CN1403822A - In-situ detection of product quality index in Chinese medicine production process - Google Patents
In-situ detection of product quality index in Chinese medicine production process Download PDFInfo
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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
- G01N2021/3595—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light using FTIR
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2201/00—Features of devices classified in G01N21/00
- G01N2201/12—Circuits of general importance; Signal processing
- G01N2201/129—Using chemometrical methods
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- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
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Abstract
The present invention provides the in-situ detection of product quality index in Chinese medicine production process and relates to one Chinese medicine producing shop, where relevant technological parameters and quality indexex are in-situ detected directly. The shop is equipped with in-situ detection system, which needs no any sample from the technological process. The system is equipped with one near infrared spectrometer and one industrial control comdputer and its in-situ real-time analysis system adopting least-square method and neural network method can be used in predicting the quality indexes in the production and providing analysis data. The method may be used in different Chinese medicine production shops.
Description
Technical field
The invention belongs to product quality and detect, relate to product quality detection in the Chinese medicine production technology, especially relate to traditional Chinese medicine extraction workshop quality index on-line detection method in the traditional Chinese medicine extraction detachment process.
Background technology
Existing traditional Chinese medicine quality control model, generally be to select a certain index components of Chinese medicine or effective constituent, set up simple physicochemical identification, spectrum, chromatogram are differentiated, content assaying method carries out traditional Chinese medicine quality control, and the object of control generally only limits to semi-manufacture and finished product in Chinese crude drug, the Chinese medicine production run, to the effectively control of mass change situation shortage of Chinese medical extract in the Chinese medicine production process.This mainly is because the Chinese medicine production run lacks necessary quality determining method.At present, the Chinese medicine production run is especially extracted detachment process, does not have online detection means substantially, causes the unsurmountable blind spot of quality control.Therefore need a kind of can on-line detection method being used for quality control index is detected in real time.
Summary of the invention
The present invention relates to the quality control index of Chinese medicine extract be implemented online detection in the traditional Chinese medicine extraction workshop.This method comprises one group of extract demarcation sample and the one group of near infrared spectrum measured that at first obtains at least one intermediate steps in this technological process, and obtains and the corresponding quality control index value of each demarcation sample.Then set up corresponding to the be associated forecast model of the quality control index value of demarcating sample with near infrared spectrum., measure the near infrared spectrum that be subjected to sample in this technological process, utilize forecast model forecast quality controlling index value, determine to be subjected to the estimated value of the quality index of sample, carry out the online detection of quality thereafter.
Product of the present invention relates to Chinese medical extract.
One group of extract of the present invention is demarcated sample and is meant and adopts qualified medicinal material, operate and one group of sample of one or two above intermediate steps in the described technology that obtains according to standard practice instructions.
Intermediate steps in the technological process of the present invention comprises: extraction, Separation of Solid and Liquid, concentrate, refining, drying etc.Wherein said extracting method comprises the following a kind of method that is selected from: cold-maceration, temperature are soaked method, percolation, decocting method, circumfluence method, the way of distillation, pressurization leaching, decompression leaching, ultrasonic extraction, Microwave Extraction method, super critical extraction, counter-flow extraction method.Extraction solvent is selected for use: water, ethanol, wine, sherwood oil, ether, chloroform, acetone, fat oil, carbon dioxide, ethene, nitrous oxide etc.The extraction assistant is selected for use: acid, alkali, glycerine, surfactant, methyl alcohol, ethanol, isopropyl alcohol, ammonia, low boiling alkanes; Wherein said Separation of Solid and Liquid comprises the following a kind of method that is selected from: filtration method, centrifuge method; Wherein said concentrate comprises the following a kind of method that is selected from: normal pressure concentrates, concentrating under reduced pressure, film concentrate; The wherein said refining following a kind of method that is selected from that comprises: alcohol precipitation, depositing in water, refrigeration, film separation, column chromatography, adverse current chromatogram; Wherein said drying comprises the following a kind of method that is selected from: hyperthermia drying, decompression low temperature drying, freeze drying, radiant drying, microwave drying, spray drying.
Quality control index of the present invention comprises following index: total constituents, stream part become to be grouped into, monomer concentration, mixture concentration, relative density, concentration of alcohol, moisture, molecular weight distribution, turbidity.
