CN106074742A - A kind of Radix Paeoniae Alba granule and Chinese medicine preparation thereof - Google Patents

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

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CN106074742A
CN106074742A CN201610454588.7A CN201610454588A CN106074742A CN 106074742 A CN106074742 A CN 106074742A CN 201610454588 A CN201610454588 A CN 201610454588A CN 106074742 A CN106074742 A CN 106074742A
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radix paeoniae
paeoniae alba
granule
sample
spectrum
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CN106074742B (en
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朱德全
刘丽萍
王闽予
林振东
陈向东
谭登平
程学仁
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Guangdong Yifang Pharmaceutical Co Ltd
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    • A61K36/18Magnoliophyta (angiosperms)
    • A61K36/185Magnoliopsida (dicotyledons)
    • A61K36/65Paeoniaceae (Peony family), e.g. Chinese peony
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    • A61K2236/30Extraction of the material
    • A61K2236/39Complex extraction schemes, e.g. fractionation or repeated extraction steps
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • 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
    • A61K2236/50Methods involving additional extraction steps
    • A61K2236/51Concentration or drying of the extract, e.g. Lyophilisation, freeze-drying or spray-drying

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Abstract

The invention discloses a kind of Radix Paeoniae Alba granule, the method comprised the steps prepare: take radix paeoniae alba decoction pieces, boiling 13 times, add 5 10 times amount water every time, heating decocts 12 hours every time;Medicinal liquid merges, and filtrate is concentrated into the clear paste that relative density is 1.02 1.12, 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 Paeoniae Alba granule at 16 40 mesh.The Radix Paeoniae Alba 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 Paeoniae Alba granule and Chinese medicine preparation thereof
Technical field
The invention belongs to technical field of traditional Chinese medicine preparation, be specifically related to a kind of Radix Paeoniae Alba granule and Chinese medicine preparation thereof.
Background technology
The Radix Paeoniae Alba is the dry root of ranunculaceae plant Radix Paeoniae Paeonia lactiflora Pall., bitter, sour, is slightly cold, return liver, Spleen channel, has nourishing blood for regulating menstruation, astringing YIN to stop sweating, easing the affected liver to relieve pain, effect of suppressing liver-YANG.
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 Paeoniae Alba granule, need several hours with reference to the method for pharmacopeia, operation The most complicated.The main chemical compositions of Radix Paeoniae Alba granule is peoniflorin, 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 production technology normalized in vain Chinese herbaceous peony granule, its preparation technology is simple, steady quality.It addition, for the quality better controling over Radix Paeoniae Alba 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 Paeoniae Alba granule.
The present invention is achieved by the following technical solutions:
On the one hand, the invention provides a kind of Radix Paeoniae Alba granule, the method comprised the steps prepare: take Radix Paeoniae Alba drink Sheet, boiling 1-3 time, add 5-10 times amount water every time, heating decocts 1-2 hour every time;Medicinal liquid merges, and filtrate is concentrated into relatively Density is the clear paste of 1.02-1.12, filters with 250-350 mesh sieve while hot;Qinghuo reagent is spray-dried, and obtains spray powder;Will spray Dry powder dry granulation, obtains the granularity Radix Paeoniae Alba granule at 16-40 mesh.
The inventors discovered that, boiling 1-3 time, add 5-10 times amount water every time, every time heating decocts 1-2 hour, can be by Effective ingredient extracts more completely.And concentrate the filtrate to the clear paste that relative density is 1.02-1.12, use 250-while hot 350 mesh sieves filter, and can quickly be removed by the moisture in clear paste by the method being spray-dried, and prevent because heated time is longer Cause the loss of effective ingredient.
As preferred scheme, Radix Paeoniae Alba granule is prepared by the method comprised the steps: takes radix paeoniae alba decoction pieces, adds decocting Boiling 2 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 Paeoniae Alba granule.
By optimizing process for producing, preferred moisture≤8.0% in the Radix Paeoniae Alba granule of gained, ethanol soluble extraction >= 40.0%, peoniflorin >=35.0mg/g.
