CN106770001A - Method and application using extract solution concentration process in the preparation process of near infrared spectroscopy quick detection qizhi weitong granules - Google Patents
Method and application using extract solution concentration process in the preparation process of near infrared spectroscopy quick detection qizhi weitong granules Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 49
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- YKRGDOXKVOZESV-WRJNSLSBSA-N Paeoniflorin Chemical compound C([C@]12[C@H]3O[C@]4(O)C[C@](O3)([C@]1(C[C@@H]42)O[C@H]1[C@@H]([C@@H](O)[C@H](O)[C@@H](CO)O1)O)C)OC(=O)C1=CC=CC=C1 YKRGDOXKVOZESV-WRJNSLSBSA-N 0.000 claims description 57
- YKRGDOXKVOZESV-UHFFFAOYSA-N paeoniflorin Natural products O1C(C)(C2(CC34)OC5C(C(O)C(O)C(CO)O5)O)CC3(O)OC1C24COC(=O)C1=CC=CC=C1 YKRGDOXKVOZESV-UHFFFAOYSA-N 0.000 claims description 55
- 238000002329 infrared spectrum Methods 0.000 claims description 36
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Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N21/359—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light using near infrared light
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- 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
- G01N21/3577—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing liquids, e.g. polluted water
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N9/00—Investigating density or specific gravity of materials; Analysing materials by determining density or specific gravity
- G01N9/24—Investigating density or specific gravity of materials; Analysing materials by determining density or specific gravity by observing the transmission of wave or particle radiation through the material
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- Physics & Mathematics (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analysing Materials By Optical Means (AREA)
Abstract
The present invention relates to the use of method and the application of extract solution concentration process in the preparation process of near infrared spectroscopy quick detection qizhi weitong granules.The present invention establishes the on-line near infrared spectroscopy analysis method of the extract solution concentration process in the preparation process of qizhi weitong granules, and it is applied to on-line checking, realize the Aulomatizeted Detect of extract solution concentration process in the preparation process of qizhi weitong granules and the real-time estimate of each quality control index content；The model prediction accuracy set up is high, and the degree of accuracy is high, meets the requirement of quantitative analysis in actual production；The method is compared with traditional official method, on the basis of the degree of accuracy is ensured, analysis efficiency is substantially increased, quality that can be fast and efficiently to extract solution concentration process carries out real-time monitoring and control, so as to advantageously ensure that security, stability and the validity of end product quality.
Description
Technical field
The invention belongs to drug tests, and in particular to using near infrared spectroscopy quick detection qizhi weitong granules
The method of extract solution concentration process and application in preparation process.
Background technology
Qizhi weitong granules is made up of radix bupleuri, corydalis tuber, Fructus Aurantii, rhizoma cyperi, the root of herbaceous peony and the taste Chinese medicine of honey-fried licorice root 6, with easypro liver
Qi-regulating and the effect of stomach and alleviating pain, for the treatment of the diseases such as stagnation of QI due to depression of the liver, feeling of stuffiness in chest turgor, gastral cavity pain, by clinical for many years real
Trample, as the fiest-tire medication of clinical treatment epigastric pain.But, the preparation process of qizhi weitong granules is complicated and cumbersome, real
The minor variations of various technological parameters are likely to directly affect the quality of final medicine in the production process of border.
Traditional Pharmaceutical Analysis technology typically uses offline analysis means, and liquid is gathered from extractor and concentration tank,
It is analyzed by high performance liquid chromatography, gas-chromatography etc. in the lab, the result after analysis is then fed back into production car
Between carry out production regulation and control.However, traditional analysis mode is due to inefficiency, production efficiency is not only leveraged, and be difficult
Reflect chemical change and the physical change of complexity in extraction process and concentration process.In propulsion modernization of industry of Chinese materia medica development
In process, with the continuous improvement of China's drug production process automaticity, in order to ensure the homogeneity of tcm product quality
And stability, the fast mass analysis method and online measuring technique of Study of Traditional Chinese Medicine pharmacy procedure, produced for improving China's Chinese medicine
Industry modernization level is significant.
Near infrared spectrum (NearInfraredSpectrumInstrument, NIRS) is for developing rapidly in recent years
Effectively easy analysis method is planted, is combined by with optical fiber and computer technology, NIR measurement signals can carry out long distance
From transmission and analysis.Near infrared light is a kind of electromagnetic wave, between visible ray (Vis) and in electromagnetic radiation between infrared (MIR)
Ripple, in 780-2526nm, near-infrared spectrum analysis have that free from environmental pollution, sampling without damage, analyze speed be fast, operation letter to wavelength
List, real-time online, overall merit, the degree of accuracy are high, analysis object extensively, without consumables associated therewith and the features such as maintenance cost.It is near red
External spectrum area is consistent with sum of fundamental frequencies and the uptake zone of frequency multiplication at different levels that hydric group in organic molecule (O-H, N-H, C-H) vibrates, leads to
The near infrared spectrum of sample is over-scanned, the characteristic information of organic molecule hydric group in sample can be obtained, using near infrared light
The maximum feature of spectral technology analysis sample is quick, lossless, in situ online etc., therefore, the technology is increasingly subject to researcher
Favor.At present, near-infrared spectrum technique obtains relatively successfully application in fields such as medicine, oil, food industry.
