CN110320286A - The content assaying method of Xiao Chai Hu granules effective component - Google Patents
The content assaying method of Xiao Chai Hu granules effective component Download PDFInfo
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- 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
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Abstract
The present invention relates to a kind of content assaying methods of Xiao Chai Hu granules effective component: taking multiple Xiao Chai Hu granules samples as calibration set, computerized near infrared scan obtains the original spectral data of calibration set；Pretreated spectra selects the modeling wave band of effective component, obtains content characteristics spectrum；The effective component of multiple Xiao Chai Hu granules samples is measured respectively using high performance liquid chromatography, obtains content true value；Content characteristics spectrum, content true value are associated using Partial Least Squares, establish normalization model；Xiao Chai Hu granules to be measured are taken, computerized near infrared scan obtains the original spectral data of the Xiao Chai Hu granules to be measured；The original spectral data of the Xiao Chai Hu granules sample to be measured is imported into normalization model, is calculated through normalization model, obtains the content of effective component.Near infrared spectrum is applied to Xiao Chai Hu granules active constituent content measuring for the first time by the present invention, and detection speed is fast, high-efficient, inspection cost, environmental pollution, better reproducibility.
Description
Technical field
The present invention relates to quality control technologies for traditional Chinese medicine fields, more particularly to small radix bupleuri granular agent effective component containing measurement
Determine method.
Background technique
Chinese herbal granules are " to mean material medicine and fit according to the definition of the Pharmacopoeia of the People's Republic of China (version in 2015)
Suitable auxiliary material is mixed and made into the dry granular formulation with certain particle size." compound preparation Xiao Chai Hu granules are by radix bupleuri, Huang
A kind of reed mentioned in ancient books, pinellia, Radix Codonopsis, ginger, Radix Glycyrrhizae and jujube is extracted refines, have the effect of inducing diaphoresis heat dissipation, soothing liver and harmonizing stomach.For
Exterior syndrome, invasion of SHAO YANG by pathogen card symptoms include fevers and chills alternate, fullness and discomfort in chest and hypochondrium, loss of appetite, vexation and vomiting, bitter taste in the mouth and dry throat.Xiao Chai Hu granules
Agent is administered orally after dissolving, and product is accurate with dosage, it is rapid to dissolve, is convenient for absorption, is rapid-action, in good taste, carrying preservation
Conveniently, the features such as dose is small, property is stablized.
Xiao Chai Hu granules at present mainly evaluate using scutelloside as it by " Chinese Pharmacopoeia " existing quality control assay
Index studies the measurement of the more major quality controlling ingredient saikosaponin a for further including the radix bupleuri in Xiao Chai Hu granules at present,
But traditional scutelloside, saikosaponin a detection method of content majority are efficient liquid phase method, need to often be carried out to sample many and diverse pre-
Processing, time and effort consuming, minute is longer, and detection process expends a large amount of reagent, and environmental pollution is larger, and to inspector
Body is damaged, information feedback lag, in preparation production, it is difficult to meet multiple batches of quick measurement and on-line checking
It is required that.Since Chinese medicine type is more, complex chemical composition, quality controls very big.
It would therefore be highly desirable to provide a kind of content assaying method of the effective component of simple, quick Xiao Chai Hu granules.
Summary of the invention
Based on this, the object of the present invention is to provide a kind of content assaying methods of small radix bupleuri granular agent effective component, this contains
The disadvantages of quantity measuring method is simple, quick, can overcome prior art time and effort consuming, low efficiency.
A kind of content assaying method of Xiao Chai Hu granules effective component, includes the following steps:
(1) take multiple Xiao Chai Hu granules samples as calibration set, computerized near infrared scan obtains the original spectrum number of calibration set
According to；
(2) Pretreated spectra is carried out to the original spectral data of the calibration set, and selects the modeling wave band of effective component,
Obtain the content characteristics spectrum of the effective component；
(3) effective component of the multiple Xiao Chai Hu granules sample is surveyed respectively using high performance liquid chromatography
It is fixed, obtain the content true value of the effective component；
(4) using Partial Least Squares to content true value obtained by content characteristics spectrum, step (3) obtained by step (2) into
Row association, establishes the normalization model of the effective component；
In wherein some embodiments, the effective component is at least one of saikosaponin a, scutelloside.
