrate is concentrated into the clear paste that relative density is 1.08 (80 DEG C), while hot with 350 mesh sieve filters Cross;Inlet temperature 160 DEG C, expecting revolution speed 400 revs/min, leaving air temp 90 DEG C, wind is sprayed under conditions of sending temperature 45 C It is dried, obtains spray powder;At punched-plate aperture 1.50mm, roller motor frequency 40HZ, feeding electric machine frequency 50HZ, oil cylinder working-pressure Dry granulation under the conditions of 18bar, obtains the granularity Radix Puerariae granule at 40 mesh;170g Radix Puerariae granule is mixed with 65g maltodextrin, adds Enter appropriate magnesium stearate, mixing, it is pressed into 1000.
Embodiment 3:
A kind of method quickly detecting Radix Puerariae granule moisture level based on near-infrared spectrum technique, specifically includes following step Rapid:
A, take Radix Puerariae particulate samples, totally 88 batches, respectively take about 3g, be ground into fine powder, load in tool plug glass sample bottle, be placed near It is scanned on infrared scanner, gathers spectrum, the condition of scanning: sweep limits 4000-12000cm-1, scanning times: 32 times, Resolution 8cm-1, real-time background correction in scanning process, 3 spectrum of every part of sample collecting, obtain 88 batches of Radix Puerariaes as shown in Figure 1 The near-infrared original absorbance spectrogram of granule;
Meanwhile, according to the standard method of regulation in 2015 editions Chinese Pharmacopoeias, its moisture uses oven drying method to measure, and takes and grinds Finely disintegrated Radix Puerariae granule about 2g, is laid in and is dried to the flat weighing botle of constant weight, accurately weighed, opens bottle cap at 100- 105 DEG C are dried 5 hours, are built by bottle cap, in dislocation exsiccator, cool down 30 minutes, accurately weighed, then are dried 1 at said temperature Hour, cooling, weigh, to the double difference weighed less than 5mg;According to the weight of less loss, calculate Radix Puerariae granule Water content (%), according to sample number and sample distribution determine calibration set and checking collection;
B, be distributed according to sample number and sample moisture measured value, choose 72 batches for calibration set, choose 16 batches of checking collection. Analysis software, Automatic Optimal chooses preprocess method and spectral region, and optimum results is shown in Table 1.Use first derivative+MSC Method carries out pretreatment to near-infrared original absorbance spectrum, chooses 5451.7-4598.3cm-1Spectral information under characteristic wave bands, fortune The quantitative model between near infrared spectrum and moisture measured value is set up with partial least square method (PLS);Sample by checking collection Product carry out near infrared spectrum scanning, utilize model, obtain the predictive value of Radix Puerariae particulate samples content, are entered with measured value by predictive value Row compares, and the accuracy of checking quantitative model and predictive ability, this model obtains cross validation coefficient R through cross validation2= 0.883, RMSECV=0.156, RPD=2.92, dimension is elected 7 as, is verified collection coefficient R2=0.933, RMSEP=0.11, The determination of moisture of 16 batches of Radix Puerariae granules the results are shown in Table 2, and the relevant figure between moisture predictive value and measured value is shown in Fig. 2, moisture Fig. 3 is shown in the comparison bar diagram of predictive value and measured value.
Table 1 water model is in different spectral regions and the model parameter under preprocess method
The determination of moisture result of 2 16 batches of Radix Puerariae granules of table
By upper table 2 it can be seen that the deviation range of Radix Puerariae granule moisture level is between 0.00-0.22%, consensus forecast The response rate is 100.08%, illustrates that this model has preferable predictive ability and stability, can be used for the fast of Radix Puerariae pellet moisture Speed detection.
