CN109856084A - A kind of stomach pill of aucklandia and amomum fruit condensed pill preparation process quality monitoring method - Google Patents
A kind of stomach pill of aucklandia and amomum fruit condensed pill preparation process quality monitoring method Download PDFInfo
- Publication number
- CN109856084A CN109856084A CN201910234079.7A CN201910234079A CN109856084A CN 109856084 A CN109856084 A CN 109856084A CN 201910234079 A CN201910234079 A CN 201910234079A CN 109856084 A CN109856084 A CN 109856084A
- Authority
- CN
- China
- Prior art keywords
- model
- sample
- aurantiamarin
- pill
- magnolol
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Withdrawn
Links
Landscapes
- Investigating Or Analysing Materials By Optical Means (AREA)
Abstract
The present invention relates to stomach pill of aucklandia and amomum fruit condensed pill preparation process quality monitoring methods, it effectively solves the problems, such as quickly to carry out quality testing to stomach pill of aucklandia and amomum fruit condensed pill during online production, the sample near infrared spectrometer that different water mention time and concentration time is scanned into sample, obtain sample original spectral data, go out the content of Calibration aurantiamarin honokiol using high effective liquid chromatography for measuring, calibration set and verifying collection are selected by index component content, area's selection is pre-processed and composed to spectroscopic data, the content that HPLC is measured makees reference value, Calibration characteristic spectrum and reference value are combined with Partial Least Squares method and establish near infrared spectrum multivariate calibration model, model is verified；NIRS map is inputted in calibration model, NIRS predicted value and HPLC reference value are analyzed；The NIRS predicted value of verification sample collection compare with the content of aurantiamarin honokiol using the measurement of HPLC method, calibration model is monitored, measures whether verification sample collection is out-of-bounds point.
Description
Technical field
The present invention relates to medical domains, especially carry out with near-infrared spectrum technique to stomach pill of aucklandia and amomum fruit (condensed pill)
Line detects and controls a kind of stomach pill of aucklandia and amomum fruit condensed pill preparation process quality monitoring method of quality.
Background technique
Stomach pill of aucklandia and amomum fruit (condensed pill) is recorded in 2015 editions " Chinese Pharmacopoeias ", is simply the fructus amomi by radix aucklandiae, dried orange peel, Rhizoma Atractylodis Macrocephalae,
The compound preparation of the 14 taste Chinese medicinal composition such as stir-baked CORTEX MAGNOLIAE OFFICINALIS with rhizoma zingiberis recens juice, has effects that warming middle-JIAO for easing the stomach, is mainly used for stomach YANG deficiency, retention of damp leading to blockage of QI institute
The stomachache of cause, feeling of fullness, symptoms include stomachache is indistinct, oppression sensation over the epigastrium, acid regurgitation, noisy discomfort, do not feel like eating, four limbs burnout.The system
Agent is evolved by traditional Chinese medicine prescription, rapid-action, and good effect, side effect is low, is clinically widely used.
Stomach pill of aucklandia and amomum fruit (condensed pill) prescription is complicated, more comprising medicinal material type, and the presently commercially available sample for having 13 producers is changed
Learn component content and meet quality inspection standard, but in the said preparation of different manufacturers ingredient content it is variant, this is from different productions
The preparation process of producer has that difference is closely bound up, therefore, is rigid in checking up very to the links in said preparation preparation process
It is necessary to.In Chinese materia medica preparation preparation process, extraction process, which is one, has the characteristics that the big dynamic change body of multivariable, disturbance
System has great influence to the quality and curative effect of Chinese materia medica preparation to the quality control of process.
Near-infrared spectrum technique is a kind of emerging technology to grow up the late 1980s, has pre-treatment letter
Single, the feature of analytic process accurately and fast, green is widely used in the Qualitive test of Chinese medicine and Chinese materia medica preparation, containing measurement
Fixed, on-line checking of preparation process etc..In test sample, near-infrared spectrum technique do not need many and diverse pre-treatment and
Chemical reaction process, so that it may complete the acquisition to the near infrared spectrum of sample, and then be completed by model foundation to sample
The measurement of multinomial performance index in this, and measurement result is stablized, favorable reproducibility.In recent years, near-infrared spectrum technique is considered as
One of the technology that can be used in on-line checking, near-infrared spectrum technique is used in actual production, on production line raw material, half
Finished product and finished product carry out on-line checking, to the situation of change of timely discovery product quality, to regulate and control in time, to maintenance product matter
The stabilization of amount is of great significance.But how to apply near infrared technology, to during online production stomach pill of aucklandia and amomum fruit condensed pill into
Row detection, controls in quality so far there are no public reporting.
Summary of the invention
For above situation, for the defect for overcoming the prior art, the object of the present invention is to provide a kind of stomach pill of aucklandia and amomum fruit is dense
Contracting ball preparation process quality monitoring method can effectively solve quickly to carry out matter to stomach pill of aucklandia and amomum fruit condensed pill during online production
Amount detection, to overcome the problems, such as that the cumbersome of conventional method, high production cost, low efficiency, wastage of material are excessive.
The technical solution that the present invention solves is, a kind of stomach pill of aucklandia and amomum fruit condensed pill preparation process quality monitoring method is, point
Different water the stomach pill of aucklandia and amomum fruit condensed pill sample of time and concentration time is not mentioned into the close of near infrared spectrometer scanning sample
Infrared absorption spectrum obtains sample original spectral data, determines Calibration orange peel using high performance liquid chromatography (HPLC)
The content of glycosides honokiol, by index component content select calibration set and verifying collect, then to spectroscopic data pretreatment and
Area's selection is composed, the content that HPLC is measured is as reference value, with Partial Least Squares (PLS) the method high-ranking officers in Chemical Measurement
Positive sample sets characteristic spectrum and reference value combine and establish near infrared spectrum multivariate calibration model (also known as calibration model), then to mould
Type is verified；The NIRS map of verification sample collection sample is inputted in calibration model, and NIRS predicted value and HPLC are referred to
Value carries out correlation analysis；By the content of the NIRS predicted value of verification sample collection and the aurantiamarin honokiol using the measurement of HPLC method
Control, is monitored calibration model, and whether measurement verification sample collection is out-of-bounds point, being capable of index in Accurate Determining coverage area
Property ingredient content, guarantee product quality.
The method of the present invention is simple, easy to operate, and the whole process time is short, speed is fast, accurate, can real-time online detection, greatly
It improves work efficiency greatly, reduces operating cost, it is ensured that product quality has significant economic and social benefit.
Detailed description of the invention
Fig. 1 is that the near infrared spectrum for 72 parts of Aqueous extracts samples that stomach pill of aucklandia and amomum fruit condensed pill difference water of the present invention mentions the time is folded
Add figure.
Fig. 2 mentions the related figure between process crosscheck error mean square root (RMSECV) and number of principal components for water of the present invention.
Fig. 3 mentions the related figure between course prediction value and reference value for water of the present invention.
Fig. 4 is the near infrared spectrum superposition of 99 parts of concentrating samples of stomach pill of aucklandia and amomum fruit condensed pill difference concentration time of the present invention
Figure.
Fig. 5 is the related figure between concentration process of the present invention crosscheck error mean square root (RMSECV) and number of principal components.
Related figure of the Fig. 6 between concentration process monitor value of the present invention and reference value.
Specific embodiment
It elaborates with reference to embodiments with concrete condition to a specific embodiment of the invention.