Therefore, extract solution concentration in a kind of preparation process that can rapidly, comprehensively detect qizhi weitong granules is set up
The method of process, the production in enormous quantities and overall quality control to qizhi weitong granules is significant.
The content of the invention
Therefore, the present invention is carried in providing a kind of preparation process of utilization near infrared spectroscopy quick detection qizhi weitong granules
Take method and the application of liquid concentration process.
In order to solve the above technical problems, the present invention is achieved through the following technical solutions：
The present invention provides extract solution in a kind of preparation process of utilization near infrared spectroscopy quick detection qizhi weitong granules
The method of concentration process,
The step of assay, relative density and/or determination of solid content including following Paeoniflorin:
A, the assay of Paeoniflorin are comprised the following steps：
(1) concentrated extracting solution of the qizhi weitong granules of known paeoniflorin content is taken, it is standby；
(2) concentrated extracting solution of the qizhi weitong granules is carried out near infrared spectrum scanning, gathers the energy-stagnation stomachache
The near infrared spectrum of the concentrated extracting solution of particle；
(3) 5449.8~6101.7cm is chosen-1With 5149.01~5442.13cm-1Spectral information under characteristic wave bands, should
Entered with the paeoniflorin content of the concentrated extracting solution of the qizhi weitong granules of the known paeoniflorin content with chemo metric software
Row association, the quantitative calibration model set up between near infrared spectrum and standard content using PLS；
(4) near-infrared is carried out to the concentrated extracting solution sample of unknown qizhi weitong granules according to the method for the step (2)
Spectral scan, and choose 5449.8~6101.7cm-1With 5149.01~5442.13cm-1Spectral information under characteristic wave bands, leads
Enter the paeoniflorin content value of the concentrated extracting solution sample of the quantitative calibration model acquisition unknown qizhi weitong granules of foundation；
B, relative density determination are comprised the following steps：
(1) concentrated extracting solution of the qizhi weitong granules of known relative density is taken, it is standby；
(2) concentrated extracting solution of the qizhi weitong granules is carried out near infrared spectrum scanning, gathers the energy-stagnation stomachache
The near infrared spectrum of the concentrated extracting solution of particle；
(3) 5469.13~7143.04cm is chosen-1With 5149.01~5442.13cm-1Spectral information under characteristic wave bands,
Applied Chemometrics software is carried out with the relative density of the concentrated extracting solution of the qizhi weitong granules of the known relative density
Association, the quantitative calibration model set up between near infrared spectrum and standard content using PLS；
(4) near-infrared is carried out to the concentrated extracting solution sample of unknown qizhi weitong granules according to the method for the step (2)
Spectral scan, and choose 5469.13~7143.04cm-1With 5149.01~5442.13cm-1Spectral information under characteristic wave bands,
Import the relative density values that the quantitative calibration model set up obtains the concentrated extracting solution sample of the unknown qizhi weitong granules；
C, determination of solid content are comprised the following steps：
(1) concentrated extracting solution of the qizhi weitong granules of known solid content is taken, it is standby；
(2) concentrated extracting solution of the qizhi weitong granules is carried out near infrared spectrum scanning, gathers the energy-stagnation stomachache
The near infrared spectrum of the concentrated extracting solution of particle；
(3) 5469.13~7143.04cm is chosen-1Spectral information under characteristic wave bands, Applied Chemometrics software and institute
The solid content for stating the concentrated extracting solution of the qizhi weitong granules of known solid content is associated, and sets up near using PLS
Quantitative calibration model between infrared spectrum and standard content；
(4) near-infrared is carried out to the concentrated extracting solution sample of unknown qizhi weitong granules according to the method for the step (2)
Spectral scan, and choose 5469.13~7143.04cm-1Spectral information under characteristic wave bands, imports the quantitative calibration model set up
Obtain the solid content value of the concentrated extracting solution sample of the unknown qizhi weitong granules.
Preferably, extracted in the preparation process of above-mentioned utilization near infrared spectroscopy quick detection qizhi weitong granules of the invention
The method of liquid concentration process,
In the step of the step of assay of the Paeoniflorin (2) neutralizes determination of solid content (2), adopted using static spectrum
Collection method carries out the near infrared spectra collection of the concentrated extracting solution of the qizhi weitong granules, and actual conditions is：Spectral acquisition times
At intervals of 10min, with air as reference, scanning times are 32 times, and resolution ratio is 8cm-1, scanning optical spectrum scope be 4000~
10000cm-1。
It is further preferred that the preparation process of above-mentioned utilization near infrared spectroscopy quick detection qizhi weitong granules of the invention
The method of middle extract solution concentration process,
In the step of assay of the Paeoniflorin (2), also including using two to the near infrared spectrum for collecting
The step of order derivative method and Norris derivative smoothing filter methods are pre-processed；
In the step of relative density (2) and/or the step of determination of solid content in (2), also including the institute to collecting
The step of stating near infrared spectrum and pre-processed using First derivative spectrograply and Norris derivative smoothing filter methods.