Embodiment 4:
A kind of method quickly detecting Radix Puerariae granule ethanol soluble extraction content based on near-infrared spectrum technique, specifically include as Lower step:
A, take Radix Puerariae particulate samples, totally 88 batches, respectively take about 3g, be ground into fine powder, load in tool plug glass sample bottle, be placed near It is scanned on infrared scanner, gathers spectrum, the condition of scanning: sweep limits 4000-12000cm-1, scanning times: 32 times, Resolution 8cm-1, real-time background correction in scanning process, 3 spectrum of every part of sample collecting, obtain 88 batches of Radix Puerariaes as shown in Figure 1 The near-infrared original absorbance spectrogram of granule;
Meanwhile, according to the standard method of regulation in 2015 editions Chinese Pharmacopoeias, its ethanol soluble extraction content uses hot dipping to survey Fixed, take the Radix Puerariae granule about 2g grinding to form fine powder, accurately weighed, to put in the conical flask of 100ml, precision adds ethanol 100ml, close Plug, weighed weight, after standing 1 hour, connect reflux condensing tube, be heated to boiling, and keep micro-boiling 1 hour;After letting cool, take off Conical flask, close plug, more weighed weight, supply the weight of less loss, shake up with ethanol, filters with being dried filter, and precision measures filtrate 50ml, puts after being dried to the evaporating dish of constant weight, being evaporated in water-bath, is dried 3 hours in 105 DEG C, put in exsiccator and cool down 30 minutes, the close weighed weight of rapid nationality;Unless otherwise specified, the content of ethanol-soluble extractives in Radix Puerariae granule is calculated with dry product (%), calibration set and checking collection are determined according to sample number and sample distribution;
B, be distributed according to sample number and sample ethanol soluble extraction content measured value, choose 72 batches for calibration set, choose 16 batches For checking collection.Analysis software, Automatic Optimal chooses preprocess method and spectral region, and optimum results is shown in Table 3.Use single order Derivative+MSC method carries out pretreatment to near-infrared original absorbance spectrum, chooses 6100.5-4247.9cm-1Spectrum under characteristic wave bands Information, uses partial least square method (PLS) to set up the quantitative model between near infrared spectrum and ethanol soluble extraction content measured value; The sample of checking collection is carried out near infrared spectrum scanning, utilizes model, obtain the predictive value of Radix Puerariae particulate samples content, will prediction Value compares with measured value, and the accuracy of checking quantitative model and predictive ability, this model obtains cross validation through cross validation Coefficient R2=0.864, RMSECV=1.68, RPD=2.71, dimension is elected 9 as, is verified collection coefficient R2=0.849, RMSEP=1.56, the ethanol soluble extraction assay of 16 batches of Radix Puerariae granules the results are shown in Table 4, ethanol soluble extraction predictive value and actual measurement Relevant figure between value is shown in that Fig. 5 is shown in the comparison bar diagram of Fig. 4, ethanol soluble extraction predictive value and measured value.
Table 3 ethanol soluble extraction model is in different spectral regions and the model parameter under preprocess method
The ethanol soluble extraction assay result of 4 16 batches of Radix Puerariae granules of table
By upper table 4 it can be seen that the deviation range of Radix Puerariae granule ethanol soluble extraction content is between 0.16-3.58%, in advance Surveying average recovery rate is 100.30%, illustrates that this model has preferable predictive ability and stability, can be used for Radix Puerariae granule second The quick detection of alcohol extract.
Embodiment 5:
A kind of quickly detect the method for puerarin content in Radix Puerariae granule based on near-infrared spectrum technique, specifically include as follows Step:
A, take Radix Puerariae particulate samples, totally 88 batches, respectively take about 3g, be ground into fine powder, load in tool plug glass sample bottle, be placed near It is scanned on infrared scanner, gathers spectrum, the condition of scanning: sweep limits 4000-12000cm-1, scanning times: 32 times, Resolution 8cm-1, real-time background correction in scanning process, 3 spectrum of every part of sample collecting, obtain 88 batches of Radix Puerariaes as shown in Figure 1 The near-infrared original absorbance spectrogram of granule;
Meanwhile, according to the standard method of regulation in 2015 editions Chinese Pharmacopoeias, its puerarin content is according to high performance liquid chromatography (four general rules 0512 of " Chinese Pharmacopoeia " version in 2015) measure, and specifically comprise the following steps that
Chromatographic condition and system suitability: with octadecylsilane chemically bonded silica as filler;With methanol-water (25: 75) for flowing phase;Detection wavelength is 250nm.Number of theoretical plate is calculated by puerarin peak should be not less than 2000.
The preparation of reference substance solution: take puerarin reference substance appropriate, accurately weighed, add 30% ethanol and make every 1ml containing 80 μ The solution of g, to obtain final product.
The preparation of need testing solution: take this product under content uniformity item, finely ground, take about 0.1g, accurately weighed, put tool plug cone In shape bottle, accurate addition 30% ethanol 100ml, weighed weight, supersound process (power 300W, frequency 40kHz) 30 minutes, put Cold, more weighed weight, supply the weight of less loss with 30% ethanol, shake up, filter, take subsequent filtrate, to obtain final product.
Algoscopy: precision draws reference substance solution and each 10 μ l of need testing solution respectively, injects chromatograph of liquid, measures, Obtain.