The Radix Paeoniae Alba granule of the present invention can further apply in various Chinese medicine preparation, to realize the pharmacologically active of the Radix Paeoniae Alba.Often The Chinese medicine preparation comprising Radix Paeoniae Alba 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 Paeoniae Alba granule of the present invention, and it is quickly to detect based on near-infrared spectrum technique, bag Include following steps:
(1), the collection of near-infrared (NIR) spectrum: take Radix Paeoniae Alba particulate samples about 3g, be ground into fine powder, carry out near infrared spectrum Scanning, gathers spectrum, obtains the original absorbance spectrogram of Radix Paeoniae Alba particulate samples, and be measured each constituent content, measure white The actual value of each constituent content of Chinese herbaceous peony particulate samples, according to sample number and sample each constituent content actual value distribution determine calibration set and Checking collection;
(2), the foundation of Radix Paeoniae Alba particle quantitative model: measure the content of Radix Paeoniae Alba pellet moisture, use min-max normalization Method carries out pretreatment to original absorbance spectrum, and the spectral region of modeling chooses 6100.5-5447.6cm-1Characteristic wave bands, dimension selects It is 6;Measure Radix Paeoniae Alba granule ethanol soluble extraction content, use first derivative and MSC method that original absorbance spectrum is carried out pretreatment, build The spectral region of mould is chosen for 6100.5-5447.6cm-1、4602.9-4247.9cm-1Characteristic wave bands, dimension elects 4 as;Measure white Chinese herbaceous peony granule paeoniflorin content, uses first derivative and vector normalization method that original absorbance spectrum is carried out pretreatment, the light of modeling Spectral limit is chosen for 6100.5-5447.6cm-1Characteristic wave bands, dimension elects 4 as;Use the reddest to calibration set of partial least square method Quantitative model is set up between the actual value of external spectrum and its corresponding each constituent content of Radix Paeoniae Alba particulate samples.
(3), checking near-infrared quantitative model: gather the near infrared light spectrogram of checking collection sample, set up by step (2) Each measured portions model, it is thus achieved that the predictive value of each constituent content of Radix Paeoniae Alba particulate samples, predictive value is compared with actual value, The accuracy of checking quantitative model;
(4), the mensuration of each constituent content of Radix Paeoniae Alba granule: take Radix Paeoniae Alba granule to be detected and carry out near-infrared according to step (1) Spectra collection, in the quantitative model set up specific band spectral information steps for importing (2), measures containing of each component of Radix Paeoniae Alba granule Amount;The near-infrared of the Radix Paeoniae Alba pellet moisture, extractum and the peoniflorin that are built up is quantitative determined model integration, sets up Radix Paeoniae Alba granule Multi-method evaluation model, by Radix Paeoniae Alba particulate samples to be detected according to step (1) gather near infrared spectrum, import Radix Paeoniae Alba granule In multi-method evaluation model, measure each constituent content of Radix Paeoniae Alba granule simultaneously.
By the method for the present invention, the content of moisture, ethanol soluble extraction and peoniflorin in Radix Paeoniae Alba granule can be measured simultaneously, Only need a few minutes just can complete the detection of each component data, substantially reduce the detection time, adapt to modern enterprise quickly, greatly The demand that amount produces.And traditional detection method, use high effective liquid chromatography for measuring paeoniflorin content, moisture analysis to contain Amount, ethanol-soluble extractives algoscopy measure ethanol soluble extraction content, complex operation, not only need multiple instrument and equipment, also need each Individual inspection post cooperates and just can smoothly complete, and data handling procedure is more complicated, time-consuming.It addition, the inventive method is set up A kind of Radix Paeoniae Alba granule near-infrared quantitative determination model, can be suitable for simultaneously 3 production links material each constituent content survey Fixed, including extractum, spray drying powder, granule.
In the assay method of the present invention, the sample preparation methods that Radix Paeoniae Alba granule near-infrared measures is: take same batch white Chinese herbaceous peony granule about 3g, is ground into fine powder, crosses 80 mesh sieves, transfers in tool plug vial.Preferably, fine powder will be ground and use leakage Bucket shifts, and makes it tight, stopper with bottle closure of rubber by the way of up-down vibration.It is highly preferred that in temperature 18-22 DEG C, Under the conditions of humidity 40-50%, granule is ground and quickly bottles.Observe bottom the sample bottle after dress sample, it is ensured that test Sample powder does not bond bottom vial, and powder does not has tomography, gap, just sample to be carried out near infrared spectrum scanning.
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 Paeoniae Alba 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 Paeoniae Alba granule.
In above-mentioned step (1), 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 Paeoniae Alba granule each component near-infrared On the basis of model, establish Radix Paeoniae Alba granule multi-method evaluation model, moisture in sample, second can be drawn by the collection of a spectrum With density of fraction etc., the multicomponent content results such as alcohol extract and peoniflorin, can distinguish that again kind is true according to mahalanobis distance simultaneously Pseudo-.