The measurement of near infrared spectrum of the present invention is to carry out with ft-nir spectrometer.
Forecast model of the present invention is to be set up by offset minimum binary method or neural net method.
Per at least five minutes of the near infrared ray that is subjected to sample of the present invention once.
The present invention carries out the Chinese medicine workshop that online detection relates to, comprise: (1) first kind of device, this device is used for measuring the near infrared spectrum of at least one intermediate steps in this technology, measures spectrum and a near infrared mensuration spectrum that is subjected to sample thereby obtain one group of one group of near infrared demarcating sample.(2) second kinds of devices, this device are used for measuring the desired value that each demarcates sample.(3) and a computing machine that is fit to following computing: set up the forecast model that described demarcation sample near infrared spectrum and demarcation sample desired value interrelate; Measure spectrum according to forecast model and the near infrared that is subjected to sample and predict the desired value that this is subjected to sample.
Adopt the method for traditional Chinese medicine extraction quality index of the present invention on-line measurement,, eliminated the blind spot of traditional Chinese medicine extraction Quality Control the Quality Control that improves the Chinese medicine production run.Homogeneity of improving the quality of products and stability.Adopt near-infrared spectrum technique to carry out the Chinese medicine on-line determination, have fast, advantages such as original position, non-destructive.In conjunction with utilizing the information processing technology to set up the forecast model that is associated of quality control index value and near infrared spectrum, forecast quality controlling index value has solved the traditional Chinese medicine ingredients complexity, is difficult to carry out the difficult problem of the online detection of quality.
Description of drawings Fig. 1 is the process flow diagram of traditional Chinese medicine extraction separation plants.Fig. 2 is the synoptic diagram of on-line measurement.Fig. 3 demarcates sample near infrared detection figure.Fig. 4 is quality index value that records and the comparison of predicting according to this method that is subjected to the sample mass desired value.
Embodiment
By following examples also in conjunction with the accompanying drawings, the present invention will further clearly be described.
Embodiment one:
Referring to Fig. 1, be the process chart of traditional Chinese medicine extraction, undertaken by the different process route according to different herbal species.General extracting technique of Chinese medicine comprises extraction, Separation of Solid and Liquid, concentrated, refining, dry.
1. comprise when extracting and be selected from following a kind of extraction solvent: water, ethanol, wine, sherwood oil, ether, chloroform, acetone, fat oil, carbon dioxide, ethene, nitrous oxide.
2. comprise when extracting and be selected from following a kind of extraction assistant: acid, alkali, glycerine, surfactant, methyl alcohol, ethanol, isopropyl alcohol, ammonia, low boiling alkanes.
3. wherein said extraction comprises the following a kind of method that is selected from: cold-maceration, temperature are soaked method, percolation, decocting method, circumfluence method, the way of distillation, pressurization leaching, decompression leaching, ultrasonic extraction, Microwave Extraction method, super critical extraction, counter-flow extraction method.
4. wherein said Separation of Solid and Liquid comprises the following a kind of method that is selected from: filtration method, centrifuge method.
5. wherein said concentrate comprises the following a kind of method that is selected from: normal pressure concentrates, concentrating under reduced pressure, film concentrate.
6. the wherein said refining following a kind of method that is selected from that comprises: alcohol precipitation, depositing in water, refrigeration, film separation, column chromatography, adverse current chromatogram.
7. wherein said column chromatography comprises the following a kind of method that is selected from: macroreticular resin, polyamide, aluminium oxide, silica gel, sephadex.
8. wherein said drying comprises the following a kind of method that is selected from: hyperthermia drying, decompression low temperature drying, freeze drying, radiant drying, microwave drying, spray drying.
9. the selection of above each process procedure concrete grammar is generally carried out according to the characteristic of different Chinese medicines.As for the Chinese medicine that contains volatile oil, can select steam distillation, super critical extraction during extraction.Can adopt water extraction and alcohol precipitation method technology for the traditional Chinese medicine extraction separation that contains polysaccharide effective constituent, in case of necessity, can add with sephadex column separation and purification technology and make with extra care.Believe that for the professional person choose reasonable of technology and combination need not to be described in detail also and can carry out smoothly.