In wherein some embodiments, the effective component is saikosaponin a, then in step (2):
For the method that Pretreated spectra uses for multiplicative scatter correction, modeling wave band is 4083~7486cm-1；Alternatively,
For the method that Pretreated spectra uses for standard normalization, modeling wave band is 4138~7289cm-1；Alternatively,
For the method that Pretreated spectra uses for first derivative, modeling wave band is 4138~7289cm-1；Alternatively,
The method that Pretreated spectra uses adds vector to normalize for first derivative, and modeling wave band is 4200~7500cm-1；Or
Person,
For the method that Pretreated spectra uses for second dervative, modeling wave band is 4200~7500cm-1。
In wherein some embodiments, in step (2), the method that Pretreated spectra uses models wave band for first derivative
For 4138~7289cm-1；Alternatively,
The method that Pretreated spectra uses adds vector to normalize for first derivative, and modeling wave band is 4200~7500cm-1；Or
Person,
For the method that Pretreated spectra uses for second dervative, modeling wave band is 4200~7500cm-1。
In wherein some embodiments, in step (2), the method that Pretreated spectra uses adds vector normalizing for first derivative
Change, modeling wave band is 4200~7500cm-1。
In wherein some embodiments, the effective component is scutelloside, then in step (2):
For the method that Pretreated spectra uses for multiplicative scatter correction, modeling wave band is 4000~5500cm-1；Alternatively,
For the method that Pretreated spectra uses for standard normalization, modeling wave band is 4000~5500cm-1；Alternatively,
For the method that Pretreated spectra uses for first derivative, modeling wave band is 4138~5432cm-1；Alternatively,
The method that Pretreated spectra uses adds vector to normalize for first derivative, and modeling wave band is 4538~5294-1；Or
Person,
For the method that Pretreated spectra uses for second dervative, modeling wave band is 4538~5294cm-1。
In wherein some embodiments, in step (2):
For the method that Pretreated spectra uses for first derivative, modeling wave band is 4138~5432cm-1；Alternatively,
The method that Pretreated spectra uses adds vector to normalize for first derivative, and modeling wave band is 4538~5294-1；Or
Person,
For the method that Pretreated spectra uses for second dervative, modeling wave band is 4538~5294cm-1。
In wherein some embodiments, in step (2):
For the method that Pretreated spectra uses for second dervative, modeling wave band is 4538~5294cm-1。
In wherein some embodiments, step (4) also verifies gained normalization model, comprising:
Take multiple Xiao Chai Hu granules samples as verifying collection, computerized near infrared scan obtains the original spectral data of verifying collection；
The original spectral data of the verifying collection is poured into the normalization model, calculates, obtains through normalization model
Verifying collection effective component predicted value；
It is detected using the effective component of the high performance liquid chromatography to verifying collection, it is true that collection effective component must be verified
Value；
Analyze the verifying collection effective component predicted value and verifying collection effective component true value.
In wherein some embodiments, the condition using computerized near infrared scan includes: resolution ratio 8cm-1, scanning optical spectrum range
4000~10000cm-1, scanning times 32 times, ambient temperature, relative humidity 30~40%.
Compared with prior art, the present invention have it is following the utility model has the advantages that
Near infrared spectrum is applied to Xiao Chai Hu granules active constituent content measuring for the first time by the present invention, and this method is according to be checked
Effective component is surveyed, corresponding normalization model is established, especially can once establish the normalization mould of multiple effective components
Type is realized and carries out assay to Xiao Chai Hu granules plurality of active ingredients simultaneously, and detection speed is fast, generally can be complete in 2 minutes
At high-efficient；Also, without using chemical reagent quality inspection cost is greatly lowered, not to environment in the content assaying method
Cause any pollution；Due to the stability of spectral measurement, test result is seldom influenced by human factor, is measured with customary amount
Method is compared, and near infrared spectrum shows better reproducibility.
The present invention is mainly the assay that near infrared spectrum is applied to Xiao Chai Hu granules saikosaponin a, scutelloside, and
Accordingly select suitable Pretreated spectra method and corresponding modeling wave band, near-infrared spectral can not only be overcome to inhale
Receive the defects of intensity is weaker, spectrum signal-to-noise ratio is low, and overlapping occurs for frequency multiplication, sum band, effectively eliminate background noise and
Physical factor interference improves the phase relation between spectrogram and effective component, obtains best modeled effect, additionally it is possible to effective removal
It is special to obtain targetedly relatively narrow saikosaponin a, content of baicalin for the interference of non-targeted effective component in Xiao Chai Hu granules prescription
Levy spectrum, with the content characteristics spectrum construct normalization model, can more accurately predict saikosaponin a in sample to be tested,
The content of scutelloside, has well solved in Xiao Chai Hu granules that saikosaponin a content is relatively low, asking of being difficult to be determined accurately
Topic, detection accuracy is high, has taken into account the Simultaneous Determination of low content saikosaponin a, high-content scutelloside on the whole.