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
1, the specification preparation technology of Radix Paeoniae Alba granule, and preparation technology is simple, and technological parameter is stable and easy to control, is suitable for white The preparation of Chinese herbaceous peony granule.
2, the present invention combines chemometrics method based on near-infrared spectrum technique, in certain spectral region, establishes Radix Paeoniae Alba granule near-infrared quantitative model, can be used to qualitative identification simultaneously, it is not necessary to sample carries out the pre-treatment of complexity, is ground Become fine powder, be not related to any reagent, environmental protection, safe and nontoxic, it is the trend of Quality Control job development from now on, for detecting the Radix Paeoniae Alba Granule provides one new method fast and accurately.Can promote the use as a kind of practical approach and produce in Chinese medicinal granule enterprise During online quality-monitoring, 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 Paeoniae Alba particulate samples;
Relevant figure between Fig. 2 Radix Paeoniae Alba pellet moisture near-infrared predictive value and actual value;
Fig. 3 Radix Paeoniae Alba pellet moisture near-infrared predictive value and the comparison bar diagram of actual value;
Relevant figure between Fig. 4 Radix Paeoniae Alba granule ethanol soluble extraction near-infrared predictive value and actual value;
Fig. 5 Radix Paeoniae Alba granule ethanol soluble extraction near-infrared predictive value and the comparison bar diagram of actual value;
Relevant figure between Fig. 6 Radix Paeoniae Alba granule peoniflorin near-infrared predictive value and actual value;
Fig. 7 Radix Paeoniae Alba granule peoniflorin near-infrared predictive value and the comparison bar diagram of actual 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 Paeoniae Alba granule: take radix paeoniae alba decoction pieces, boiling 2 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 150-190 DEG C, expecting revolution speed 400-700 rev/min, leaving air temp 80-95 DEG C, wind sprays under conditions of sending temperature 35-45 DEG C Mist is dried, and obtains spray powder;At punched-plate aperture 1.50mm, roller motor frequency 40-50HZ, feeding electric machine frequency 30-50HZ, oil Dry granulation under the conditions of cylinder pressure 16-24bar, obtains the granularity Radix Paeoniae Alba granule at 16-40 mesh.
Embodiment 2:
Preparation containing the Chinese medicine preparation of Radix Paeoniae Alba granule: take radix paeoniae alba decoction pieces, boiling 2 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;In inlet temperature 150-190 DEG C, expecting revolution speed 400-700 rev/min, leaving air temp 80-95 DEG C, wind send temperature 35-45 DEG C Under the conditions of be spray-dried, obtain spray powder;At punched-plate aperture 1.50mm, roller motor frequency 40-50HZ, feeding motor frequency Dry granulation under the conditions of rate 30-50HZ, oil cylinder working-pressure 16-24bar, obtains the granularity Radix Paeoniae Alba granule at 16-40 mesh.By the 100g Radix Paeoniae Alba Granule mixes with 65g maltodextrin, adds appropriate magnesium stearate, mixing, is pressed into 1000.
Embodiment 3:
A kind of method quickly detecting Radix Paeoniae Alba granule moisture level based on near-infrared spectrum technique, specifically includes following step Rapid:
A, take Radix Paeoniae Alba particulate samples, totally 106 batches, respectively take about 3g, be ground into fine powder, load in tool plug glass sample bottle, be placed in It is scanned on infrared diaphanoscopy instrument, gathers spectrum, the condition of scanning: sweep limits 4000-12000cm-1, scanning times: 32 Secondary, resolution 8cm-1, real-time background correction in scanning process, 3 spectrum of every part of sample collecting, obtain 106 batches as shown in Figure 1 The near-infrared original absorbance spectrogram of Radix Paeoniae Alba 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 Paeoniae Alba 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 Paeoniae Alba 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 88 batches for calibration set, choose 18 batches for checking Collection.Analysis software, Automatic Optimal chooses preprocess method and spectral region, and optimum results is shown in Table 1.Use min-max Normalization method carries out pretreatment to near-infrared original absorbance spectrum, chooses 6100.5-5447.6cm-1Spectrum letter under characteristic wave bands Breath, uses partial least square method (PLS) to set up the quantitative model between near infrared spectrum and moisture actual value;Checking is collected Sample carry out near infrared spectrum scanning, utilize model, obtain the predictive value of Radix Paeoniae Alba particulate samples content, by predictive value with true Value compares, and the accuracy of checking quantitative model and predictive ability, this model obtains cross validation correlation coefficient through cross validation R2=0.880, RMSECV=0.143, RPD=2.89, dimension is elected 6 as, is verified collection coefficient R2=0.825, RMSEP= The determination of moisture of 0.099,18 batch of Radix Paeoniae Alba granule the results are shown in Table 2, and the relevant figure between moisture predictive value and actual value is shown in figure 2, Fig. 3 is shown in the comparison bar diagram of moisture predictive value and actual value.