10. the selection of the concrete quality control index of above each process procedure, generally according to the existing research data of each prescription medicinal material, according to middle medical drugs theory, with monarch, minister, help, make that the characteristics of principle and each process procedure select that total constituents such as total alkaloid content, general flavone content, total polysaccharides content, total saponin content, total protein content, total anthraquinones content, total acid content, general coumarin content, stream part become to be grouped into, monomer concentration, mixture concentration, molecular weight distribution and relative density, concentration of alcohol, moisture, turbidity be as quality control index.
Embodiment two:
Referring to Fig. 2, be the synoptic diagram that is used for on-line measurement among the present invention, in the typical production technology of Chinese medicine, the Chinese medical extract of each time point of producing in each technological process is measured with near infrared.In embodiment of the present invention, used spectrometer is a ft-nir spectrometer, it is the spectrometer that a kind of design is used for measuring near infrared region, and the output of spectrometer is the spectroscopic data of absorption spectrum of the Chinese medical extract of tested each time point of technological process, and is that computing machine adopts.
1. the one group of near infrared that obtains one group of demarcation sample of at least one intermediate steps in the described technology is measured spectrum and quality index value.
2. spectrum pre-service: adopt that single order differential, second-order differential, vector normalization, straight line subtract each other, minimum maximum normalization, many times of scatter corrections, normal side-play amounts eliminate and single order differential smoothings and other disposal routes method such as combine is carried out pre-service to original near infrared spectrum.With the noise that is contained in effective removal original spectrum, factors such as reduction sample solvent improve the precision of prediction of model to the interference of spectrum.The method of correspondence is as last practical application prediction when being minimum by contrasting the internal chiasma checking mean square deviation RMSECV under the different preprocess methods, choosing RMSECV.
3. set up the forecast model that described quality index is associated with near infrared spectrum.
4. measure a near infrared spectrum that is subjected to sample of at least one intermediate steps in the described technology.Wherein once to per at least five minutes of the described described spectroscopic assay that is subjected to sample.
5. according to described forecast model and the described near infrared spectrum that is subjected to sample, determine to be subjected to the estimated value of the quality index of sample, carry out the online detection of Chinese medical extract quality index.
Data analysis:, need to use the suitable data analytical approach to handle near infrared spectrum data for making full use of the information that near infrared spectrum provides.Must will carry out relatedly earlier with multivariate calibration methods according to the measure spectrum of demarcating sample and quality index value, set up calibration model.Multivariate calibration methods commonly used has multiple linear regression (MLR), principal component regression (PCR), partial least squares regression (PLS), artificial neural network (ANN) etc.The present invention is an example with the PLS method, and data analysing method is described.Form the nominal data matrix with demarcating sample at the spectroscopic data that each wave number obtains, demarcate the quality index value of sample simultaneously and form the quality index data battle array.The PLS algorithm compresses dimensionality reduction by factorial analysis with the nominal data matrix, in dimensionality reduction, considered the effect of quality index data battle array, by rationally choosing to the major component variable, remove the component variable that contains interfering component and disturbing factor, only get and contain the recurrence of participating in mass parameter with the major component variable of quantity of information maximum, set up forecast model.
In order to assess the quality of calibration model, internal chiasma checking mean square deviation RMSECV and prediction mean square deviation RMSEP are 2 the most frequently used parameters
C wherein
iBe true value,
Be predicted value, n is the calibration set sample number, and the number of principal components that p is to use, m are checking collection sample numbers.When calculating RMSECV,
Adopting leaving-one method that whole correction data set are carried out cross validation calculates.And RMSEP to be the calibration model that will set up be used for predicting m independently sample (not in former calibration set) and comparative experiments value (C
i) and predicted value (
) and draw.The RMSEP value can be assessed the forecast quality and the robust performance of the calibration model of being set up.When calibration model is unstable, the RMSEP value will significantly increase, otherwise the RMSEP value will be also littler than RMSECV.