B, be distributed according to sample number and sample puerarin content measured value, choose 72 batches for calibration set, choose 16 batches for testing Card collection.Analysis software, Automatic Optimal chooses preprocess method and spectral region, and optimum results is shown in Table 5.Use first derivative + vector normalization method carries out pretreatment to near-infrared original absorbance spectrum, chooses 6100.5-4598.8cm-1Under characteristic wave bands Spectral information, uses partial least square method (PLS) to set up the quantitative model between near infrared spectrum and puerarin standard content;Will The sample of checking collection carries out near infrared spectrum scanning, utilizes model, obtains the predictive value of Radix Puerariae particulate samples content, by predictive value Comparing with measured value, the accuracy of checking quantitative model and predictive ability, this model obtains cross validation phase through cross validation Close coefficients R2=0.912, RMSECV=3.31, RPD=3.37, dimension is elected 9 as, is verified collection coefficient R2=0.900, RMSEP The puerarin content measurement result of=3.74,16 batches of Radix Puerariae granules is shown in Table 6, the relevant figure between puerarin predictive value and measured value See that Fig. 7 is shown in the comparison bar diagram of Fig. 6, puerarin predictive value and measured value.
Table 5 puerarin model is in different spectral regions and the model parameter under preprocess method
6 16 batches of Radix Puerariae granule puerarin content measurement results of table
By upper table 6 it can be seen that the deviation range of Radix Puerariae granule puerarin is between 0.00-7.21mg/g, it was predicted that average The response rate is 100.55%.Illustrate that this model has preferable predictive ability and stability, can be used for Radix Puerariae granule puerarin Quickly detection.
Embodiment 6:
A kind of method based on near-infrared spectrum technique Fast Evaluation Radix Puerariae granular mass, specifically includes following steps:
A. use software, the Radix Puerariae granule puerarin built, moisture and extractum quantitative model are imported, and sets each group The content limit divided, according to the quality standard of Radix Puerariae granule, sets moisture≤8.0%, ethanol soluble extraction >=26.0%, puerarin >=52mg/g, sets up the multi-method evaluation model of Radix Puerariae granule;
B. gather sample near-infrared absorption spectrum figure, spectrogram is imported in multi-method evaluation model, read each group of sample The content divided and evaluation information.
For verifying predictive ability and the accuracy of this model, the present invention uses mono blind method to test, to Radix Puerariae, Radix Salviae Miltiorrhizae etc. 10 batches Particulate samples is evaluated, and sample message table is shown in Table 7.Gather the spectrogram of numbering 1~10 sample respectively, spectrogram is imported Pueraria lobota In root granule multi-method evaluation model, read content and the evaluation information of each component of sample, the results are shown in Table 8.
Table 7 multi-method evaluation model verification sample information table
Table 8 Radix Puerariae granule multi-method evaluation result
-representing surveyed sample passes, * represents institute's test sample product abnormal (different samples or content are undesirable)
As can be seen from Table 8, this multi-method evaluation model can according to sample spectra information, analyze draw mahalanobis distance, Whether density of fraction, by the size of its value, can be Radix Puerariae granule with principium identification institute test sample product, be identified as Radix Puerariae granule Sample can draw the accurate predictor of each component simultaneously.Illustrate that this model has preferable predictive ability and accuracy, can be quick Evaluate the quality of Radix Puerariae granule.

Claims (10)

1. a Radix Puerariae granule, it is characterised in that prepared by the method comprised the steps: take Radix Puerariae decoction pieces, boiling 2-3 time, adding 5-10 times amount water, heating decocts 1-2 hour every time;Medicinal liquid merges, and it is 1.02-1.10 that filtrate is concentrated into relative density Clear paste, while hot with 250-350 mesh sieve filter;Qinghuo reagent is spray-dried, and obtains spray powder;By spray powder dry granulation, Granularity is at the Radix Puerariae granule of 16-40 mesh.
2. Radix Puerariae granule as claimed in claim 1, it is characterised in that prepared by the method comprised the steps: take Radix Puerariae Decoction pieces, boiling 3 times, add 8 times amount water every time, heating decocts 1.5 hours every time;Medicinal liquid merges, and filtrate is concentrated into the closeest Degree is the clear paste of 1.08, filters with 350 mesh sieves while hot;In inlet temperature 150-190 DEG C, expect revolution speed 400-700 rev/min, go out Air temperature 80-95 DEG C, wind is spray-dried under conditions of sending temperature 35-45 DEG C, obtains spray powder;In punched-plate aperture 1.50mm, dry method system under the conditions of roller motor frequency 40-50HZ, feeding electric machine frequency 30-50HZ, oil cylinder working-pressure 16-24bar Grain, obtains the granularity Radix Puerariae granule at 16-40 mesh.