It is further preferred that the preparation process of above-mentioned utilization near infrared spectroscopy quick detection qizhi weitong granules of the invention
The method of middle extract solution concentration process,
The bulk drug of the qizhi weitong granules is constituted：
The weight portion of radix bupleuri 30~100, the weight portion of Radix Glycyrrhizae 15~60, the weight portion of rhizoma cyperi 35~120, the weight of corydalis tuber 35~120
Amount part, the weight portion of the root of herbaceous peony 40~150, the weight portion of Fructus Aurantii 35~120.
It is further preferred that the preparation process of above-mentioned utilization near infrared spectroscopy quick detection qizhi weitong granules of the invention
The method of middle extract solution concentration process,
The preparation method of the qizhi weitong granules is comprised the following steps：
(3) Fructus Aurantii and rhizoma cyperi of selected weight portion are taken, volatile oil is extracted, liquid is standby, and the dregs of a decoction are discarded；
(4) radix bupleuri, Radix Glycyrrhizae, corydalis tuber and the root of herbaceous peony of selected weight portion are taken, is added water to cook 2 times, the 1st decoction 0.5~4 is small
When, the 2nd decoction 0.5~3 hour；
(3) decocting liquid of combining step (1) and step (2), filtering, filtrate be concentrated into relative density be 1.10~1.30 it is clear
Cream；
(4) qinghuo reagent, plus auxiliary material, mixing are made particle, dry, and spray into volatile oil, obtain final product granule.
The bulk drug composition and preparation method of qizhi weitong granules of the present invention are with reference to Chinese patent literature CN1712048A.
It is further preferred that the preparation process of above-mentioned utilization near infrared spectroscopy quick detection qizhi weitong granules of the invention
The method of middle extract solution concentration process,
In the step of assay of the Paeoniflorin (3), relative density determination the step of (3) neutralize determination of solid content
In step (3), also including evaluating the estimated performance of the quantitative calibration model set up the step of, the evaluation index
Including coefficient R, calibration set mean square deviation RMSEC, checking collection root mean square RMSEP, cross validation root mean square RMSECV and prediction
Relative deviation RSEP, when R values closer to 1, RMSEC and RMSEP values it is smaller and closer to when, evaluation model stability is better,
Prediction precision is higher, then disclosure satisfy that the precision of prediction requirement of qizhi weitong granules Direct Analysis；Conversely, not applying to then.
It is further preferred that the preparation process of above-mentioned utilization near infrared spectroscopy quick detection qizhi weitong granules of the invention
The method of middle extract solution concentration process,
In the step of assay of the Paeoniflorin (1), using known Paeoniflorin described in high effective liquid chromatography for measuring
The paeoniflorin content of content qizhi weitong granules is used as standard content；
In the step of determination of solid content (3), the known solid content qizhi weitong granules is determined using oven drying method
Solid content is used as standard content.
It is further preferred that the preparation process of above-mentioned utilization near infrared spectroscopy quick detection qizhi weitong granules of the invention
The method of middle extract solution concentration process,
The paeoniflorin content of known paeoniflorin content qizhi weitong granules described in the use high effective liquid chromatography for measuring
Concretely comprise the following steps：
(1) 4~6mL of concentrated extracting solution of the qizhi weitong granules is taken, in rotating speed 12000-14000r/min bars
8~12min is centrifuged under part, supernatant is taken, as need testing solution；
(2) precision weighs 1-3mg Paeoniflorin reference substances and is placed in 20mL measuring bottles, plus methyl alcohol be made every mL containing 0.05~
The solution of 0.15mg, shakes up, used as reference substance solution；
(3) chromatographic condition：It is chromatographic column with 4.6 × 250mm, 5 μm of Agilent Zorbax SB-C18, with 0.1% phosphorus
Aqueous acid is mobile phase A, carries out gradient elution according to following program by Mobile phase B of acetonitrile：0-13min, A：B is 85%：
15%；13-15min, A：B is 85%：15% → 10%：90%；15-19min, A：B is 10%：90%；19-25min, A：B
It is 10%：90% → 0%：100%；25-30min, A：B is 0%：100% → 85%：15%；Flow velocity 1.0mL/min, column temperature
30 DEG C, Detection wavelength 230nm；
(4) it is accurate to draw the need testing solution and each 5 μ L of reference substance solution, liquid chromatograph is injected, determine；
The use oven drying method determines concretely comprising the following steps for the solid content of the known solid content qizhi weitong granules：
The measuring cup of the concentrated extracting solution as drying to constant weight of qizhi weitong granules described in 4~6mL is taken, in 105 DEG C of bakings
Dry 5~7h, moves to 20~40min of cooling in drier, weighs；Dried 0.5~1.5 hour at 105 DEG C, cooling is weighed；
To double difference of weighing no more than 5mg, solid content is calculated.