A kind of stomach pill of aucklandia and amomum fruit condensed pill preparation process quality monitoring method of the present invention is to collect different water to mention time and dense
The stomach pill of aucklandia and amomum fruit condensed pill sample of contracting time obtains sample original with the near-infrared absorption spectrum of near infrared spectrometer scanning sample
Beginning spectroscopic data is determined the content of Calibration aurantiamarin honokiol using high performance liquid chromatography (HPLC), passed through
Index component content selects calibration set and verifying collection, then pre-processes and composes area's selection to spectroscopic data, HPLC is measured
Content is as reference value, with Partial Least Squares (PLS) method in Chemical Measurement by Calibration characteristic spectrum and ginseng
It examines value and combines and establish near infrared spectrum multivariate calibration model (also known as calibration model), then model is verified；It specifically includes
Following steps:
(1), the stomach pill of aucklandia and amomum fruit condensed pill that different water mention time and concentration time, the stomach pill of aucklandia and amomum fruit concentration are collected
Ball is by radix aucklandiae 210g, fructus amomi 210g, Rhizoma Atractylodis Macrocephalae 300g, dried orange peel 300g, Poria cocos 300g, tuber of pinellia 300g processed, prepared RHIZOMA CYPERI with vinegar 210g, fries trifoliate orange
Real 210g, decladding cardamom 210g, stir-baked CORTEX MAGNOLIAE OFFICINALIS with rhizoma zingiberis recens juice 210g, Pogostemon cablin 210g, Radix Glycyrrhizae 90g, ginger 90g and jujube 150g are as Chinese medicine original
Material is made, in which: by dried orange peel, prepared RHIZOMA CYPERI with vinegar, the radix aucklandiae extraction volatilization for frying the dried immature fruit of citron orange, stir-baked CORTEX MAGNOLIAE OFFICINALIS with rhizoma zingiberis recens juice, Pogostemon cablin, ginger and 80% weight
Oil；The tuber of pinellia processed of the remaining dregs of a decoction and Rhizoma Atractylodis Macrocephalae, Poria cocos, Radix Glycyrrhizae, jujube and 20% weight adds water to cook, and filters, and filtrate is condensed into 60
DEG C relative density is the thick paste of 1.35-1.40；Fructus amomi, decladding cardamom and the remaining tuber of pinellia processed and radix aucklandiae are ground into medicinal powder again；
Medicinal powder, thick paste, volatile oil and maltose are mixed, pill, drying, polishing, as finished product stomach pill of aucklandia and amomum fruit condensed pill；It is producing
In, the quality for mentioning process and concentration process to water is monitored；
(2), the quality-monitoring during water mentions, comprising the following steps:
1., prepare test solution and Aqueous extracts sample:
By radix aucklandiae 168g, dried orange peel 300g, prepared RHIZOMA CYPERI with vinegar 210g, fry dried immature fruit of citron orange 210g, stir-baked CORTEX MAGNOLIAE OFFICINALIS with rhizoma zingiberis recens juice 210g, Pogostemon cablin 210g and ginger
90g is crushed, this 7 taste medicinal material is set in a round bottom flask, adds 10 times of weight distilled water, extracts volatile oil；After extracting volatile oil
The dregs of a decoction are mixed with jujube 150g, Poria cocos 300g, tuber of pinellia 60g processed, Radix Glycyrrhizae 90g and Rhizoma Atractylodis Macrocephalae 300g again, and radix aucklandiae, old is added
Skin, prepared RHIZOMA CYPERI with vinegar fry the dried immature fruit of citron orange, stir-baked CORTEX MAGNOLIAE OFFICINALIS with rhizoma zingiberis recens juice, Pogostemon cablin, ginger, jujube, Poria cocos, the tuber of pinellia processed, Radix Glycyrrhizae and 10 times of Rhizoma Atractylodis Macrocephalae bulking value
Distilled water, the bulking value refer to solid in terms of g, and liquid is in terms of mL, and timing decocts 2h since boiling, takes every 10min
Sample is primary, each 15mL, and every 15mL is a test solution, and the distilled water that equivalent is added after every sub-sampling immediately supplies decoction
Liquid after decocting for the first time, adds radix aucklandiae, dried orange peel, prepared RHIZOMA CYPERI with vinegar, fries the dried immature fruit of citron orange, stir-baked CORTEX MAGNOLIAE OFFICINALIS with rhizoma zingiberis recens juice, Pogostemon cablin, ginger, jujube, Fu
Siberian cocklebur, the tuber of pinellia processed, Radix Glycyrrhizae and 10 times of Rhizoma Atractylodis Macrocephalae bulking value of distilled water carry out second and decoct, and timing decocts 2h since boiling, are decocting
It boils in extraction process and samples according to upper method to get 24 parts of Aqueous extracts samples, prepare 3 batches of Aqueous extracts in this approach, collect 72 parts altogether
Aqueous extracts sample；
2., establish calibration model, method is:
A, the acquisition of NIRS spectrum: Aqueous extracts sample is scanned using air as reference near infrared spectrometer, is deducted
Background acquires spectrogram, using optical fiber transflector, resolution ratio 8cm-1, light path 2.0mm, scanning times 64 times, scanning range: 4000
~12000cm-1, 20 DEG C of temperature, relative humidity 33%~35% is scanned by above-mentioned condition, each sample multiple scanning 3
It is secondary, averaged spectrum is acquired, original spectral data is obtained；
B, the HPLC of aurantiamarin and Determination of Magnolol is measured in Aqueous extracts sample, and method is:
1), aurantiamarin HPLC chromatogram condition are as follows: high performance liquid chromatograph, Symmetry C18 chromatographic column 4.6mm ×
150mm, 5 μm, Yi Jing ︰ water=67 ︰s 33 of the mobile phase for volume ratio, column temperature: 30 DEG C, sample volume 10 μ L, flow velocity 1mLmin-1,
Detection wavelength 225nm；
Magnolol HPLC chromatogram condition are as follows: high performance liquid chromatograph, Symmetry C18 chromatographic column 4.6mm × 150mm, 5 μ
M, Yi Jing ︰ Shui ︰ glacial acetic acid=62 ︰ 37 ︰ 1 of the mobile phase for volume ratio, column temperature: 30 DEG C, sample volume 10 μ L, flow velocity 1mLmin-1,
Detection wavelength 284nm；
2), the preparation of reference substance solution: precision weighs aurantiamarin, magnolol reference substance, is respectively placed in volumetric flask, adds first
Alcohol dissolution, is made solution of every 1mL containing 49 μ g of reference substance, 60 μ g, 0.45 μm of filtering with microporous membrane obtains reference substance solution；
3), Aqueous extracts sample measures: accurate respectively to draw reference substance solution and the efficient liquid of each 20 μ L injection of Aqueous extracts sample
Chromatography measurement, obtains aurantiamarin and Determination of Magnolol；
C, the selection of calibration set and verifying collection sample: according to the content distribution of aurantiamarin in sample, by 72 parts of samples of gained
It is divided into calibration set and verifying collection, wherein calibration set is 60 parts, 12 parts of verifying collection, and verifying collection range is made to be evenly distributed on calibration set
Within content range, in which:
Aurantiamarin: calibration set, maximum value 1.255%, minimum value 0.651%, average value 0.953%；Verifying collection, maximum value
1.250%, minimum value 0.775%, average value 1.013%；
Magnolol: calibration set, maximum value 0.297%, minimum value 0.070%, average value 0.184%；Verifying collection, maximum value
0.292%, minimum value 0.075%, average value 0.184%；
D, the selection of preprocessing procedures: the physical properties such as particle size, uniformity of sample and measuring condition
Difference can all influence the acquisition of near infrared spectrum, lead to spectrum drift.The pretreatment of spectrum can purify spectrogram, reduction spectrum floats
It moves, reduce random noise, improve the robustness of near-infrared model；Quantitative model is with cross-validation related coefficient (R2), school
Positive mean square deviation (RMSEC), prediction mean square deviation (RMSEP) are that overall target evaluates model, and R2 illustrates sample closer to 1
Chemical score and near-infrared predicted value correlation are better, and RMSEC, RMSEP are smaller, illustrate that the estimated performance of model is better, using not
Same preprocess method is investigated, and optimal combination is selected to carry out the foundation of model, obtains aurantiamarin and magnolol near-infrared is fixed
The best preprocess method for measuring model is respectively PLS+1st Der+FD, PLS+2nd Der, and different preprocess method results is shown in
Table 1.
The selection of 1 different pretreatments method of table
E, it builds the selection for touching wave band: being established in stomach pill of aucklandia and amomum fruit condensed pill water extraction process using Partial Least Squares PLS
The Quantitative Monitoring model of aurantiamarin, with R2It is index closest to 1 and RMSECV, different spectral coverages is in optimized selection, orange peel
It is 4084.49~11574.66cm that glycosides, which models wave band,-1Spectral coverage, it is 5467.00~11357.04cm that magnolol, which models spectral coverage,-1；
F, the selection of number of principal components: the selection of principal component has a great impact to the prediction result of model, when selected
When principal component is excessive, model includes excessive measurement noise, over-fitting occurs；When principal component is very few, and it will lead to modeling
Information is not complete, and predictive ability is poor, and accordingly, aurantiamarin is established in model, and the number of principal components PLS factor is 9, is aurantiamarin best modeled
Number of principal components；In magnolol model foundation, the number of principal components PLS factor is 9, is magnolol best modeled number of principal components；
G, aurantiamarin model is established with the PLS method in TQAnalyst8.0 software, PLS+1st Der+ is carried out to spectrum
FD pretreatment, using 4084.49~11574.66cm-1Wave band, 9 number of principal components are modeled, the R of established model2=
0.99899, RMSECV=0.00125, RMSEP=0.00130；Cortex Magnoliae Officinalis is established with the PLS method in TQAnalyst8.0 software
Phenol model carries out PLS+2nd Der pretreatment to spectrum, using 5467.00~11357.04cm-1Wave band, 9 number of principal components into
Row modeling, the R of established model2=0.97998, RMSECV=0.00122, RMSEP=0.00139；
3., the verifying of calibration model:
By in the NIRS map input calibration model of 12 parts of verifying collection samples, and by NIRS predicted value and HPLC reference value into
The related identification of row, aurantiamarin prediction related coefficient and prediction mean square deviation are respectively 0.9971,0.0016；Magnolol predicts phase relation
Number is respectively 0.9872,0.0023 with prediction mean square deviation, measures the content of aurantiamarin and magnolol；
(3), the monitoring of the concentration process quality of stomach pill of aucklandia and amomum fruit condensed pill, method is:
1., the preparation of sample and test sample: choose 5 parts of Aqueous extracts, every part of 4000mL 1. prepared by step (2), use