Embodiment three: the online detection of Chinese medicine industry macroreticular resin detachment process
With a plurality of alkaloids of the coptis serves as to investigate index, make the standard control method with efficient liquid phase chromatographic analysis, obtain the desired value of demarcating sample, by near infrared spectral range rationally chosen optimization with the original spectrum preprocess method, employing offset minimum binary algorithm has been set up the correlation model between near infrared spectrum and coptis alkaloid concentration, and predicts the elution curve of coptis alkaloid in macroreticular resin chromatography process with this.Method of the present invention can be measured a plurality of alkaloids content in the eluate simultaneously, and the testing process of each sample only needed to finish in 30 seconds, and precision of prediction meets the demands, and the result is referring to Fig. 3, Fig. 4.
Step:
1. collect the eluent of different elution time points and demarcate sample.
2. each alkaloid concentration of the coptis of eluent being demarcated in the sample with the RP-HPLC method is analyzed.
Chromatographic condition: chromatographic column: C
18Post 4.6 * 250mm, 5 μ m; Moving phase: acetonitrile-1%SDS aqueous solution 54: 46; Detect wavelength: 346nm;
3. with near-infrared method eluent being demarcated sample scans.
Immersing the optical fiber transmission-type probe that the NIR spectrometer carries during scanning optical spectrum in demarcating sample liquid, is reference with the air.Test condition: scanning times 32 times, resolution 8cm
-1, the scanning optical spectrum scope is 11000-4000cm
-1The near infrared light spectrogram is seen Fig. 3.
4. spectrum pre-service: the method for adopt that single order differential, second-order differential, vector normalization, straight line subtract each other, minimum maximum normalization, many times of scatter corrections, normal side-play amounts being eliminated and single order differential smoothings and other disposal routes combine is carried out pre-service to original near infrared spectrum.The result shows: original spectrum is carried out the single order differential handle, can purify the figure spectrum information effectively, seek out in the spectrum by the strong definite peak value scope that absorbs the little band that is covered.Jamaicin and two quality index of total alkaloids are further handled the single order differential and straight line subtractive method Combined Treatment, can be obtained more satisfactory calibration model; Jateorrhizine and two quality index of palmatine are further handled the single order differential and vector normalization Combined Treatment, can be obtained more satisfactory calibration model.
5. sample cross validation and predicted value
By contrast optimization, set up the calibration model of alkaloid concentration in the near infrared spectroscopy detection coptis macroreticular resin eluent with the offset minimum binary algorithm Return Law to modeling spectral coverage and original spectrum preprocess method.The model internal chiasma is verified and predicted the outcome and shows: the prediction effect to total alkaloids is best, secondly is jamaicin, is palmatine then, is jateorrhizine at last.
6. value of forecasting checking: the elution samples liquid of collecting different elution time points.Predict the quality index value of unknown sample collection with the model of being set up, and adopt the RP-HPLC method that each alkaloid concentration of the coptis in the elution samples liquid is carried out assay, measurement result and predicted value compare, with the reliability of checking forecast model.The results are shown in Table 1, Fig. 4.
Table 1 predicted value and measured value are relatively
HPLC records
The sample number into spectrum predicted value
Value
mg/ml mg/ml
1 0.729 1.366
2 11.135 11.410
3 22.637 21.955
4 17.044 18.880
5 11.119 12.520
6 7.026 7.758
7 4.825 4.952
8 2.609 2.741
9 1.954 1.441
10 1.61 0.599
11 0.751 0.325
Above example just is used to illustrate the present invention, and unrestricted the present invention.The present invention also can be applicable to various Chinese medicine production technologies, comprising: extraction, Separation of Solid and Liquid, concentrated, refining, dry.The quality index of online detection can part become to be grouped into for total alkaloid content, general flavone content, total polysaccharides content, total saponin content, total protein content, total anthraquinones content, total acid content, general coumarin content, stream, monomer concentration, mixture concentration, relative density, concentration of alcohol, moisture, molecular weight distribution, turbidity etc.
The online detection of product quality indicator in the Chinese medicine production technology provided by the invention, relate to one to directly and product quality related technical parameters and quality index implement the Chinese medicine workshop of online detection.An on-line detecting system that does not need to extract from technological process any sample material is equipped with in this workshop, and this system adopts the thermal resistance of a ft-nir spectrometer, industrial control computer, measurement temperature and measures the proportion instrument of relative density.Adopt the online in real time analytic system of offset minimum binary (PLS) and neural net method can predict the quality index of Chinese medicine production run, and data analysis is provided.This method can be used for different Chinese medicine workshops.