Extracted in the preparation process that above-mentioned utilization near infrared spectroscopy quick detection qizhi weitong granules is also provided of the invention
Purposes of the method for liquid concentration process in qizhi weitong granules quality testing and control.
Above-mentioned technical proposal of the invention has advantages below compared to existing technology：
(1) method of the preparation process of utilization near infrared spectroscopy quick detection qizhi weitong granules of the present invention, will
Near infrared spectroscopy is applied in the quality quick detection of extract solution concentration process in the preparation process of qizhi weitong granules, for
Extract solution concentration process determines quality control index, can be quick to the extract solution concentration process in the preparation process of qizhi weitong granules
Determine, realize in the preparation process to qizhi weitong granules extract solution concentration process quickly, comprehensively detection, and have
The advantages of simple to operate, accuracy is high, accuracy is high, can quickly judge extract solution concentration in the preparation process of qizhi weitong granules
Whether process is qualified, shortens detection time, saves production cost, improve production efficiency and economic benefit, it is ensured that energy-stagnation stomachache
Granular mass is safely, effectively；
(2) extract solution is dense in the preparation process of utilization near infrared spectroscopy quick detection qizhi weitong granules of the present invention
The method of compression process, by the near of each quality control index in extract solution concentration process in the preparation process for selecting qizhi weitong granules
Spectral band in infrared spectrum, extracts effective characteristic spectrum wave band, this feature spectral band with according to existing conventional method
Each quality control index for determining has good correlation, can in effective monitoring qizhi weitong granules preparation process extract solution it is concentrated
Whether journey is qualified；
(3) extract solution is dense in the preparation process of utilization near infrared spectroscopy quick detection qizhi weitong granules of the present invention
The method of compression process, for extract solution concentration process in each quality control index be separately optimized the pretreatment of near-infrared original spectrum
Method, with filter information, reduces noise, improves the accuracy of the preparation process of the method detection qizhi weitong granules and accurate
Degree；
(4) near infrared spectrum of extract solution concentration process is online in the preparation process for establishing qizhi weitong granules of the invention
Analysis method, and be applied to on-line checking, realize in the preparation process of qizhi weitong granules extract solution concentration process from
Dynamicization detects the real-time estimate with each quality control index content；The model prediction accuracy set up is high, and the degree of accuracy is high, meets actual raw
The requirement of quantitative analysis in product；The method on the basis of the degree of accuracy is ensured, is substantially increased point compared with traditional official method
Analysis efficiency, quality that can be fast and efficiently to extract solution concentration process carries out real-time monitoring and control, so as to advantageously ensure that
The security of end product quality, stability and validity.
Brief description of the drawings
In order that present disclosure is more likely to be clearly understood, below according to specific embodiment of the invention and combine
Accompanying drawing, the present invention is further detailed explanation, wherein：
Fig. 1 be the qizhi weitong granules in embodiment 1 preparation process in extract solution concentration process original near infrared light
Spectrum；
Fig. 2 is the Paeoniflorin reference substance chromatogram in embodiment 1；
Fig. 3 is the Paeoniflorin sample chromatogram figure in embodiment 1；
Fig. 4 is that the near-infrared predicted value of the Paeoniflorin calibration set sample in embodiment 1 is related to efficient liquid phase measured value
Graph of a relation；
Fig. 5 is the dependency relation figure of the near-infrared predicted value with measured value of the relative density calibration set sample in embodiment 1；
Fig. 6 is the dependency relation figure of the near-infrared predicted value with measured value of the solid content calibration set sample in embodiment 1；
Fig. 7 is that the near-infrared predicted value of the Paeoniflorin checking collection sample in embodiment 1 is related to efficient liquid phase measured value
Graph of a relation；
Fig. 8 is the dependency relation figure of the near-infrared predicted value with measured value of the relative density checking collection sample in embodiment 1；
Fig. 9 is the dependency relation figure of the near-infrared predicted value with measured value of the solid content checking collection sample in embodiment 1；
Figure 10 is extract solution concentration process liquid chromatogram measuring and model prediction Paeoniflorin in the preparation process in embodiment 1
Change in concentration compares figure；
Figure 11 is that the extract solution concentration process relative density determination in embodiment 1 becomes with the concentration of model prediction relative density
Change compares figure；
Figure 12 is extract solution concentration process determination of solid content and model prediction solid content in the preparation process in embodiment 1
Change in concentration compares figure.
Specific embodiment
Embodiment 1Near-infrared spectrum technique is used for the research of extract solution concentration process in the preparation process of qizhi weitong granules
1st, experiment material
1.1 medicinal materials and reagent
Qizhi weitong granules concentrate (Liaoning Huarun Benxi Third Pharmaceutical Co., Ltd.'s offer)；(Chengdu is graceful for Paeoniflorin reference substance
Si Te bio tech ltd, lot number：MUST-11030608)；Acetonitrile (Merck, Germany)；Phosphoric acid (Aladdin)；
Heartily pure water.