Conventional concentration method carries out heating under reduced pressure concentration under the conditions of temperature 60 C, vacuum degree 0.08-0.09MPa, leads in concentration process
Needle tubing connection plastic pipe on-line period is crossed, each batch is respectively separated 5min, 7min, 9min, and 11min, 13min sampling are primary,
It extracts 10mL every time to be placed in tool plug centrifuge tube, the extracting solution of 5 batches collects 99 parts of concentrate altogether；
2., establish calibration model:
A, the acquisition of NIRS spectrum: concentrate sample is scanned using air as reference near infrared spectrometer, is deducted
Background acquires spectrogram, using optical fiber transflector, resolution ratio 8cm-1, light path 2.0mm, scanning times 64 times, scanning range: 4000
~12000cm-1, 24 DEG C of temperature, humidity 42%~45% is scanned by above-mentioned experimental condition, each sample multiple scanning 3
It is secondary, averaged spectrum is acquired, original spectral data is obtained；
B, the HPLC of aurantiamarin and Determination of Magnolol is measured in sample:
1), aurantiamarin HPLC chromatogram condition are as follows: high performance liquid chromatograph, Symmetry C18 chromatographic column 4.6mm ×
150mm, 5 μm, mobile phase be volume ratio Yi Jing ︰ water=67 ︰ 33, column temperature: 30 DEG C, sample volume 10 μ L, flow velocity 1mLmin-1, inspection
Survey wavelength 225nm；
Magnolol HPLC chromatogram condition are as follows: high performance liquid chromatograph, Symmetry C18 chromatographic column 4.6mm × 150mm, 5 μ
M, mobile phase be volume ratio Yi Jing ︰ Shui ︰ glacial acetic acid=62 ︰, 37 ︰ 1, column temperature: 30 DEG C, sample volume 10 μ L, flow velocity 1mLmin-1, inspection
Survey wavelength 284nm；
2), the preparation of reference substance solution: precision weighs aurantiamarin, magnolol reference substance, is respectively placed in 10mL volumetric flask,
Add methanol to dissolve and be settled to scale, solution of every 1mL containing 49 μ g of reference substance, 60 μ g is made, 0.45 μm of filtering with microporous membrane obtains
Reference substance solution；
3), sample measures: accurate respectively to draw reference substance solution and each 20 μ L injection high performance liquid chromatography of test solution
Instrument, measurement obtain the aurantiamarin and Determination of Magnolol of HPLC measurement；
C, in concentration process relative density measurement: according to 2015 editions " Chinese Pharmacopoeia " annex VII A relative density determinations
Bottle method measures relative density in method；
D, the selection of calibration set and verifying collection sample: according to the content of aurantiamarin, magnolol and relative density in sample point
99 parts of samples of gained are divided into calibration set and verifying collect by cloth, are evenly distributed on verifying collection range within calibration set content range,
The content distribution range of calibration set and verifying collection aurantiamarin, magnolol and relative density is shown in Table 2:
2 calibration set of table and verifying collection sample content distribution
D, the selection of preprocessing procedures: when near infrared spectrometer acquires spectrum, since external environment, instrument work
The difference of state, sample physical property can cause bigger influence to the foundation of model, by being pre-processed most to spectrum
The reductions of limits influences, and to establish accurate model, accordingly, preprocessing procedures are: PLS+1st Der+FD, right
The original spectral data of Calibration is pre-processed, and with coefficient of determination R2It is identification index with RMSECV, it is pre- to spectrum
Processing result is identified；
E, it builds the selection for touching wave band: being established in stomach pill of aucklandia and amomum fruit condensed pill water extraction process using Partial Least Squares PLS
The Quantitative Analysis Model of aurantiamarin, aurantiamarin model modeling spectral coverage are 4084.49~11574.66cm-1, magnolol model modeling
Spectral coverage is 4447.00~9257.53cm-1, relative density model modeling spectral coverage is 4564.00~10254.00cm-1；
F, the selection of number of principal components: the selection of principal component has a great impact to the prediction result of model, when selected
When principal component is excessive, model includes excessive measurement noise, over-fitting occurs；When principal component is very few, and it will lead to modeling
Information is not complete, and predictive ability is poor, and the PLS factor is 9, RMSECV minimum, to model number of principal components；
G, model is established with the PLS method in TQAnalyst8.0 software, PLS+1st Der+FD is carried out to spectrum and is located in advance
Reason, using 4084.49~1174.66cm-1Wave band, 9 number of principal components are modeled, the R of established aurantiamarin model2=
0.99899, RMSECV=0.00125, RMSEP=0.00130；
PLS+1st Der+FD pretreatment is carried out to spectrum, using 4084.49~11574.66cm-1Wave band, 9 principal components
Number is modeled, the R of established magnolol model2=0.99899, RMSECV=0.00125, RMSEP=0.00130；
PLS+1st Der+FD pretreatment is carried out to spectrum, using 4084.49~11574.66cm-1Wave band, 9 principal components
Number is modeled, the R of established relative density model2=0.99899, RMSECV=0.00125, RMSEP=0.00130；
3., the verifying of calibration model:
By in the NIRS map input calibration model of 24 parts of verifying collection samples, and by NIRS predicted value and HPLC reference value into
The related monitoring of row, measures the variation of the relative density of its coverage area, realizes the monitoring to concentration process quality, guarantee product matter
Amount.
The near infrared spectrometer is 6700 type near infrared spectrometers of U.S. ThermoNicole company.
The high performance liquid chromatograph is Waters2695 type high performance liquid chromatograph.
It can be seen from the above, a kind of stomach pill of aucklandia and amomum fruit condensed pill preparation process quality monitoring method of the present invention, has green, fast
It is fast, accurate, it is realized by following steps:
(1) foundation of calibration model: the sample that different water mention time and concentration time is acquired respectively, near infrared spectrum
Instrument is scanned, and acquires original spectral data, is distributed according to index component content, remaining using 4/5 sample as calibration set
Conduct verify collection, make verifying collection range be evenly distributed within calibration set content range.With TQ quantitative analysis software, to original
The preprocess method and wave band of spectroscopic data are selected, and obtain the characteristic spectrum information of aurantiamarin honokiol content, meanwhile,
Using the content for the aurantiamarin honokiol that HPLC method measurement correcting sample is concentrated, by the content data measured and Calibration
The characteristic spectrum information of middle aurantiamarin honokiol content combines, and establishes calibration model using PLS method；
(2) verifying of calibration model: by the NIRSS map of verification sample collection sample input calibration model, and by NIRS
Predicted value and HPLC reference value carry out correlation analysis.By the NIRSS predicted value of verification sample collection and utilize the orange of HPLC method measurement
The content of skin glycosides honokiol compares, and verifies to calibration model, and whether decision verification sample sets are out-of-bounds point, judges the mould
Whether type is capable of the content of the index ingredient of Accurate Prediction its coverage area.
Described stomach pill of aucklandia and amomum fruit (condensed pill) sample:
(1) water gets sample product: according to 2015 editions " Chinese Pharmacopoeia " one, take radix aucklandiae, dried orange peel, prepared RHIZOMA CYPERI with vinegar, the dried immature fruit of citron orange, stir-baked CORTEX MAGNOLIAE OFFICINALIS with rhizoma zingiberis recens juice,
Pogostemon cablin, appropriate ginger crush, and weigh radix aucklandiae 56g, dried orange peel 100g, prepared RHIZOMA CYPERI with vinegar, the dried immature fruit of citron orange, stir-baked CORTEX MAGNOLIAE OFFICINALIS with rhizoma zingiberis recens juice, wide in prescription ratio precision
Each 70g of wrinkled giant hyssop, ginger sets this 7 taste medicinal material in a round bottom flask, adds 10 times of amount distilled water, extracts volatile oil；Its dregs of a decoction is taken,
2h is decocted with jujube, Poria cocos, the tuber of pinellia, Radix Glycyrrhizae, the 5 taste medicinal material of Rhizoma Atractylodis Macrocephalae of same prescription ratio；In decocting extraction process, opened from boiling
Beginning timing, takes that extract sample primary every 10min, and each 15mL is added etc. immediately to get a test solution after every sub-sampling
The distilled water of amount supplies decoction liquor.Decocting for the first time terminates, and 10 times of amount distilled water progress second are added in the dregs of a decoction by regulation and decoct,
Decoct 2h.It samples in decocting extraction process according to upper method to get 24 parts of Aqueous extracts samples.3 batches of Aqueous extracts are prepared in this approach,
72 parts of Aqueous extracts samples are collected altogether.
(2) concentrating sample: mentioning Aqueous extracts obtained in process for water and be divided into 5 parts, every part of about 4000mL, using Conventional concentration
Method carries out heating under reduced pressure concentration under the conditions of temperature 60 C, vacuum degree 0.08-0.09MPa, is connected in concentration process by needle tubing
Plastic pipe on-line period is connect, each batch is respectively separated 5min, 7min, 9min, and 11min, 13min are sampled, and extracts every time
10mL is placed in tool plug centrifuge tube, spare.The extracting solution of 5 batches collects 99 parts of concentrate altogether.
The acquisition correction sample sets original spectral data: with 6700 type near-infrareds of ThermoNicole company, the U.S.
Spectrometer is scanned using air as reference sample, and background correction acquires spectrogram, using optical fiber transflector, resolution ratio 8cm-1, light path 2.0mm, scanning times 64 times, scanning range: 4000~12000cm-1, 20 DEG C of temperature, relative humidity 33%~
35%.It is scanned by above-mentioned experimental condition, each sample multiple scanning 3 times acquires averaged spectrum.Up to original spectral data
The Pretreated spectra is: water is proposed process and is located in advance using PLS+1st Der+FD to original spectral data
Reason, waveband selection is 4 084.49~11 574.66cm-1；Concentration process is using PLS+1st Der+FD to original spectral data
It is pre-processed, waveband selection is 4 084.49~11 574.66cm-1。
The content of the aurantiamarin honokiol concentrated using HPLC method measurement correcting sample:
1), chromatographic condition: aurantiamarin HPLC chromatogram condition are as follows: Waters2695 type efficient liquid phase chromatographic analysis,
Symmetry C18 chromatographic column (4.6mm × 150mm, 5 μm), mobile phase: acetonitrile: water (67:33), column temperature: 30 DEG C, sample volume 10
μ L, flow velocity 1mLmin-1, Detection wavelength 225nm.