3. Radix Puerariae granule as claimed in claim 1 or 2, it is characterised in that moisture≤8.0% in Radix Puerariae granule, ethanol leaches Thing >=26.0%, puerarin >=52mg/g.
4. a Chinese medicine preparation, it is characterised in that comprise the Radix Puerariae granule as described in one of claim 1-3 and pharmaceutically can connect The adjuvant being subject to.
5. the detection method of the Radix Puerariae granule as described in one of claim 1-3, it is characterised in that based near infrared spectrum Technology quickly detects, and comprises the steps:
A. the collection of near infrared spectrum: take Radix Puerariae particulate samples about 3g, be ground into fine powder, carries out near infrared spectrum scanning, gathers light Spectrum, obtains the original absorbance spectrogram of Radix Puerariae particulate samples, and is measured each constituent content, measure Radix Puerariae particulate samples each The measured value of constituent content, determines calibration set and checking collection according to the distribution of sample number and sample each constituent content measured value;
B. the foundation of Radix Puerariae particle quantitative model: measure the content of Radix Puerariae pellet moisture, uses first derivative+MSC method to original Absorption spectrum carries out pretreatment, and the spectral region of modeling chooses 5451.7-4598.8cm-1Characteristic wave bands, dimension elects 7 as;Measure Radix Puerariae granule ethanol soluble extraction content, uses first derivative+MSC method that original absorbance spectrum is carried out pretreatment, the spectrum of modeling Scope is chosen for 6100.5-4247.9cm-1Characteristic wave bands, dimension elects 9 as;Measure Radix Puerariae granule puerarin content, use single order Derivative+vector normalization method carries out pretreatment to original absorbance spectrum, and the spectral region of modeling is chosen for 6100.5- 4598.8cm-1Characteristic wave bands, dimension elects 9 as;Use partial least square method to the near infrared spectrum of calibration set and its corresponding Radix Puerariae Quantitative model is set up between the measured value of each constituent content of particulate samples;
C. checking near-infrared quantitative model: gather the near infrared light spectrogram of checking collection sample, each component set up by step b Quantitative model, it is thus achieved that the predictive value of each constituent content of Radix Puerariae particulate samples, compares predictive value with measured value, and checking is quantitatively The accuracy of model;
D. the mensuration of each constituent content of Radix Puerariae granule: take Radix Puerariae granule to be detected and carry out near infrared light according to the method for step a Spectrum gathers, and in the quantitative model set up specific band spectral information steps for importing b, measures the content of each component of Radix Puerariae granule; By whole by near-infrared analysis software for the near-infrared quantitative determination model of the Radix Puerariae pellet moisture, extractum and the puerarin that are built up Close, set up the multi-method evaluation model of Radix Puerariae granule, Radix Puerariae particulate samples to be detected is gathered the reddest according to the method for step a External spectrum, imports in Radix Puerariae granule multi-method evaluation model, measures each constituent content of Radix Puerariae granule simultaneously.
6. the detection method of Radix Puerariae granule as claimed in claim 5, it is characterised in that the sample that Radix Puerariae granule near-infrared measures Preparation method is: take same batch Radix Puerariae granule about 3g, is ground into fine powder, crosses 80 mesh sieves, transfers to what near-infrared measured In tool plug vial.
7. the detection method of Radix Puerariae granule as claimed in claim 6, it is characterised in that: carry out turning by grinding fine powder use funnel Move, make it tight by the way of up-down vibration, stopper with bottle closure of rubber.
8. the detection method of Radix Puerariae granule as claimed in claim 6, it is characterised in that: in temperature 18-22 DEG C, humidity 40- Under the conditions of 50%, granule is ground and quickly bottles.
9. the detection method of Radix Puerariae granule as claimed in claim 6, it is characterised in that: observe bottom the sample bottle after dress sample, The sample powder of guarantee test does not bond bottom vial, just sample can be carried out near infrared spectrum scanning.
10. the detection method of Radix Puerariae granule as claimed in claim 5, it is characterised in that: in step a, described NIR spectra is adopted The condition of scanning integrated is: sweep limits is as 4000cm-1-12000cm-1, scanning times is 32 times, and resolution is 8cm-1, scanned Real-time background correction in journey, 3 spectrum of every part of sample collecting.
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