1.2 key instruments and equipment
Agilent1200 high performance liquid chromatographs (Agilent1200 pumps, Agilent1200 photo-diode array detections
Device, Agilent1200 chromatographic work stations, Agilent Technologies of the U.S.)；Antaris ft-nir spectrometers
(Thermo Nicolet, USA)；Equipped with corresponding transmission detector annex sampling system and signal acquisition and Result,
The data processing softwares such as TQAnalyst；Sartorius CP225D electronic analytical balances (Beijing limited public affairs of Sai Duolisi balances
Department)；RE-52AA Rotary Evaporators (Shanghai Yarong Biochemical Instrument Plant)；(Zhejiang temperature brother's mechanical valve industry has 40L multi-function extractors
Limit company)；HS6150 types ultrasonic cleaner (Tianjin perseverance AudioCodes skill Development Co., Ltd).
2. method and result
The collection of 2.1 concentrate samples
Because the medicine workshop concentrator (coiled vacuum concentration pan) of Liaoning China Resources Benxi three can in concentration process
To take out concentrate sample, concentration process sample is in Liaoning Huarun Benxi Third Pharmaceutical Co., Ltd.'s workshop collection in worksite.Extract
The standing filtered fluid of liquid is in input disc tube type vacuum concentration pan and when reaching default thickening temperature and pressure as time zero
And starting sampling, sample volume is 50mL.Often sample every other hour within first 8 hours or so.Concentration in all single-action and economic benefits and social benefits
Liquid was sampled once after being input to coiled vacuum concentration pan every 20 minutes, until going out cream, repeated 10 batches.All batch realities
120 samples are obtained after the completion of testing.Using the 1st, 2,3,4,6,7,8,9,10 concentrate samples of experiment as calibration set, the
5 concentrate samples collect as checking.
2.2 near infrared spectra collections
Gather the transmitted spectrum of the concentrate of qizhi weitong granules：Set the 4000~10000cm of sweep limits of spectrum-1,
Scanning times are 32 times, and resolution ratio is 8cm-1, with air as background, using the cylindrical glass colorimetric cylinder of 5mm light paths, at one
In constant environment (temperature be 25 DEG C, humidity be 35%~45%) collection qizhi weitong granules concentrate transmitted spectrum,
Each sample replication 3 times, calculates averaged spectrum.Extract solution concentration process is original in the preparation process of qizhi weitong granules
Near infrared spectrum is as shown in Figure 1.
A series of wave bands have selected using TQ, OPUS and correlation coefficient process respectively, by comparing each wave band and not
With the modeling effect of band combination, 5449.8~6101.7cm is finally selected-1, 5149.01~5442.13cm-1With 5469.13
~7143.04cm-1, 5149.01~5442.13cm-1With 5469.13~7143.04cm-1Respectively as Paeoniflorin, it is relatively close
Degree, the modeling wave band of solid content, and using single order, second dervative treatment, smooth, vector normalizing, scattering effect correction, polynary line
Property various chemometrics methods such as correction, wavelet transformation, this model sets up and combines S-G using single order, second dervative treatment
Or the method for Norris smothing filterings is pre-processed to spectrum, using setting up Chinese herbaceous peony after original spectrum and different pretreatments method
The R that medicine glycosides, relative density, the near-infrared quantitative calibration models of solid content are obtained2, RMSEC, RMSECV value is respectively such as table 1, table 2
With shown in table 3, preprocess method is determined by RMSEC the and RMSECV values for comparing the model that different pretreatments method is set up.
The parameter of the Paeoniflorin quantitative determination model of the extract solution concentration process of the different pretreatments method of table 1
The extract solution concentration process relative density quantitative determination model parameter of the different pretreatments method of table 2
The extract solution concentration process solid content quantitative determination model parameter of the different pretreatments method of table 3
From table 1, table 2 and table 3, different pretreatments method is set up in PLS calibration models, the RMSECV values of Paeoniflorin
It is relatively close with RMSEC values to be processed through second dervative when the spectrum after the method for+Norris smothing filterings is processed is modeled as minimum
The RMSECV values and RMSEC values of degree and solid content are with the light after the method treatment that+Norris smothing filterings are processed through first derivative
It is minimum during spectrum modeling.Therefore, Paeoniflorin model spectrum is carried out using the method for second dervative treatment+Norris smothing filterings
Pretreatment, is carried out pre- using the method for first derivative treatment+Norris smothing filterings to relative density and solid content model spectrum
Treatment；Quantitative model is calculated using PLS (PLSR).
2.3 paeoniflorin contents are determined
The above-mentioned extract solution sample for collecting is centrifuged 10min (13000r/min), supernatant is pipetted, according to sample concentration
With 5 times or 10 times of distilled water diluting, HPLC assays are carried out, HPLC conditions are as follows：
Chromatographic column：Agilent Zorbax SB-C18 (4.6 × 250mm, 5 μm)；
Mobile phase：0.1% phosphoric acid water (A)-acetonitrile (B)；Sample size：5μL
Flow velocity：1.0mL/min；Column temperature：30℃；Detection wavelength：230nm；
Gradient program is shown in Table 4.