Magnolol HPLC chromatogram condition are as follows: Waters2695 type efficient liquid phase chromatographic analysis, Symmetry C18 chromatographic column
(4.6mm × 150mm, 5 μm), mobile phase: acetonitrile: water: glacial acetic acid (62:37:1), column temperature: 30 DEG C, 10 μ L of sample volume, flow velocity
1mL·min-1, Detection wavelength 284nm.
2), the preparation of reference substance solution: it is appropriate that precision weighs aurantiamarin, magnolol reference substance, is respectively placed in 10mL capacity
In bottle, adds methanol to dissolve and be settled to scale, solution of every 1mL containing 49 μ g of reference substance, 60 μ g, 0.45 μm of miillpore filter mistake is made
Filter to get；
3), sample measures: accurate respectively to draw reference substance solution and each 20 μ L injection high performance liquid chromatography of test solution
Instrument, measurement, the correcting sample up to HPLC measurement concentrate aurantiamarin, Determination of Magnolol.
The present invention is that applicant crystallizes through scientific research, test and to the creative work that practice summary is made, and warp is more
Secondary test repeatedly achieves identical and similar as a result, related physical resource is as follows:
The stomach pill of aucklandia and amomum fruit condensed pill is by radix aucklandiae 210g, fructus amomi 210g, Rhizoma Atractylodis Macrocephalae 300g, dried orange peel 300g, Poria cocos
300g, tuber of pinellia 300g processed, prepared RHIZOMA CYPERI with vinegar 210g, dried immature fruit of citron orange 210g, decladding cardamom 210g, stir-baked CORTEX MAGNOLIAE OFFICINALIS with rhizoma zingiberis recens juice 210g, Pogostemon cablin 210g, Radix Glycyrrhizae are fried
90g, ginger 90g and jujube 150g are made as Chinese medicine material, in which: by dried orange peel, prepared RHIZOMA CYPERI with vinegar, fry the dried immature fruit of citron orange, stir-baked CORTEX MAGNOLIAE OFFICINALIS with rhizoma zingiberis recens juice, the wide leaves of pulse plants
Fragrant, ginger and the radix aucklandiae of 80% weight extract volatile oil；The remaining dregs of a decoction and Rhizoma Atractylodis Macrocephalae, Poria cocos, Radix Glycyrrhizae, the system of jujube and 20% weight
The tuber of pinellia adds water to cook, filtration, and filtrate is condensed into the thick paste that 60 DEG C of relative densities are 1.35-1.40；Again by fructus amomi, decladding cardamom and
The remaining tuber of pinellia processed and radix aucklandiae are ground into medicinal powder；Medicinal powder, thick paste, volatile oil and maltose are mixed, pill, drying, polishing, as
Finished product stomach pill of aucklandia and amomum fruit condensed pill；In production, the quality for mentioning process and concentration process to water is monitored experiment；
1, the quality-monitoring experiment during water mentions:
1., the preparation of sample and test sample:
By radix aucklandiae 168g, dried orange peel 300g, prepared RHIZOMA CYPERI with vinegar 210g, fry dried immature fruit of citron orange 210g, stir-baked CORTEX MAGNOLIAE OFFICINALIS with rhizoma zingiberis recens juice 210g, Pogostemon cablin 210g and ginger
90g is crushed, this 7 taste medicinal material is set in a round bottom flask, adds 10 times of weight distilled water, extracts volatile oil；After extracting volatile oil
The dregs of a decoction are mixed with jujube 150g, Poria cocos 300g, tuber of pinellia 60g processed, Radix Glycyrrhizae 90g and Rhizoma Atractylodis Macrocephalae 300g again, and radix aucklandiae, old is added
Skin, prepared RHIZOMA CYPERI with vinegar fry the dried immature fruit of citron orange, stir-baked CORTEX MAGNOLIAE OFFICINALIS with rhizoma zingiberis recens juice, Pogostemon cablin, ginger, jujube, Poria cocos, the tuber of pinellia processed, Radix Glycyrrhizae and 10 times of Rhizoma Atractylodis Macrocephalae bulking value
Distilled water, the bulking value refer to solid in terms of g, and liquid is in terms of mL, and timing decocts 2h since boiling, takes every 10min
Sample is primary, each 15mL, and every 15mL is a test solution, and the distilled water that equivalent is added after every sub-sampling immediately supplies decoction
Liquid after decocting for the first time, adds radix aucklandiae, dried orange peel, prepared RHIZOMA CYPERI with vinegar, fries the dried immature fruit of citron orange, stir-baked CORTEX MAGNOLIAE OFFICINALIS with rhizoma zingiberis recens juice, Pogostemon cablin, ginger, jujube, Fu
Siberian cocklebur, the tuber of pinellia processed, Radix Glycyrrhizae and 10 times of Rhizoma Atractylodis Macrocephalae bulking value of distilled water carry out second and decoct, and timing decocts 2h since boiling, are decocting
It boils in extraction process and samples according to upper method to get 24 parts of Aqueous extracts samples, prepare 3 batches of Aqueous extracts in this approach, collect 72 parts altogether
Aqueous extracts sample；
2., establish calibration model, method is:
A, the acquisition of NIRS spectrum: near infrared spectrometer (6700 types of ThermoNicole company, the U.S.) to Aqueous extracts
Sample is scanned using air as reference, and background correction acquires spectrogram, using optical fiber transflector, resolution ratio 8cm-1, light path
2.0mm, scanning times 64 times, scanning range: 4000~12000cm-1, 20 DEG C of temperature, relative humidity 33%~35%.By above-mentioned
Experimental condition is scanned, and each sample multiple scanning 3 times acquires averaged spectrum, obtains original spectral data (institute as shown in figure 1
Show)；
B, the HPLC of aurantiamarin and Determination of Magnolol is measured in sample, and method is:
1), aurantiamarin HPLC chromatogram condition are as follows: high performance liquid chromatographs (Waters2695 type), SymmetryC18
Chromatographic column 4.6mm × 150mm, 5 μm, mobile phase is Yi Jing ︰ water=67 ︰ 33 of volume ratio, column temperature: 30 DEG C, 10 μ L of sample volume, is flowed
Fast 1mLmin-1, Detection wavelength 225nm；
Magnolol HPLC chromatogram condition are as follows: high performance liquid chromatograph (Waters2695 type), Symmetry C18 chromatographic column
4.6mm × 150mm, 5 μm, Yi Jing ︰ Shui ︰ glacial acetic acid=62 ︰ 37 ︰ 1 of the mobile phase for volume ratio, column temperature: 30 DEG C, 10 μ of sample volume
L, flow velocity 1mLmin-1, Detection wavelength 284nm；
2), the preparation of reference substance solution: precision weighs aurantiamarin, magnolol reference substance, is respectively placed in volumetric flask (such as 10mL
Volumetric flask) in, add methanol to dissolve, solution of every 1mL containing 49 μ g of reference substance, 60 μ g, 0.45 μm of filtering with microporous membrane is made；
3), sample measures: accurate respectively to draw reference substance solution and each 20 μ L injection high performance liquid chromatography of test solution
Instrument (HPLC) measurement, obtains aurantiamarin and Determination of Magnolol；
C, the selection of calibration set and verifying collection sample: according to the content distribution of aurantiamarin in sample, by 72 parts of samples of gained
It is divided into calibration set and verifying collection, wherein calibration set is 60 parts, 12 parts of verifying collection, and verifying collection range is made to be evenly distributed on calibration set
Within content range, the content distribution range such as table 3 of calibration set and verifying collection aurantiamarin, magnolol:
3 calibration set of table and verifying collection sample content distribution
D, the selection of preprocessing procedures: when near infrared spectrometer acquires spectrum, since external environment, instrument work
The difference of state, sample physical property can cause bigger influence to the foundation of model, by being pre-processed most to spectrum
The reduction of limits influences, and to establish accurate model, accordingly, preprocessing procedures are: using first derivative, second order
The primary light of derivative, smoothing processing, one of multiplicative scatter correction, standard normalization method or a variety of combinations to Calibration
Modal data is pre-processed, and with the coefficient of determination (R2) and RMSECV be performance assessment criteria, Pretreated spectra result is identified,
PLS+1st Der+FD is the best preprocess method of aurantiamarin model；PLS+2nd Der is the magnolol model most preferably side of pretreatment
Method is specifically shown in Table 4:
The selection of 4 different pretreatments method of table
E, it builds the selection for touching wave band: stomach pill of aucklandia and amomum fruit (condensed pill) water extraction process is established using Partial Least Squares PLS
The Quantitative Analysis Model of middle aurantiamarin, when establishing near-infrared diffusing reflection spectrum qualitative analysis model, the selection pair of spectrum
Modeling effect has a significant impact, it is generally the case that wider spectral region is selected model can be ensured to greatest extent to various
The pollution or the enough sensitivities of interference being likely to occur；With R2It is index with RMSECV, different spectral coverages is in optimized selection, orange
It is 4084.49~11574.66cm that skin glycosides, which models wave band,-1Spectral coverage, it is 5467.00~11357.04cm that magnolol, which models spectral coverage,-1,
R2Closest to 1, RMSECV minimum, optimum choice test result is shown in Table 5,
Table 5 models influence of the wave band to model
F, the selection of number of principal components: the selection of principal component has a great impact to the prediction result of model.When selected
When principal component is excessive, model includes excessive measurement noise, over-fitting occurs；When principal component is very few, and it will lead to modeling
Information is not complete, and predictive ability is poor, and accordingly, aurantiamarin is established in model, and when the PLS factor is 9, RMSECV minimum, this is aurantiamarin
Best modeled number of principal components；In magnolol model foundation, when the PLS factor is 9, RMSECV minimum, this is magnolol best modeled
Number of principal components, as shown in Figure 2；
G, aurantiamarin model is established with the PLS method in TQAnalyst8.0 software, PLS+1st Der+ is carried out to spectrum
FD pretreatment, using 4084.49~11574.66cm-1Wave band, 9 number of principal components are modeled, the R of established model2=
0.99899, RMSECV=0.00125, RMSEP=0.00130；Cortex Magnoliae Officinalis is established with the PLS method in TQAnalyst8.0 software
Phenol model carries out PLS+2nd Der pretreatment to spectrum, using 5467.00~11357.04cm-1Wave band, 9 number of principal components into
Row modeling, the R of established model2=0.97998, RMSECV=0.00122, RMSEP=0.00139；Stomach pill of aucklandia and amomum fruit concentration
The NIRS predicted value of aurantiamarin honokiol figure related to reference value is shown in Fig. 3 in ball water extraction process, as can be seen from the figure
The NIRS predicted value and reference value of two kinds of index ingredients are close, and the model established can be used for stomach pill of aucklandia and amomum fruit condensed pill water and mention
The quantitative analysis of aurantiamarin and magnolol during taking；
3., the verifying of calibration model:
By in the NIRS map input calibration model of 12 parts of verifying collection samples, and by NIRS predicted value and HPLC reference value into
The related identification of row, the results are shown in Table 6；As seen from table: the NIRS predicted value of 12 parts of verifying collection samples connects compared with the reference value of HPLC
Closely, aurantiamarin prediction related coefficient and prediction mean square deviation are respectively 0.9971,0.0016；Magnolol prediction related coefficient and prediction
Mean square deviation is respectively 0.9872,0.0023, which is capable of the aurantiamarin of Accurate Prediction its coverage area and the content of magnolol.