Table 1 water model is in different spectral regions and the model parameter under preprocess method
The determination of moisture result of 2 18 batches of Radix Paeoniae Alba granules of table
By upper table 2 it can be seen that the deviation range of Radix Paeoniae Alba granule moisture level is between 0.00-0.21%, consensus forecast The response rate is 100.87%, illustrates that this model has preferable predictive ability and stability, can be used for the fast of Radix Paeoniae Alba pellet moisture Speed detection.
Embodiment 4:
A kind of method quickly detecting Radix Paeoniae Alba granule ethanol soluble extraction content based on near-infrared spectrum technique, specifically include as Lower step:
A, take Radix Paeoniae Alba particulate samples, totally 106 batches, respectively take about 3g, be ground into fine powder, load in tool plug glass sample bottle, be placed in It is scanned on infrared diaphanoscopy instrument, gathers spectrum, the condition of scanning: sweep limits 4000-12000cm-1, scanning times: 32 Secondary, resolution 8cm-1, real-time background correction in scanning process, 3 spectrum of every part of sample collecting, obtain 106 batches as shown in Figure 1 The near-infrared original absorbance spectrogram of Radix Paeoniae Alba 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 Paeoniae Alba 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 Paeoniae Alba 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 86 batches for calibration set, choose 20 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 6100.5-5447.6cm-1、4602.9- 4247.9cm-1Spectral information under characteristic wave bands, uses partial least square method (PLS) to set up near infrared spectrum and ethanol soluble extraction Quantitative model between content actual value;The sample of checking collection is carried out near infrared spectrum scanning, utilizes model, obtain the Radix Paeoniae Alba The predictive value of grain sample size, compares predictive value with actual value, the accuracy of checking quantitative model and predictive ability, should Model obtains cross validation coefficient R through cross validation2=0.866, RMSECV=2.14, RPD=2.74, dimension is elected 4 as, is tested Card collection coefficient R2The ethanol soluble extraction assay of=0.838, RMSEP=2.32,20 batch Radix Paeoniae Alba granule the results are shown in Table 4, Relevant figure between ethanol soluble extraction predictive value and actual value is shown in the comparison cylindricality of Fig. 4, ethanol soluble extraction predictive value and actual value Figure is shown in Fig. 5
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 20 batches of Radix Paeoniae Alba granules of table
By upper table 4 it can be seen that the deviation range of Radix Paeoniae Alba granule ethanol soluble extraction content is between 0.17-4.26%, in advance Surveying average recovery rate is 98.56%, illustrates that this model has preferable predictive ability and stability, can be used for Radix Paeoniae Alba granule alcohol leaching Go out the quick detection of thing.
Embodiment 5:
A kind of quickly detect the method for paeoniflorin content in Radix Paeoniae Alba granule based on near-infrared spectrum technique, specifically include as follows Step:
A, take Radix Paeoniae Alba particulate samples, totally 106 batches, respectively take about 3g, be ground into fine powder, load in tool plug glass sample bottle, be placed in It is scanned on infrared diaphanoscopy instrument, gathers spectrum, the condition of scanning: sweep limits 4000-12000cm-1, scanning times: 32 Secondary, resolution 8cm-1, real-time background correction in scanning process, 3 spectrum of every part of sample collecting, obtain 106 batches as shown in Figure 1 The near-infrared original absorbance spectrogram of Radix Paeoniae Alba granule;
Meanwhile, according to the standard method of regulation in 2015 editions Chinese Pharmacopoeias, its paeoniflorin 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 are with octadecylsilane chemically bonded silica as filler;With acetonitrile-0.1% phosphorus Acid solution (14: 86) is flowing phase;Detection wavelength is 230nm.Number of theoretical plate is calculated by peoniflorin peak should be not less than 3000.