Detailed description of the invention
The original infrared spectrogram of Fig. 1, small radix bupleuri granular agent；
The original infrared spectroscopy of Fig. 2, small radix bupleuri granular agent is through chromatogram obtained by polynary scattering preprocess method；
The original infrared spectroscopy of Fig. 3, small radix bupleuri granular agent is through spectrogram obtained by standard normalization preprocess method；
The original infrared spectroscopy of Fig. 4, small radix bupleuri granular agent is through spectrogram obtained by first derivative preprocess method；
The original infrared spectroscopy of Fig. 5, small radix bupleuri granular agent adds spectrogram obtained by vector normalization preprocess method through first derivative；
The original infrared spectroscopy of Fig. 6, small radix bupleuri granular agent is through spectrogram obtained by second dervative preprocess method；
Fig. 7, Xiao Chai Hu granules saikosaponin a predicted value, true value；
Fig. 8, Xiao Chai Hu granules scutelloside predicted value, true value.
Specific embodiment
Of the invention is described in further detail below in conjunction with specific embodiment.
Embodiment
The present embodiment provides a kind of content assaying methods of small radix bupleuri granular agent effective component, include the following steps:
(1) calibration set and original spectral data acquisition
The sample that 75 batches are acquired from small radix bupleuri granular agent, chooses representative from this 75 batch samples
65 batches of known content samples are calibration set, selection 10 batches is verifying collection, and sample comminution crosses 60 meshes；The small radix bupleuri granular agent is pressed
It is prepared according to the prescription in Pharmacopoeia of the People's Republic of China current edition " Xiao Chai Hu granules ", preparation method；Xiao Chai Hu granules batch
The acquisition of secondary sample uses blind choosing, as far as possible enhancement factor range of variation, has obtained representative calibration set.The present embodiment
The representative sample includes the small radix bupleuri granular agent sample of stable effective ingredients by HPLC test.Verifying collects
HPLC test, stable effective ingredients or unstable small radix bupleuri granular agent sample, it is mainly right after acquisition original spectrum
Calibration model plays verification the verifying results, if resulting predicted value differs greatly with true value after being input to calibration model, verifies
As a result poor for calibration model predictive ability, if resulting predicted value is approached with true after being input to calibration model, verify knot
Fruit is that calibration model has preferable predictive ability.
Using near infrared spectrometer acquisition correction collection original spectral data, the original near infrared spectrum of Xiao Chai Hu granules is obtained
Data；Wherein, near infrared spectrometer: II FT-NIR Analyzer Thermo Fischer Scient Inc. of Antaris, the U.S., light source；
Tungsten halogen lamp, detector: InGaAs, integrating sphere diffusing reflection acquisition system.
The condition of acquisition correction collection original spectral data includes: resolution ratio 8cm-1, scanning optical spectrum range 4000~
10000cm-1, scanning times 32 times, ambient temperature, relative humidity 30~40%.
(2) high performance liquid chromatograph detects scutelloside, saikosaponin a content
1) high performance liquid chromatograph is used, according to small radix bupleuri granular agent in Pharmacopoeia of the People's Republic of China version in 2015
Content of baicalin under in content determination of Baicalin method measurement sample；
Specific step is as follows:
Chromatographic condition and system suitability test: using octadecylsilane chemically bonded silica as filler；With methanol-water-phosphorus
Sour (47:53:0.2) is mobile phase；Detection wavelength is 315mm.Number of theoretical plate is calculated by scutelloside peak should be not less than 3000.
The preparation of reference substance solution: taking scutelloside reference substance appropriate, accurately weighed, adds 70% ethyl alcohol that every 1ml is made containing 60 μ
G solution to get.
The preparation of test solution: taking this product under content uniformity item, mixes, and takes in right amount, finely ground, takes about 3g, and precision claims
It is fixed, it sets in stuffed conical flask, 70% ethyl alcohol 50ml, close plug is added in precision, and weighed weight is ultrasonically treated (power 250W, frequency
It 50kHz) 30 minutes, lets cool, then weighed weight, the weight of less loss is supplied with 70% ethyl alcohol, is shaken up, filter, take subsequent filtrate, i.e.,
?.
Measuring method: accurate absorption reference substance solution and each 10 μ l of test solution respectively, injection liquid chromatograph, measurement,
To obtain the final product.
2) high performance liquid chromatograph is used, according under the Pharmacopoeia of the People's Republic of China general rule 0512 of version four in 2015
Method measures the saikosaponin a content in Xiao Chai Hu granules.