The near-infrared model predicted value of 6 12 parts of table verifying collection samples
(3), the concentration process of stomach pill of aucklandia and amomum fruit condensed pill
1., the preparation of sample and test sample: choose 5 parts of Aqueous extracts, every part of 4000mL 1. prepared by step (2), use
Conventional concentration method carries out heating under reduced pressure concentration under the conditions of temperature 60 C, vacuum degree 0.08-0.09MPa, leads in concentration process
Needle tubing connection plastic pipe on-line period is crossed, each batch is respectively separated 5min, 7min, 9min, and 11min, 13min sampling are primary,
It extracts 10mL every time to be placed in tool plug centrifuge tube, the extracting solution of 5 batches collects 99 parts of concentrate altogether；
2., establish calibration model:
A, the acquisition of NIRS spectrum: near infrared spectrometer (6700 types of ThermoNicole company, the U.S.) to concentrate
Sample is scanned using air as reference, and background correction acquires spectrogram, using optical fiber transflector, resolution ratio 8cm-1, light path
2.0mm, scanning times 64 times, scanning range: 4000~12000cm-1, 24 DEG C of temperature, humidity 42%~45%.By above-mentioned test
Condition is scanned, and each sample multiple scanning 3 times acquires averaged spectrum, obtains original spectral data (as shown in fig. 1)；
B, the HPLC of aurantiamarin and Determination of Magnolol is measured in sample
1), aurantiamarin HPLC chromatogram condition are as follows: high performance liquid chromatograph (Waters2695 type), Symmetry C18 chromatography
Column 4.6mm × 150mm, 5 μm, mobile phase is volume ratio Yi Jing ︰ water=67 ︰ 33, column temperature: 30 DEG C, 10 μ L of sample volume, flow velocity
1mL·min-1, Detection wavelength 225nm；
Magnolol HPLC chromatogram condition are as follows: high performance liquid chromatograph (Waters2695 type), Symmetry C18 chromatographic column
4.6mm × 150mm, 5 μm, mobile phase be volume ratio Yi Jing ︰ Shui ︰ glacial acetic acid=62 ︰, 37 ︰ 1, column temperature: 30 DEG C, 10 μ L of sample volume,
Flow velocity 1mLmin-1, Detection wavelength 284nm；
2), the preparation of reference substance solution: precision weighs aurantiamarin, magnolol reference substance, is respectively placed in 10mL volumetric flask,
Add methanol to dissolve and be settled to scale, solution of every 1mL containing 49 μ g of reference substance, 60 μ g is made, 0.45 μm of filtering with microporous membrane obtains
Reference substance solution；
3), sample measures: accurate respectively to draw reference substance solution and each 20 μ L injection high performance liquid chromatography of test solution
Instrument, measurement obtain the aurantiamarin and Determination of Magnolol of HPLC measurement；
C, in concentration process relative density measurement: according to 2015 editions " Chinese Pharmacopoeia " annex VII A relative density determinations
Bottle method measures in method；
D, the selection of calibration set and verifying collection sample: according to the content of aurantiamarin, magnolol and relative density in sample point
99 parts of samples of gained are divided into calibration set and verifying collect by cloth, are evenly distributed on verifying collection range within calibration set content range,
The content distribution range of calibration set and verifying collection aurantiamarin, magnolol and relative density is shown in Table 7:
7 calibration set of table and verifying collection sample content distribution
D, the selection of preprocessing procedures: when near infrared spectrometer acquires spectrum, since external environment, instrument work
The difference of state, sample physical property can cause bigger influence to the foundation of model, by being pre-processed most to spectrum
The reduction of limits influences, and to establish accurate model, the preprocessing procedures are: using first derivative, two
Order derivative, smoothing processing, one of the methods of multiplicative scatter correction, standard normalization method or a variety of combinations are to Calibration
Original spectral data pre-processed, and with the coefficient of determination (R2) and RMSECV be performance assessment criteria, to Pretreated spectra result
It is analyzed, the preprocess method of PLS+1st Der+FD is best as can be seen from Table 8；
The selection of 8 different pretreatments method of table
E, build the selection for touching wave band: test establishes the extraction of stomach pill of aucklandia and amomum fruit (condensed pill) water using Partial Least Squares PLS
The Quantitative Analysis Model of aurantiamarin in the process, during aurantiamarin model foundation, in 4084.49~11574.66cm-1Spectral coverage
In section, R2Closest to 1, RMSECV minimum, select this wave band as aurantiamarin best modeled wave band；Magnolol model foundation
In the process, in 4447.00~9257.53cm-1In spectral coverage section, R2Closest to 1, RMSECV minimum, select this wave band as
Magnolol best modeled wave band；It establishes in relative density model process, in 4564.00~10254.00cm-1In spectral coverage section, R2
Closest to 1, RMSECV minimum, selects this wave band as best modeled wave band in relative density model foundation, is shown in Table 9:
Table 9 models influence of the wave band to model
F, the selection of number of principal components: the selection of principal component has a great impact to the prediction result of model, when selected
When principal component is excessive, model includes excessive measurement noise, over-fitting occurs；When principal component is very few, and it will lead to modeling
Information is not complete, and predictive ability is poor, and Fig. 2 show influence of the number of principal components to PLS Quantitative Analysis Model RMSECV；When RMSECV most
Hour, selected number of principal components is best, as shown in Figure 2: when the PLS factor is 9, RMSECV minimum, for best modeled number of principal components；When
The PLS factor is 9, RMSECV minimum, is best modeled number of principal components；When the PLS factor is 9, RMSECV minimum, for best modeled master
Component number；
G, model is established with the PLS method in TQAnalyst8.0 software, PLS+1st Der+FD is carried out to spectrum and is located in advance
Reason, using 4084.49~1174.66cm-1Wave band, 9 number of principal components are modeled, the R of established aurantiamarin model2=
0.99899, RMSECV=0.00125, RMSEP=0.00130；
PLS+1st Der+FD pretreatment is carried out to spectrum, using 4084.49~11574.66cm-1Wave band, 9 principal components
Number is modeled, the R of established magnolol model2=0.99899, RMSECV=0.00125, RMSEP=0.00130；
PLS+1st Der+FD pretreatment is carried out to spectrum, using 4084.49~11574.66cm-1Wave band, 9 principal components
Number is modeled, the R of established relative density model2=0.99899, RMSECV=0.00125, RMSEP=0.00130；
NIRS predicted value and the reference of aurantiamarin, magnolol, relative density in stomach pill of aucklandia and amomum fruit condensed pill water extraction process
The related figure of value is shown in Fig. 3, and as can be seen from Figure 3 NIRS predicted value and reference value are close, which is respectively used to cyperus-amomum stomach
Ball condensed pill prepares the quantitative analysis of aurantiamarin in concentration process, magnolol, relative density；
3., the verifying of calibration model:
By in the NIRS map input calibration model of 24 parts of verifying collection samples, and by NIRS predicted value and HPLC reference value into
Row correlation analysis, aurantiamarin model verification result are shown in Table 10；As shown in Table 10: 24 parts verifying collection sample NIRS predicted value with
The reference value of HPLC relatively, R2It is respectively 0.9954,0.0019 with prediction mean square deviation RMSEP, which can be accurately pre-
Survey the content of the aurantiamarin of its coverage area；Magnolol model verification result is shown in Table 11, as shown in Table 11: 24 parts of verifyings collect sample
NIRS predicted value and HPLC reference value relatively, prediction related coefficient and prediction mean square deviation be respectively 0.9961,0.0016,
The model is capable of the content of the magnolol of Accurate Prediction its coverage area；Relative density model verification result is shown in Table 12, by table 12
Known to: relatively, prediction related coefficient and prediction are square for 24 parts of NIRS predicted values for verifying collection sample and the reference value of HPLC
Difference is respectively 0.9968,0.0017, which is capable of the variation of the relative density of Accurate Prediction its coverage area；
The near-infrared model predicted value of 10 24 parts of aurantiamarin verifying collection samples of table
The near-infrared model predicted value of 11 magnolol of table verifying collection sample
12 concentration process relative density near-infrared model predicted value of table
The present invention is mentioned and aurantiamarin honokiol in concentration process using HPLC measurement stomach pill of aucklandia and amomum fruit (condensed pill) water
Changes of contents rule, establishes and extracts terminal, establish water with Partial Least Squares combination near-infrared and mention and aurantiamarin in concentration process
The Quantitative Analysis Model of honokiol analyzes the monitoring of quality convenient for preparation process.Experimental result shows that is established quantifies
Analysis model can be used for stomach pill of aucklandia and amomum fruit (condensed pill) water and mention and the control of the quality of concentration process.