It is appropriate that the preparation of reference substance solution takes peoniflorin reference substance, accurately weighed, adds methanol and makes molten containing 50 μ g of every 1ml Liquid, to obtain final product.
The preparation of need testing solution takes this product under content uniformity item, finely ground, takes about 0.1g, accurately weighed, accurate addition Diluted Alcohol 50ml, weighed weight, supersound process (power 300W, frequency 40kHz) 30 minutes, let cool, more weighed weight, use dilute second The weight of less loss supplied by alcohol, shakes up, and filters, and precision measures subsequent filtrate 3ml, puts in 10ml measuring bottle, adds Diluted Alcohol to scale, shakes Even, to obtain final product.
Algoscopy precision respectively draws reference substance solution and need testing solution each 5-10 μ l, injects chromatograph of liquid, measures, Obtain.
B, be distributed according to sample number and sample paeoniflorin content measured value, choose 86 batches for calibration set, choose 20 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 6100.5-5447.6cm-1Under characteristic wave bands Spectral information, uses partial least square method (PLS) to set up the quantitative model between near infrared spectrum and peoniflorin standard content;Will The sample of checking collection carries out near infrared spectrum scanning, utilizes model, obtains the predictive value of Radix Paeoniae Alba particulate samples content, by predictive value Comparing with actual value, the accuracy of checking quantitative model and predictive ability, this model obtains cross validation phase through cross validation Close coefficients R2=0.849, RMSECV=4.22, RPD=2.57, dimension is elected 4 as, is verified collection coefficient R2=0.838, RMSEP The paeoniflorin content measurement result of=4.17,20 batches of Radix Paeoniae Alba granules is shown in Table 6, the relevant figure between peoniflorin predictive value and actual value See that Fig. 7 is shown in the comparison bar diagram of Fig. 6, peoniflorin predictive value and actual value.
Table 5 peoniflorin model is in different spectral regions and the model parameter under preprocess method
6 20 batches of Radix Paeoniae Alba granule paeoniflorin content measurement results of table
By upper table 6 it can be seen that the deviation range of Radix Paeoniae Alba granule peoniflorin is between 0.16-8.92mg/g, it was predicted that average The response rate is 101.8%.Illustrate that this model has preferable predictive ability and stability, can be used for the fast of Radix Paeoniae Alba granule peoniflorin Speed detection.
Embodiment 6:
A kind of method based on near-infrared spectrum technique Fast Evaluation Radix Paeoniae Alba granular mass, specifically includes following steps:
A. use software, the Radix Paeoniae Alba granule peoniflorin built, moisture and extractum quantitative model are imported, and sets each group The content limit divided, according to the quality standard of Radix Paeoniae Alba granule, sets moisture≤8.0%, ethanol soluble extraction >=40.0%, peoniflorin >=35.0mg/g, sets up the multi-method evaluation model of Radix Paeoniae Alba 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 the Radix Paeoniae Alba, 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 white In Chinese herbaceous peony 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 Paeoniae Alba 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 Paeoniae Alba granule with principium identification institute test sample product, be identified as Radix Paeoniae Alba 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 Paeoniae Alba granule.

Claims (10)

1. a Radix Paeoniae Alba granule, it is characterised in that prepared by the method comprised the steps: take radix paeoniae alba decoction pieces, boiling 1-3 time, adding 5-10 times amount water, heating decocts 1-2 hour every time every time;Medicinal liquid merges, and it is 1.02-that filtrate is concentrated into relative density The clear paste of 1.12, filters with 250-350 mesh sieve while hot;Qinghuo reagent is spray-dried, and obtains spray powder;By spray powder dry method system Grain, obtains the granularity Radix Paeoniae Alba granule at 16-40 mesh.
2. Radix Paeoniae Alba granule as claimed in claim 1, it is characterised in that prepared by the method comprised the steps: take the Radix Paeoniae Alba Decoction pieces, boiling 2 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 Paeoniae Alba granule at 16-40 mesh.
3. Radix Paeoniae Alba granule as claimed in claim 1 or 2, it is characterised in that moisture≤8.0% in Radix Paeoniae Alba granule, ethanol leaches Thing >=40.0%, peoniflorin >=35.0mg/g.
4. a Chinese medicine preparation, it is characterised in that comprise the Radix Paeoniae Alba granule as described in one of claim 1-3 and maltodextrin.