The gradient elution program of table 4
Analyzed by 2.3 chromatographic conditions, sample size is 5 μ L, determines the content of different batches Paeoniflorin.Paeoniflorin containing measurement
Determine result as shown in table 5, the HPLC collection of illustrative plates of Paeoniflorin reference substance is as shown in Fig. 2 HPLC collection of illustrative plates such as Fig. 3 institutes of Paeoniflorin sample
Show.
The extract solution concentration process paeoniflorin content measurement result of table 5
2.4 relative density determinations
Supernatant is pipetted after concentrate sample centrifugation (13000r/min, 10min), constant temperature in 50 DEG C of water-baths is placed in and is kept
30min.Precision pipettes 1mL supernatant samples, weighs, and institute's value is concentrating sample relative density values (g/mL), by 2.4 phases
To density measurement method, the relative density of different batches concentrate is determined, the results are shown in Table 6.
The extract solution concentration process relative density determination result of table 6
2.5 determination of solid content
Extract solution stand 24h, measure 4mL supernatants to dried to constant weight flat bottle (twice dry after weight difference away from
Less than 5mg) (X0), weigh (X1), put and dry under the conditions of 105 DEG C of baking oven to weight difference of weighing twice away from less than 5mg, count X2。
Solid content (%)=(X2-X0)/(X1-X0) × 100%
By " 2.5 determination of solid content " method, the solid content of different batches concentrate, the assay result such as institute of table 7 are determined
Show.
The extract solution concentration process determination of solid content result of table 7
The foundation of 2.6 quantitative models
The wave band and Pretreated spectra side for selecting optimum modeling are set up extract solution concentration process Paeoniflorin, relative density, are consolidated
Content quantitative detection model, the parameter of gained model is as shown in table 21.The near-infrared predicted value of Paeoniflorin calibration set sample and height
The dependency relation figure of liquid phase measurement value is imitated as shown in figure 4, the near-infrared predicted value and measured value of relative density calibration set sample
Dependency relation figure is as shown in figure 5, near-infrared predicted value and dependency relation figure such as Fig. 6 institutes of measured value of solid content calibration set sample
Show.From Fig. 4~Fig. 6, correlation is good between near-infrared predicted value and measured value, and measurement result reaches unanimity substantially.By
Knowable to table 8, Paeoniflorin, relative density, solid content model calibration set coefficient R2Respectively up to 0.98125,0.99551,
0.99977, RMSEC is respectively 0.597,0.00584,0.247, now corresponds to RMSECV minimum.
The quantitative determination model parameter of the extract solution concentration process of table 8
2.7 extract solution concentration process are predicted
The sample of the 5th batch of extraction is predicted with the calibration model set up, the near-infrared of Paeoniflorin checking collection sample
The dependency relation figure of predicted value and HPLC measured values is as shown in fig. 7, near-infrared predicted value and the survey of relative density checking collection sample
The dependency relation figure of definite value is as shown in figure 8, the near-infrared predicted value and the dependency relation figure of measured value of solid content checking collection sample
As shown in Figure 9.From Fig. 7~Fig. 9, Paeoniflorin, relative density, solid content forecast set coefficient R2Respectively 0.99859,
0.99876th, 0.99743, this shows, there is good correlation between predicted value and control value, and model has preferable performance；Chinese herbaceous peony
Glycosides, relative density, the RMSEP of solid content be respectively 0.407,0.00677,0.436, Paeoniflorin, relative density, solid content
RSEP is respectively 7.10%, 0.62%, 1.86%, controls within 10%, disclosure satisfy that Chinese Traditional Medicine monitor in real time point
The required precision of analysis.
Extract solution concentration process determination of solid content is as shown in Figure 10 with the change in concentration compares figure of model prediction solid content, carries
Take liquid concentration process relative density determination as shown in figure 11 with the change in concentration compares figure of model prediction relative density, extract solution is dense
Compression process determination of solid content is as shown in figure 12 with the change in concentration compares figure of model prediction solid content.From Figure 10~Figure 12,
The near-infrared predicted value that model is obtained is consistent substantially with Paeoniflorin, relative density, determination of solid content value, its predicted value
Process trend is also substantially the same with real process.
After Paeoniflorin, relative density, solid content calibration model are established, using institute's construction method, NIRS completes one-shot measurement only
Need 20 seconds, and efficient liquid phase completes 1 paeoniflorin content and determine at least to need 30min, relative density, determination of solid content are then at least
Some hours.Therefore, extraction of traditional Chinese medicine active constituent content and solid content can be not only realized using near infrared spectroscopy
Real-time monitoring, and its detection method is easier than conventional method, more rapidly.