In conclusion the present invention is the method for stomach pill of aucklandia and amomum fruit (condensed pill) preparation process online quality control, it is nearly red
External spectrum technical application is monitored quality into the production process of stomach pill of aucklandia and amomum fruit (condensed pill), traditional Chinese medicine matter
Information digitalization and standardization are measured, provides a quick, lossless, free of contamination green method for traditional Chinese medicine quality monitoring, it can
Quickly, the content of Accurate Determining preparation process aurantiamarin honokiol, while quality testing cost is reduced, it reduces environmental pollution,
With significant economic and social benefit.
Claims (4)
1. a kind of stomach pill of aucklandia and amomum fruit condensed pill preparation process quality monitoring method, which is characterized in that different water are mentioned the time respectively
And the stomach pill of aucklandia and amomum fruit condensed pill sample of concentration time obtains sample with the near-infrared absorption spectrum of near infrared spectrometer scanning sample
This original spectral data goes out the content of Calibration aurantiamarin honokiol using high effective liquid chromatography for measuring, passes through finger
Mark property component content selection calibration set and verifying collection, then pre-process and are composed to spectroscopic data area's selection, contain what HPLC was measured
Amount is used as reference value, mutually ties Calibration characteristic spectrum with reference value with the Partial Least Squares method in Chemical Measurement
It builds vertical near infrared spectrum multivariate calibration model jointly, then model is verified；The NIRS map of verification sample collection sample is inputted
In calibration model, and NIRS predicted value and HPLC reference value are subjected to correlation analysis；By the NIRS predicted value of verification sample collection with
It is compareed using the content of the aurantiamarin honokiol of HPLC method measurement, calibration model is monitored, measurement verification sample collection is
It is no for out-of-bounds point, can in Accurate Determining coverage area index ingredient content, guarantee product quality.
2. stomach pill of aucklandia and amomum fruit condensed pill preparation process quality monitoring method according to claim 1, which is characterized in that including
Following steps:
(1), the stomach pill of aucklandia and amomum fruit condensed pill that different water mention time and concentration time is collected, the stomach pill of aucklandia and amomum fruit condensed pill is
By radix aucklandiae 210g, fructus amomi 210g, Rhizoma Atractylodis Macrocephalae 300g, dried orange peel 300g, Poria cocos 300g, tuber of pinellia 300g processed, prepared RHIZOMA CYPERI with vinegar 210g, fry the dried immature fruit of citron orange
210g, decladding cardamom 210g, stir-baked CORTEX MAGNOLIAE OFFICINALIS with rhizoma zingiberis recens juice 210g, Pogostemon cablin 210g, Radix Glycyrrhizae 90g, ginger 90g and jujube 150g are as Chinese medicine material
It is made, in which: by dried orange peel, prepared RHIZOMA CYPERI with vinegar, the radix aucklandiae extraction volatile oil for frying the dried immature fruit of citron orange, stir-baked CORTEX MAGNOLIAE OFFICINALIS with rhizoma zingiberis recens juice, Pogostemon cablin, ginger and 80% weight；
The tuber of pinellia processed of the remaining dregs of a decoction and Rhizoma Atractylodis Macrocephalae, Poria cocos, Radix Glycyrrhizae, jujube and 20% weight adds water to cook, and filters, and filtrate is condensed into 60 DEG C of phases
The thick paste for being 1.35-1.40 to density；Fructus amomi, decladding cardamom and the remaining tuber of pinellia processed and radix aucklandiae are ground into medicinal powder again；By medicine
Powder, thick paste, volatile oil and maltose mix, pill, drying, polishing, as finished product stomach pill of aucklandia and amomum fruit condensed pill；In production, right
Water proposes process and the quality of concentration process is monitored；
(2), the quality-monitoring during water mentions, comprising the following steps:
1., prepare test solution and Aqueous extracts sample:
By radix aucklandiae 168g, dried orange peel 300g, prepared RHIZOMA CYPERI with vinegar 210g, fry dried immature fruit of citron orange 210g, stir-baked CORTEX MAGNOLIAE OFFICINALIS with rhizoma zingiberis recens juice 210g, Pogostemon cablin 210g and ginger 90g
It crushes, this 7 taste medicinal material is set in a round bottom flask, add 10 times of weight distilled water, extract volatile oil；The dregs of a decoction after extracting volatile oil
It is mixed again with jujube 150g, Poria cocos 300g, tuber of pinellia 60g processed, Radix Glycyrrhizae 90g and Rhizoma Atractylodis Macrocephalae 300g, radix aucklandiae, dried orange peel, vinegar is added
Rhizoma cyperi fries the dried immature fruit of citron orange, stir-baked CORTEX MAGNOLIAE OFFICINALIS with rhizoma zingiberis recens juice, Pogostemon cablin, ginger, jujube, Poria cocos, the tuber of pinellia processed, Radix Glycyrrhizae and 10 times of Rhizoma Atractylodis Macrocephalae bulking value of distillation
Water, the bulking value refer to solid in terms of g, and liquid is in terms of mL, and timing decocts 2h since boiling, samples one every 10min
Secondary, each 15mL, every 15mL are a test solution, and the distilled water that equivalent is added after every sub-sampling immediately supplies decoction liquor,
For the first time decoct after, add radix aucklandiae, dried orange peel, prepared RHIZOMA CYPERI with vinegar, fry the dried immature fruit of citron orange, stir-baked CORTEX MAGNOLIAE OFFICINALIS with rhizoma zingiberis recens juice, Pogostemon cablin, ginger, jujube, Poria cocos,
The tuber of pinellia, Radix Glycyrrhizae and 10 times of Rhizoma Atractylodis Macrocephalae bulking value of distilled water processed carry out second and decoct, and timing decocts 2h since boiling, mentions in decoction
It samples during taking according to upper method to get 24 parts of Aqueous extracts samples, prepares 3 batches of Aqueous extracts in this approach, collect 72 parts of water altogether and mention
Liquid sample；
2., establish calibration model, method is:
A, the acquisition of NIRS spectrum: Aqueous extracts sample is scanned using air as reference near infrared spectrometer, background correction
Spectrogram is acquired, using optical fiber transflector, resolution ratio 8cm-1, light path 2.0mm, scanning times 64 times, scanning range: 4000~
12000cm-1, 20 DEG C of temperature, relative humidity 33%~35% is scanned by above-mentioned condition, each sample multiple scanning 3 times,
Averaged spectrum is acquired, original spectral data is obtained；
B, the HPLC of aurantiamarin and Determination of Magnolol is measured in Aqueous extracts sample, and method is:
1), aurantiamarin HPLC chromatogram condition are as follows: high performance liquid chromatograph, Symmetry C18 chromatographic column 4.6mm × 150mm, 5 μ
M, Yi Jing ︰ water=67 ︰s 33 of the mobile phase for volume ratio, column temperature: 30 DEG C, sample volume 10 μ L, flow velocity 1mLmin-1, Detection wavelength
225nm；
Magnolol HPLC chromatogram condition are as follows: high performance liquid chromatograph, Symmetry C18 chromatographic column 4.6mm × 150mm, flow by 5 μm
Dynamic is mutually Yi Jing ︰ Shui ︰ glacial acetic acid=62 ︰, 37 ︰ 1 of volume ratio, column temperature: 30 DEG C, sample volume 10 μ L, flow velocity 1mLmin-1, detection
Wavelength 284nm；
2), the preparation of reference substance solution: precision weighs aurantiamarin, magnolol reference substance, is respectively placed in volumetric flask, adds methanol molten
Solution, is made solution of every 1mL containing 49 μ g of reference substance, 60 μ g, 0.45 μm of filtering with microporous membrane obtains reference substance solution；
3), Aqueous extracts sample measures: accurate respectively to draw reference substance solution and each 20 μ L injection high-efficient liquid phase color of Aqueous extracts sample
Spectrometer measurement, obtains aurantiamarin and Determination of Magnolol；
C, the selection of calibration set and verifying collection sample: according to the content distribution of aurantiamarin in sample, 72 parts of samples of gained are divided into
Calibration set and verifying collection, wherein calibration set is 60 parts, 12 parts of verifying collection, and verifying collection range is made to be evenly distributed on calibration set content
Within the scope of, in which:
Aurantiamarin: calibration set, maximum value 1.255%, minimum value 0.651%, average value 0.953%；Verifying collection, maximum value
1.250%, minimum value 0.775%, average value 1.013%；
Magnolol: calibration set, maximum value 0.297%, minimum value 0.070%, average value 0.184%；Verifying collection, maximum value
0.292%, minimum value 0.075%, average value 0.184%；
D, the selection of preprocessing procedures: the difference of the physical properties such as particle size, uniformity of sample and measuring condition
The acquisition that will influence near infrared spectrum, leads to spectrum drift, the pretreatment of spectrum can purify spectrogram, reduce spectrum drift,