Need not further to elaborate, believe and adopt the disclosed content in front, those skilled in the art can use the present invention to greatest extent.Therefore, the various measuring methods of technological process, quality index and other similar change all belong to the scope of the invention.
Claims (10)
1. product quality indicator online test method in the Chinese medicine production technology, be the quality control index of Chinese medicine extract to be implemented online detection in the traditional Chinese medicine extraction workshop, it is characterized in that: this detection method comprises one group of extract demarcation sample and the one group of demarcation sample near infrared spectrum that records that at first obtains at least one intermediate steps in this technological process, and obtain and the corresponding quality control index value of each demarcation sample, then set up corresponding to the be associated forecast model of the quality control index value of demarcating sample with near infrared spectrum, thereafter, measure the near infrared spectrum that is subjected to sample of at least one intermediate steps in this technological process, utilize forecast model forecast quality controlling index value, determine to be subjected to the estimated value of the quality index of sample, carry out the online detection of quality.
2. the online detection of product quality indicator in the Chinese medicine production technology as claimed in claim 1, it is characterized in that: described product is meant Chinese medical extract.
3. as claimed in claim 1ly obtain one group of extract and demarcate sample, it is characterized in that: adopt qualified medicinal material, operate and one group of sample of one or more intermediate steps in the described technology that obtains according to standard practice instructions.
4. the intermediate steps in the production technology as claimed in claim 3 is characterized in that: intermediate steps comprises extraction, Separation of Solid and Liquid, concentrates, refining, drying etc.
5. as Chinese medicine production technology as described in the claim 4, it is characterized in that: extracting method can be selected from following arbitrary method: cold-maceration, temperature is soaked method, percolation, decocting method, circumfluence method, the way of distillation, pressurization is leached, decompression is leached, ultrasonic extraction, the Microwave Extraction method, super critical extraction, the counter-flow extraction method, extraction solvent is selected for use: water, ethanol, wine, sherwood oil, ether, chloroform, acetone, fat oil, carbon dioxide, ethene, nitrous oxide etc., the extraction assistant is selected for use: acid, alkali, glycerine, surfactant, methyl alcohol, ethanol, isopropyl alcohol, ammonia, the low boiling alkanes, Separation of Solid and Liquid can be selected from following arbitrary method: filtration method, centrifuge method, concentrate and can be selected from following arbitrary method: normal pressure concentrates, concentrating under reduced pressure, film concentrates, make with extra care and to be selected from following arbitrary method: alcohol precipitation, depositing in water, refrigeration, film separates, column chromatography, adverse current chromatogram, drying can be selected from following arbitrary method: hyperthermia drying, the decompression low temperature drying, freeze drying, radiant drying, microwave drying, spray drying.
6. quality control index as claimed in claim 1 is characterized in that: index comprises that total constituents, stream part become to be grouped into, monomer concentration, mixture concentration, relative density, concentration of alcohol, moisture, molecular weight distribution, turbidity.
7. the measurement of near infrared spectrum as claimed in claim 1 is characterized in that: measure with near infrared spectrometer.
8. forecast model as claimed in claim 1 is characterized in that: this model is set up by offset minimum binary method or neural net method.
9. the near infrared ray that is subjected to sample as claimed in claim 1 is characterized in that: per at least five minutes of near infrared ray once.
10. the online detection of product quality indicator in the Chinese medicine production technology as claimed in claim 1, it is characterized in that: the Chinese medicine workshop device that online detection relates to comprises: (1) first kind of device, this device is used for measuring the near infrared spectrum of at least one intermediate steps in this technology, measures spectrum and a near infrared mensuration spectrum that is subjected to sample thereby obtain one group of one group of near infrared demarcating sample.(2) second kinds of devices, this device are used for measuring the desired value that each demarcates sample.(3) and a computing machine that is fit to following computing: set up the forecast model that described demarcation sample near infrared spectrum and demarcation sample desired value interrelate; Measure spectrum according to forecast model and the near infrared that is subjected to sample and predict the desired value that this is subjected to sample.
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