To sum up, the near infrared spectrum of extract solution concentration process exists in the preparation process for establishing qizhi weitong granules of the invention
Provision of on-line analysis methodology, and it is applied to on-line checking, realize extract solution concentration process in the preparation process of qizhi weitong granules
Aulomatizeted Detect and each quality control index content real-time estimate；The model prediction accuracy set up is high, and the degree of accuracy is high, meets real
The requirement of quantitative analysis in the production of border.
Obviously, above-described embodiment is only intended to clearly illustrate example, and not to the restriction of implementation method.It is right
For those of ordinary skill in the art, can also make on the basis of the above description other multi-forms change or
Change.There is no need and unable to be exhaustive to all of implementation method.And the obvious change thus extended out or
Among changing still in the protection domain of the invention.
Claims (9)
1. in a kind of preparation process of utilization near infrared spectroscopy quick detection qizhi weitong granules extract solution concentration process side
Method, it is characterised in that
The step of assay, relative density and/or determination of solid content including following Paeoniflorin:
A, the assay of Paeoniflorin are comprised the following steps：
(1) concentrated extracting solution of the qizhi weitong granules of known paeoniflorin content is taken, it is standby；
(2) concentrated extracting solution of the qizhi weitong granules is carried out near infrared spectrum scanning, gathers the qizhi weitong granules
Concentrated extracting solution near infrared spectrum；
(3) 5449.8~6101.7cm is chosen-1With 5149.01~5442.13cm-1Spectral information under characteristic wave bands, application
Meterological software is learned to be closed with the paeoniflorin content of the concentrated extracting solution of the qizhi weitong granules of the known paeoniflorin content
Connection, the quantitative calibration model set up between near infrared spectrum and standard content using PLS；
(4) near infrared spectrum is carried out to the concentrated extracting solution sample of unknown qizhi weitong granules according to the method for the step (2)
Scanning, and choose 5449.8~6101.7cm-1With 5149.01~5442.13cm-1Spectral information under characteristic wave bands, importing is built
Vertical quantitative calibration model obtains the paeoniflorin content value of the concentrated extracting solution sample of the unknown qizhi weitong granules；
B, relative density determination are comprised the following steps：
(1) concentrated extracting solution of the qizhi weitong granules of known relative density is taken, it is standby；
(2) concentrated extracting solution of the qizhi weitong granules is carried out near infrared spectrum scanning, gathers the qizhi weitong granules
Concentrated extracting solution near infrared spectrum；
(3) 5469.13~7143.04cm is chosen-1With 5149.01~5442.13cm-1Spectral information under characteristic wave bands, application
Chemo metric software is associated with the relative density of the concentrated extracting solution of the qizhi weitong granules of the known relative density,
The quantitative calibration model set up between near infrared spectrum and standard content using PLS；
(4) near infrared spectrum is carried out to the concentrated extracting solution sample of unknown qizhi weitong granules according to the method for the step (2)
Scanning, and choose 5469.13~7143.04cm-1With 5149.01~5442.13cm-1Spectral information under characteristic wave bands, imports
The quantitative calibration model of foundation obtains the relative density values of the concentrated extracting solution sample of the unknown qizhi weitong granules；
C, determination of solid content are comprised the following steps：
(1) concentrated extracting solution of the qizhi weitong granules of known solid content is taken, it is standby；
(2) concentrated extracting solution of the qizhi weitong granules is carried out near infrared spectrum scanning, gathers the qizhi weitong granules
Concentrated extracting solution near infrared spectrum；
(3) 5469.13~7143.04cm is chosen-1Spectral information under characteristic wave bands, Applied Chemometrics software with it is described
Know that the solid content of the concentrated extracting solution of the qizhi weitong granules of solid content is associated, near-infrared is set up using PLS
Quantitative calibration model between spectrum and standard content；
(4) near infrared spectrum is carried out to the concentrated extracting solution sample of unknown qizhi weitong granules according to the method for the step (2)
Scanning, and choose 5469.13~7143.04cm-1Spectral information under characteristic wave bands, imports the quantitative calibration model set up and obtains
The solid content value of the concentrated extracting solution sample of the unknown qizhi weitong granules.
2. extracted in the preparation process of utilization near infrared spectroscopy quick detection qizhi weitong granules according to claim 1
The method of liquid concentration process, it is characterised in that
In the step of the step of assay of the Paeoniflorin (2) neutralizes determination of solid content (2), using static spectrum acquisition method
The near infrared spectra collection of the concentrated extracting solution of the qizhi weitong granules is carried out, actual conditions is：Spectral acquisition times are spaced
It is 10min, with air as reference, scanning times are 32 times, and resolution ratio is 8cm-1, scanning optical spectrum scope is 4000~10000cm-1。
3. in the preparation process of utilization near infrared spectroscopy quick detection qizhi weitong granules according to claim 1 and 2
The method of extract solution concentration process, it is characterised in that
In the step of assay of the Paeoniflorin (2), also including being led using second order to the near infrared spectrum for collecting
The step of number method and Norris derivative smoothing filter methods are pre-processed；
In the step of relative density (2) and/or the step of determination of solid content in (2), also including described near to what is collected
The step of infrared spectrum is pre-processed using First derivative spectrograply and Norris derivative smoothing filter methods.