Reduce random noise, improves the robustness of near-infrared model；Quantitative model is square with cross-validation coefficient R 2, correction
Poor RMSEC, prediction mean square deviation RMSEP are that overall target evaluates model, and R2 illustrates sample chemical value and close closer to 1
Infrared predicted value correlation is better, and RMSEC, RMSEP are smaller, illustrates that the estimated performance of model is better, using different pretreatments
Method is investigated, and is selected optimal combination to carry out the foundation of model, is obtained aurantiamarin and magnolol near-infrared quantitative model most
Good preprocess method is respectively PLS+1st Der+FD, PLS+2nd Der；
E, it builds the selection for touching wave band: orange peel in stomach pill of aucklandia and amomum fruit condensed pill water extraction process is established using Partial Least Squares PLS
The Quantitative Monitoring model of glycosides, with R2It is index closest to 1 and RMSECV, different spectral coverages is in optimized selection, aurantiamarin is built
Mould wave band is 4084.49~11574.66cm-1Spectral coverage, it is 5467.00~11357.04cm that magnolol, which models spectral coverage,-1；
F, the selection of number of principal components: the selection of principal component has a great impact to the prediction result of model, when it is selected it is main at
When dividing excessive, model includes excessive measurement noise, over-fitting occurs；When principal component is very few, and it will lead to modeling information
Incomplete, predictive ability is poor, and accordingly, aurantiamarin is established in model, and the number of principal components PLS factor is 9, be aurantiamarin best modeled it is main at
Score；In magnolol model foundation, the number of principal components PLS factor is 9, is magnolol best modeled number of principal components；
G, aurantiamarin model is established with the PLS method in TQAnalyst8.0 software, it is pre- to carry out PLS+1st Der+FD to spectrum
Processing, using 4084.49~11574.66cm-1Wave band, 9 number of principal components are modeled, the R of established model2=
0.99899, RMSECV=0.00125, RMSEP=0.00130；Cortex Magnoliae Officinalis is established with the PLS method in TQAnalyst8.0 software
Phenol model carries out PLS+2nd Der pretreatment to spectrum, using 5467.00~11357.04cm-1Wave band, 9 number of principal components into
Row modeling, the R of established model2=0.97998, RMSECV=0.00122, RMSEP=0.00139；
3., the verifying of calibration model:
The NIRS map of 12 parts of verifying collection samples is inputted in calibration model, and NIRS predicted value and HPLC reference value are subjected to phase
Identification is closed, aurantiamarin prediction related coefficient and prediction mean square deviation are respectively 0.9971,0.0016；Magnolol prediction related coefficient with
It predicts that mean square deviation is respectively 0.9872,0.0023, measures the content of aurantiamarin and magnolol；
(3), the monitoring of the concentration process quality of stomach pill of aucklandia and amomum fruit condensed pill, method is:
1., the preparation of sample and test sample: choose 5 parts of Aqueous extracts 1. prepared by step (2), every part of 4000mL, using routine
Method for concentration carries out heating under reduced pressure concentration under the conditions of temperature 60 C, vacuum degree 0.08-0.09MPa, passes through needle in concentration process
Pipe connects plastic pipe on-line period, and each batch is respectively separated 5min, 7min, 9min, and 11min, 13min sampling are primary, every time
It extracts 10mL to be placed in tool plug centrifuge tube, the extracting solution of 5 batches collects 99 parts of concentrate altogether；
2., establish calibration model:
A, the acquisition of NIRS spectrum: concentrate sample is scanned using air as reference near infrared spectrometer, background correction
Spectrogram is acquired, using optical fiber transflector, resolution ratio 8cm-1, light path 2.0mm, scanning times 64 times, scanning range: 4000~
12000cm-1, 24 DEG C of temperature, humidity 42%~45% is scanned by above-mentioned experimental condition, each sample multiple scanning 3 times,
Averaged spectrum is acquired, original spectral data is obtained；
B, the HPLC of aurantiamarin and Determination of Magnolol is measured in sample:
1), aurantiamarin HPLC chromatogram condition are as follows: high performance liquid chromatograph, Symmetry C18 chromatographic column 4.6mm × 150mm, 5 μ
M, mobile phase be volume ratio Yi Jing ︰ water=67 ︰ 33, column temperature: 30 DEG C, sample volume 10 μ L, flow velocity 1mLmin-1, Detection wavelength
225nm；
Magnolol HPLC chromatogram condition are as follows: high performance liquid chromatograph, Symmetry C18 chromatographic column 4.6mm × 150mm, flow by 5 μm
Dynamic is mutually volume ratio Yi Jing ︰ Shui ︰ glacial acetic acid=62 ︰, 37 ︰ 1, column temperature: 30 DEG C, sample volume 10 μ L, flow velocity 1mLmin-1, detect wave
Long 284nm；
2), the preparation of reference substance solution: precision weighs aurantiamarin, magnolol reference substance, is respectively placed in 10mL volumetric flask, adds first
Alcohol dissolves and is settled to scale, and solution of every 1mL containing 49 μ g of reference substance, 60 μ g is made, and 0.45 μm of filtering with microporous membrane must compare
Product solution；
3), sample measures: it is accurate respectively to draw reference substance solution and each 20 μ L injection high performance liquid chromatograph of test solution, it surveys
It is fixed, obtain the aurantiamarin and Determination of Magnolol of HPLC measurement；
C, in concentration process relative density measurement: according to 2015 editions " Chinese Pharmacopoeia " annex VII A relative density determination methods
Middle bottle method measures relative density；
D, the selection of calibration set and verifying collection sample:, will according to the content distribution of aurantiamarin, magnolol and relative density in sample
99 parts of samples of gained are divided into calibration set and verifying collection, are evenly distributed on verifying collection range within calibration set content range, correct
The content distribution range of collection and verifying collection aurantiamarin, magnolol and relative density is as follows:
Calibration set and verifying collection sample content distribution
D, the selection of preprocessing procedures: when near infrared spectrometer acquires spectrum, due to external environment, instrument work shape
The difference of state, sample physical property can cause bigger influence to the foundation of model, maximum by carrying out pretreatment to spectrum
The reduction of limit influences, and to establish accurate model, accordingly, preprocessing procedures are: PLS+1st Der+FD, to school
The original spectral data of positive sample sets is pre-processed, and with coefficient of determination R2It is identification index with RMSECV, spectrum is located in advance
Reason result is identified；
E, it builds the selection for touching wave band: orange peel in stomach pill of aucklandia and amomum fruit condensed pill water extraction process is established using Partial Least Squares PLS
The Quantitative Analysis Model of glycosides, aurantiamarin model modeling spectral coverage are 4084.49~11574.66cm-1, magnolol model modeling spectral coverage
For 4447.00~9257.53cm-1, relative density model modeling spectral coverage is 4564.00~10254.00cm-1；
F, the selection of number of principal components: the selection of principal component has a great impact to the prediction result of model, when it is selected it is main at
When dividing excessive, model includes excessive measurement noise, over-fitting occurs；When principal component is very few, and it will lead to modeling information
Incomplete, predictive ability is poor, and the PLS factor is 9, RMSECV minimum, to model number of principal components；
G, model is established with the PLS method in TQAnalyst8.0 software, PLS+1st Der+FD pretreatment is carried out to spectrum, is adopted
With 4084.49~1174.66cm-1Wave band, 9 number of principal components are modeled, the R of established aurantiamarin model2=0.99899,
RMSECV=0.00125, RMSEP=0.00130；
PLS+1st Der+FD pretreatment is carried out to spectrum, using 4084.49~11574.66cm-1Wave band, 9 number of principal components into
Row modeling, the R of established magnolol model2=0.99899, RMSECV=0.00125, RMSEP=0.00130；
PLS+1st Der+FD pretreatment is carried out to spectrum, using 4084.49~11574.66cm-1Wave band, 9 number of principal components into
Row modeling, the R of established relative density model2=0.99899, RMSECV=0.00125, RMSEP=0.00130；
3., the verifying of calibration model:
The NIRS map of 24 parts of verifying collection samples is inputted in calibration model, and NIRS predicted value and HPLC reference value are subjected to phase
Monitoring is closed, the variation of the relative density of its coverage area is measured, realizes the monitoring to concentration process quality, guarantees product quality.
3. stomach pill of aucklandia and amomum fruit condensed pill preparation process quality monitoring method according to claim 2, which is characterized in that described
Near infrared spectrometer be U.S. ThermoNicole company 6700 type near infrared spectrometers.