Specific step is as follows:
Chromatographic condition and system suitability test: using octadecylsilane chemically bonded silica as filler；With acetonitrile-water (45:
It 55) is mobile phase；Detection wavelength 203mm, number of theoretical plate is calculated by saikosaponin a peak should be not less than 5000.
The preparation of reference substance solution: taking saikosaponin a reference substance appropriate, accurately weighed, adds methanol that every 1ml is made containing radix bupleuri
The solution of saponin(e a 0.2mg, shake up to get.
The preparation of test solution: taking this product under content uniformity item, mixes, and takes in right amount, finely ground, takes about 1g, and precision claims
It is fixed, it sets in stuffed conical flask, water 50ml is added, ultrasonic treatment (power 200W, frequency 40kHz) makes it dissolve, adds water saturated
Extracting n-butyl alcohol 3 times, each 50ml, merge n-butanol liquid, water-bath volatilizes, and residue is transferred to 10ml measuring bottle with proper amount of methanol solution
In, add methanol dilution to shake up to scale, filter, take subsequent filtrate to get.
Measuring method: accurate absorption reference substance solution and each 10 μ l of test solution respectively, injection liquid chromatograph, measurement,
To obtain the final product.
(3) foundation of normalization model
The original spectral data for the calibration set that step (1) obtains is subjected to pretreatment and wavelength band selection, obtains small bavin
Scutelloside, saikosaponin a content characteristics spectrum in Hu granule；
Multiple calibration models are established to scutelloside, saikosaponin a in Xiao Chai Hu granules, with inclined in TQ quantitative analysis software
Least square (PLS) is associated with calculating with the standard content value of step (2) target component, establishes calibration model, and collect sample with verifying
Product carry out external certificate.
In order to eliminate the influence to the calibration results such as noise and baseline drift, the original absorbance spectrum of sample is located in advance
Reason.The R being calculated after distinct methods processing according to model2And RMSECV, R2For the calibration set cross-validation coefficient of determination；
RMSECV is calibration set cross-validation mean square deviation, and RMSEC is correction error root mean square.R2With RMSECV, LV, RMSEC, this
The deviation size of a little parameter characterization calculated values and actual value (or reference value), is to obtain after modeling with HPLC true value correlation comparison
Out.Optimal calibration model is screened with this.
The present invention mainly uses a variety of preprocess methods: multiplicative scatter correction, standard normalization, first derivative, single order
Derivative normalization, second dervative.Spectrum after original spectrum optimizes with part is as shown in Figures 1 to 6.
By comparing RMSECV the and RMSEC value under various algorithms in table 1, multi-stress number etc. considers, final choice
Optimal models: 1) preprocessing procedures: first derivative+vector normalization；2) modeling factors number (PLS factors): 9；3)
The coefficient of determination (R2): 0.9973；4) wave band (Wavelength Region) is modeled: 4200~7500；5) cross validation mean square deviation
(RMSECV): 0.0139.
By comparing RMSECV the and RMSEC value under various algorithms in table 2, multi-stress number etc. considers, final choice
Optimal models: 1) preprocessing procedures: second dervative；2) modeling factors number (PLS factors): 6；3) coefficient of determination
(R2): 0.9935；4) wave band (Wavelength Region) is modeled: 4538~5294；5) cross validation mean square deviation
(RMSECV): 0.0163.
(4) verifying of calibration model
10, small radix bupleuri granular agent sample are chosen, the verifying collection of calibration model is formed；
Verifying collection original spectral data, (II FT-NIR Analyzer of Antaris match are acquired using near infrared spectrometer
Silent ThermoFisher Scientific Company, the U.S., light source；Tungsten halogen lamp, detector: InGaAs, integrating sphere diffusing reflection acquisition system) resolution ratio
8cm-1, 4000~10000cm of scanning optical spectrum range-1, scanning times 32 times, ambient temperature, relative humidity 30~40% obtains
The original near infrared spectrum data of Xiao Chai Hu granules is input to the system for having imported optimal calibration model, and verifying collection is calculated
Predicted value.
True value is measured according to step (2) method.
The predicted value of verifying collection is compareed with true value, is tested to calibration model.
As shown in table 2, predicted value and true value absolute deviation are smaller, illustrate that calibration model has good predictive ability.
Since the saikosaponin a content of radix bupleuri in Xiao Chai Hu granules is lower, detection difficulty is relatively large, as shown in Table 3, bavin
Accuracy rate of the Hu saponin(e a relative deviation less than 5% reaches 90%, thus the saikosaponin a model built of the present invention have it is good
Predictive ability.