4. the preparation of the utilization near infrared spectroscopy quick detection qizhi weitong granules according to claim any one of 1-3
The method of extract solution concentration process in journey, it is characterised in that
The bulk drug of the qizhi weitong granules is constituted：
The weight portion of radix bupleuri 30~100, the weight portion of Radix Glycyrrhizae 15~60, the weight portion of rhizoma cyperi 35~120, the weight portion of corydalis tuber 35~120,
The weight portion of the root of herbaceous peony 40~150, the weight portion of Fructus Aurantii 35~120.
5. the preparation of the utilization near infrared spectroscopy quick detection qizhi weitong granules according to claim any one of 1-4
The method of extract solution concentration process in journey, it is characterised in that
The preparation method of the qizhi weitong granules is comprised the following steps：
(1) Fructus Aurantii and rhizoma cyperi of selected weight portion are taken, volatile oil is extracted, liquid is standby, and the dregs of a decoction are discarded；
(2) radix bupleuri, Radix Glycyrrhizae, corydalis tuber and the root of herbaceous peony of selected weight portion are taken, are added water to cook 2 times, the 1st decoction 0.5~4 hour,
Decoct 0.5~3 hour for 2nd time；
(3) decocting liquid of combining step (1) and step (2), filtering, filtrate is concentrated into the clear cream that relative density is 1.10~1.30；
(4) qinghuo reagent, plus auxiliary material, mixing are made particle, dry, and spray into volatile oil, obtain final product granule.
6. the preparation of the utilization near infrared spectroscopy quick detection qizhi weitong granules according to claim any one of 1-5
The method of extract solution concentration process in journey, it is characterised in that
In the step of assay of the Paeoniflorin (3), relative density determination the step of (3) neutralize determination of solid content the step of
(3) in, also including evaluating the estimated performance of the quantitative calibration model set up the step of, the evaluation index includes
Coefficient R, calibration set mean square deviation RMSEC, checking collection root mean square RMSEP, cross validation root mean square RMSECV and prediction are relative
Deviation RSEP, when R values closer to 1, RMSEC and RMSEP values it is smaller and closer to when, evaluation model stability is better, prediction
Precision is higher, then disclosure satisfy that the precision of prediction requirement of qizhi weitong granules Direct Analysis；Conversely, not applying to then.
7. the preparation of the utilization near infrared spectroscopy quick detection qizhi weitong granules according to claim any one of 1-6
The method of extract solution concentration process in journey, it is characterised in that
In the step of assay of the Paeoniflorin (1), using known paeoniflorin content described in high effective liquid chromatography for measuring
The paeoniflorin content of qizhi weitong granules is used as standard content；
In the step of determination of solid content (3), the solid of known solid content qizhi weitong granules is determined using oven drying method and is contained
Amount is used as standard content.
8. extracted in the preparation process of utilization near infrared spectroscopy quick detection qizhi weitong granules according to claim 7
The method of liquid concentration process, it is characterised in that
The tool of the paeoniflorin content of known paeoniflorin content qizhi weitong granules described in the use high effective liquid chromatography for measuring
Body step is：
(1) 4~6mL of concentrated extracting solution of the qizhi weitong granules is taken, under the conditions of rotating speed 12000-14000r/min
8~12min of centrifugation, takes supernatant, as need testing solution；
(2) precision weighs 1-3mg Paeoniflorin reference substances and is placed in 20mL measuring bottles, plus methyl alcohol is made every mL and contains 0.05~0.15mg's
Solution, shakes up, used as reference substance solution；
(3) chromatographic condition：It is chromatographic column with 4.6 × 250mm, 5 μm of Agilent Zorbax SB-C18, with 0.1% phosphoric acid water
Solution is mobile phase A, carries out gradient elution according to following program by Mobile phase B of acetonitrile：0-13min, A：B is 85%：15%；
13-15min, A：B is 85%：15% → 10%：90%；15-19min, A：B is 10%：90%；19-25min, A：B is
10%：90% → 0%：100%；25-30min, A：B is 0%：100% → 85%：15%；Flow velocity 1.0mL/min, column temperature 30
DEG C, Detection wavelength 230nm；
(4) it is accurate to draw the need testing solution and each 5 μ L of reference substance solution, liquid chromatograph is injected, determine；
The use oven drying method determines concretely comprising the following steps for the solid content of the known solid content qizhi weitong granules：
The measuring cup of the concentrated extracting solution of qizhi weitong granules described in 4~6mL as drying to constant weight is taken, dry 5 in 105 DEG C~
7h, moves to 20~40min of cooling in drier, weighs；Dried 0.5~1.5 hour at 105 DEG C, cooling is weighed；To even
Continuous difference of weighing twice calculates solid content no more than untill 5mg.
9. in the preparation process of the utilization near infrared spectroscopy quick detection qizhi weitong granules described in any one of claim 1-8
Purposes of the method for extract solution concentration process in qizhi weitong granules quality testing and control.
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