4. stomach pill of aucklandia and amomum fruit condensed pill preparation process quality monitoring method according to claim 2, which is characterized in that described
High performance liquid chromatograph be Waters2695 type high performance liquid chromatograph.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910234079.7A CN109856084A (en) | 2019-03-26 | 2019-03-26 | A kind of stomach pill of aucklandia and amomum fruit condensed pill preparation process quality monitoring method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910234079.7A CN109856084A (en) | 2019-03-26 | 2019-03-26 | A kind of stomach pill of aucklandia and amomum fruit condensed pill preparation process quality monitoring method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN109856084A true CN109856084A (en) | 2019-06-07 |
Family
ID=66901994
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910234079.7A Withdrawn CN109856084A (en) | 2019-03-26 | 2019-03-26 | A kind of stomach pill of aucklandia and amomum fruit condensed pill preparation process quality monitoring method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109856084A (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111402989A (en) * | 2020-06-08 | 2020-07-10 | 江西汇仁药业股份有限公司 | Method for evaluating comprehensive quality of traditional Chinese medicine |
| CN111595816A (en) * | 2020-07-24 | 2020-08-28 | 江西中医药大学 | Method for distinguishing tablet coating end point based on near-infrared PCA analysis and application thereof |
| CN111665217A (en) * | 2020-06-09 | 2020-09-15 | 吉林省农业科学院 | Near infrared spectrum detection method for sucrose content of soybean seeds |
| CN111896497A (en) * | 2020-09-15 | 2020-11-06 | 四川长虹电器股份有限公司 | Spectral data correction method based on predicted value |
| CN112113929A (en) * | 2020-09-23 | 2020-12-22 | 鲁南制药集团股份有限公司 | Quality control method for extraction process of children's oral liquid for removing food retention and relieving cough |
| CN112964690A (en) * | 2021-02-04 | 2021-06-15 | 浙江工业大学 | Method for monitoring extraction process of traditional Chinese medicine formula particles in real time based on Raman spectrum |
Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101328162A (en) * | 2008-08-01 | 2008-12-24 | 中南大学 | Use of citrus aurtantium extract hydration meranzin for preparing gastrointestinal dynamic promoting drugs and preparation |
| CN102106939A (en) * | 2011-03-21 | 2011-06-29 | 江西汇仁药业有限公司 | Quality control method for extract concentrated liquor of condensed pills of six ingredients with rehmannia root |
| CN103033486A (en) * | 2012-11-23 | 2013-04-10 | 广东药学院 | Method for near infrared spectrum monitoring of quality of pericarpium citri reticulatae and citrus chachiensis hortorum medicinal materials |
| US20140319351A1 (en) * | 2013-04-25 | 2014-10-30 | Sumitomo Electric Industries, Ltd. | Inspection apparatus and an inspection method |
| CN104922639A (en) * | 2015-06-29 | 2015-09-23 | 李镇江 | Traditional Chinese medicine stomach-nourishing pill and preparation method thereof |
| JP2016160237A (en) * | 2015-03-03 | 2016-09-05 | 国立大学法人広島大学 | Methods for producing anti-leishmania compounds and anti-leishmania agents |
| CN106177858A (en) * | 2016-08-22 | 2016-12-07 | 上海典实医疗科技有限公司 | XIANGSHA YANGWEI WAN and preparation method thereof |
| CN107036998A (en) * | 2016-11-11 | 2017-08-11 | 辽宁华润本溪三药有限公司 | Utilize method and the application that volatile oil process is extracted in the preparation process of near infrared spectroscopy quick detection qizhi weitong granules |
| CN107137446A (en) * | 2017-07-07 | 2017-09-08 | 河南中医药大学 | The tripterygium wilfordii prepared slices of Chinese crude drugs that a kind of desmodium processes |
-
2019
- 2019-03-26 CN CN201910234079.7A patent/CN109856084A/en not_active Withdrawn
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101328162A (en) * | 2008-08-01 | 2008-12-24 | 中南大学 | Use of citrus aurtantium extract hydration meranzin for preparing gastrointestinal dynamic promoting drugs and preparation |
| CN102106939A (en) * | 2011-03-21 | 2011-06-29 | 江西汇仁药业有限公司 | Quality control method for extract concentrated liquor of condensed pills of six ingredients with rehmannia root |
| CN103033486A (en) * | 2012-11-23 | 2013-04-10 | 广东药学院 | Method for near infrared spectrum monitoring of quality of pericarpium citri reticulatae and citrus chachiensis hortorum medicinal materials |
| US20140319351A1 (en) * | 2013-04-25 | 2014-10-30 | Sumitomo Electric Industries, Ltd. | Inspection apparatus and an inspection method |
| JP2016160237A (en) * | 2015-03-03 | 2016-09-05 | 国立大学法人広島大学 | Methods for producing anti-leishmania compounds and anti-leishmania agents |
| CN104922639A (en) * | 2015-06-29 | 2015-09-23 | 李镇江 | Traditional Chinese medicine stomach-nourishing pill and preparation method thereof |
| CN106177858A (en) * | 2016-08-22 | 2016-12-07 | 上海典实医疗科技有限公司 | XIANGSHA YANGWEI WAN and preparation method thereof |
| CN107036998A (en) * | 2016-11-11 | 2017-08-11 | 辽宁华润本溪三药有限公司 | Utilize method and the application that volatile oil process is extracted in the preparation process of near infrared spectroscopy quick detection qizhi weitong granules |
| CN107137446A (en) * | 2017-07-07 | 2017-09-08 | 河南中医药大学 | The tripterygium wilfordii prepared slices of Chinese crude drugs that a kind of desmodium processes |
Non-Patent Citations (1)
| Title |
|---|
| 周琳琳: "一种香砂养胃丸浓缩丸制备过程质量监测方法", 《中国优秀硕士学位论文全文数据库 医药卫生科技辑》 * |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111402989A (en) * | 2020-06-08 | 2020-07-10 | 江西汇仁药业股份有限公司 | Method for evaluating comprehensive quality of traditional Chinese medicine |
| CN111402989B (en) * | 2020-06-08 | 2020-11-06 | 江西汇仁药业股份有限公司 | Method for evaluating comprehensive quality of traditional Chinese medicine |
| CN111665217A (en) * | 2020-06-09 | 2020-09-15 | 吉林省农业科学院 | Near infrared spectrum detection method for sucrose content of soybean seeds |
| CN111595816A (en) * | 2020-07-24 | 2020-08-28 | 江西中医药大学 | Method for distinguishing tablet coating end point based on near-infrared PCA analysis and application thereof |
| CN111595816B (en) * | 2020-07-24 | 2020-11-20 | 江西中医药大学 | Method for distinguishing tablet coating end point based on near-infrared PCA analysis and application thereof |
| CN111896497A (en) * | 2020-09-15 | 2020-11-06 | 四川长虹电器股份有限公司 | Spectral data correction method based on predicted value |
| CN111896497B (en) * | 2020-09-15 | 2022-04-08 | 四川长虹电器股份有限公司 | Spectral data correction method based on predicted value |
| CN112113929A (en) * | 2020-09-23 | 2020-12-22 | 鲁南制药集团股份有限公司 | Quality control method for extraction process of children's oral liquid for removing food retention and relieving cough |
| CN112964690A (en) * | 2021-02-04 | 2021-06-15 | 浙江工业大学 | Method for monitoring extraction process of traditional Chinese medicine formula particles in real time based on Raman spectrum |
| CN112964690B (en) * | 2021-02-04 | 2024-03-26 | 浙江工业大学 | Method for monitoring extraction process of traditional Chinese medicine formula particles in real time based on Raman spectrum |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN109856084A (en) | A kind of stomach pill of aucklandia and amomum fruit condensed pill preparation process quality monitoring method | |
| CN104237060B (en) | Multi-index quick detection method of honeysuckle | |
| CN104792652B (en) | A kind of Milkvetch Root multiple index quick detecting method | |
| CN108982720A (en) | The construction method of compound Ganmaoling Granules HPLC standard finger-print and application | |
| CN108241033B (en) | Method for rapidly detecting content of 6 quality index substances in radix ophiopogonis alcohol extract and application | |
| CN110907546B (en) | HPLC fingerprint detection method of traditional Chinese medicine for tonifying kidney and strengthening bone | |
| CN102106939A (en) | Quality control method for extract concentrated liquor of condensed pills of six ingredients with rehmannia root | |
| CN106018576A (en) | Establishment method for UPLC fingerprint spectrum of gynecological reconstruction pill | |
| CN108362788A (en) | A kind of steamed sealwort Quality Detection analysis method | |
| CN104568813A (en) | Multi-index fast detection method of dogwood medicinal materials | |
| CN108562657A (en) | The method of content of ginsenoside and application in a kind of quick detection red ginseng alcohol extract | |
| CN101664495A (en) | On-line detection method of near infrared spectrum for production process of traditional Chinese medicine, pill of six ingredients with rehmannia | |
| CN108051396A (en) | A kind of rapid detection method of Xin Ke Shu ' tablet for treating coronary heart disease active constituent content | |
| CN113281439B (en) | Quality control detection method of Shenbao tablets | |
| CN105911161A (en) | Anti-inflammatory tablet HPLC fingerprint construction method | |
| Chen et al. | Determination of marker constituents in radix Glycyrrhizae and radix Notoginseng by near infrared spectroscopy | |
| CN102106950B (en) | Quality control method in NuJin capsule extraction and concentration process | |
| CN114858934A (en) | Method for measuring 5-hydroxymethylfurfural and acrylamide in different processing processes of polygonatum sibiricum | |
| CN105784951B (en) | A kind of Liuwei Dihuang Wan condensed pill crude drug powder multiple index quick detecting method | |
| CN110346323B (en) | Method for detecting Huagaisan concentrated solution on line based on near infrared spectrum technology | |
| CN110007031B (en) | Fingerprint detection method of glossy privet fruit roasted with liquorice juice | |
| CN104833751B (en) | The method for building up of XIAOER GANMAO TANGJIANG Aqueous extracts HPLC standard finger-print and application thereof | |
| Haibo et al. | Rapid determination of Panax ginseng by near-infrared spectroscopy | |
| CN107036997A (en) | Method and application using the preparation process of near infrared spectroscopy quick detection qizhi weitong granules | |
| CN102106956B (en) | Method for controlling quality of Shenbao mixture percolating fluid |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WW01 | Invention patent application withdrawn after publication | ||
| WW01 | Invention patent application withdrawn after publication |
Application publication date: 20190607 |