5. the detection method of the Radix Paeoniae Alba 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:
(1), the collection of near infrared spectrum: take Radix Paeoniae Alba particulate samples about 3g, be ground into fine powder, carry out near infrared spectrum scanning, gather Spectrum, obtains the original absorbance spectrogram of Radix Paeoniae Alba particulate samples, and is measured each constituent content, measure Radix Paeoniae Alba particulate samples The actual value of each constituent content, determines calibration set and checking collection according to the distribution of sample number and sample each constituent content actual value;
(2), the foundation of Radix Paeoniae Alba particle quantitative model: measure the content of Radix Paeoniae Alba pellet moisture, use min-max normalization method pair Original absorbance spectrum carries out pretreatment, and the spectral region of modeling chooses 6100.5-5447.6cm-1Characteristic wave bands, dimension elects 6 as; Measure Radix Paeoniae Alba granule ethanol soluble extraction content, use first derivative and MSC method that original absorbance spectrum is carried out pretreatment, modeling Spectral region is chosen for 6100.5-5447.6cm-1、4602.9-4247.9cm-1Characteristic wave bands, dimension elects 4 as;Measure the Radix Paeoniae Alba Grain paeoniflorin content, uses first derivative and vector normalization method that original absorbance spectrum is carried out pretreatment, the spectrum model of modeling Enclose and be chosen for 6100.5-5447.6cm-1Characteristic wave bands, dimension elects 4 as;Use the partial least square method near infrared light to calibration set Quantitative model is set up between the actual value of spectrum and its corresponding each constituent content of Radix Paeoniae Alba particulate samples;
(3), checking near-infrared quantitative model: gather checking collection sample near infrared light spectrogram, by step (2) set up each Measured portions model, it is thus achieved that the predictive value of each constituent content of Radix Paeoniae Alba particulate samples, compares predictive value with actual value, checking The accuracy of quantitative model;
(4), the mensuration of each constituent content of Radix Paeoniae Alba granule: take Radix Paeoniae Alba granule to be detected and carry out near infrared spectrum according to step (1) Gather, in the quantitative model set up specific band spectral information steps for importing (2), measure the content of each component of Radix Paeoniae Alba granule; The near-infrared of the Radix Paeoniae Alba pellet moisture, extractum and the peoniflorin that are built up is quantitative determined model integration, sets up Radix Paeoniae Alba granule Multi-method evaluation model, gathers near infrared spectrum by Radix Paeoniae Alba particulate samples to be detected according to step (1), imports Radix Paeoniae Alba granule many In method evaluation model, measure each constituent content of Radix Paeoniae Alba granule simultaneously.
6. the detection method of Radix Paeoniae Alba granule as claimed in claim 5, it is characterised in that the sample that Radix Paeoniae Alba granule near-infrared measures Preparation method is: take same batch Radix Paeoniae Alba granule about 3g, is ground into fine powder, crosses 80 mesh sieves, transfers in tool plug vial.
7. the detection method of Radix Paeoniae Alba 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 Paeoniae Alba granule as claimed in claim 6, it is characterised in that in temperature 18-22 DEG C, humidity 40-50% Under the conditions of, granule is ground and quickly bottles.
9. the detection method of Radix Paeoniae Alba granule as claimed in claim 6, it is characterised in that observe bottom the sample bottle after dress sample, protect The sample powder of card test does not bond bottom vial, and powder does not has tomography, gap, just sample to be carried out near infrared spectrum Scanning.
10. the detection method of Radix Paeoniae Alba granule as claimed in claim 5, it is characterised in that in step (1), described NIR spectra The condition of scanning gathered is: sweep limits is 4000cm-1-12000cm-1, scanning times is 32 times, and resolution is 8cm-1, scanning During in real time background correction, 3 spectrum of every part of sample collecting.
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CN106770001A (en) * 2016-11-11 2017-05-31 本溪国家中成药工程技术研究中心有限公司 Method and application using extract solution concentration process in the preparation process of near infrared spectroscopy quick detection qizhi weitong granules
CN113995784A (en) * 2021-11-04 2022-02-01 陕西孙思邈高新制药有限公司 Preparation process of white peony root formula granules
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CN106770001A (en) * 2016-11-11 2017-05-31 本溪国家中成药工程技术研究中心有限公司 Method and application using extract solution concentration process in the preparation process of near infrared spectroscopy quick detection qizhi weitong granules
CN113995784A (en) * 2021-11-04 2022-02-01 陕西孙思邈高新制药有限公司 Preparation process of white peony root formula granules
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