As seen from the above table, accuracy rate of the saikosaponin a relative deviation less than 5% reaches 90%, and scutelloside relative deviation is small
Accuracy rate in 2% reaches 100% and illustrates that model built has good predictive ability.
(5) Xiao Chai Hu granules measurement to be measured
Take Xiao Chai Hu granules to be measured；
Using near infrared spectrometer acquisition correction collection original spectral data, scan sample spectra (about 20 seconds/batches) obtain to
Survey the original near infrared spectrum of Xiao Chai Hu granules；Near infrared spectrometer: the silent winged generation of II FT-NIR Analyzer of Antaris match
That scientific & technical corporation, the U.S., light source；Tungsten halogen lamp, detector: InGaAs, integrating sphere diffusing reflection acquisition system；Resolution ratio 8cm-1, sweep
Retouch 4000~10000cm of spectral region-1, scanning times 32 times, ambient temperature, relative humidity 30~40%.
The original near infrared spectrum of Xiao Chai Hu granules to be measured is imported into the optimal of the normalization of step (4) predicted mistake
It is calculated in model, obtains the content of saikosaponin a, scutelloside in small radix bupleuri granular agent sample.
As a result see Fig. 7,8.As seen from the figure, the predicted value for the target component that model built of the present invention is examined connects with true value
Closely, show that model established by the present invention has good predictive ability.Prediction result is accurate, quick, and testing a sample only needs
2min。
Step in the embodiment of the present invention is not fixed, be can according to the actual situation adjustment sequence.
Comparative example
This comparative example is the comparative example of above embodiments, and difference is shown in Table 5.According to table 5, this comparative example is relative to implementation
The difference of example is that pretreated method and modeling wave band mismatch:
For saikosaponin a, the pretreated method of selection is that first derivative+vector normalizes (same to embodiment), modeling
Wave band is 4138~7289cm-1(the modeling wave band be embodiment in the matched modeling wave band of preprocess method " first derivative "；
For scutelloside, the pretreated method of selection is that (the pretreated method is the normalization of first derivative+vector
4538~5294cm-1The matched preprocess method of modeling wave band), modeling wave band be 4538~5294cm-1(same to embodiment).
The same embodiment of remaining step.
Normalization model constructed by comparative example is verified, and the results are shown in Table 6:
Find out from comparative example, saikosaponin a content is low, and detection difficulty is larger, selects wave band unreasonable, measured content phase
It is larger to deviation.There are more interference values by first derivative vector normalized peak shape for scutelloside, lead to content virtual height.
The present invention is by being associated with modeling with small radix bupleuri granular agent Contents of Main Components to sample ir data, by building
Mould wave band, pretreated optimal screening, so that it is high to detect essence close to true value for model built；The present invention is small radix bupleuri granular agent
A kind of quick, Accurate Determining content new method is provided, it is environmentally friendly, safe and nontoxic, online quality control, which is produced, for enterprise mentions
Larger help is supplied.
Each technical characteristic of embodiment described above can be combined arbitrarily, for simplicity of description, not to above-mentioned reality
It applies all possible combination of each technical characteristic in example to be all described, as long as however, the combination of these technical characteristics is not deposited
In contradiction, all should be considered as described in this specification.
The embodiments described above only express several embodiments of the present invention, and the description thereof is more specific and detailed, but simultaneously
It cannot therefore be construed as limiting the scope of the patent.It should be pointed out that coming for those of ordinary skill in the art
It says, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to protection of the invention
Range.Therefore, the scope of protection of the patent of the invention shall be subject to the appended claims.
Claims (10)
1. a kind of content assaying method of Xiao Chai Hu granules effective component, which comprises the steps of:
(1) take multiple Xiao Chai Hu granules samples as calibration set, computerized near infrared scan obtains the original spectral data of calibration set；
(2) Pretreated spectra is carried out to the original spectral data of the calibration set, and selects the modeling wave band of effective component, obtained
The content characteristics spectrum of the effective component；
(3) effective component of the multiple Xiao Chai Hu granules sample is measured respectively using high performance liquid chromatography,
Obtain the content true value of the effective component；
(4) content true value obtained by content characteristics spectrum, step (3) obtained by step (2) is closed using Partial Least Squares
Connection, establishes the normalization model of the effective component；
(5) Xiao Chai Hu granules to be measured are taken, computerized near infrared scan obtains the original spectral data of the Xiao Chai Hu granules to be measured；It should
The original spectral data of Xiao Chai Hu granules sample to be measured imported into step (4) normalization model, calculates through normalization model,
Obtain the content of Xiao Chai Hu granules effective component to be detected.
2. the content assaying method of Xiao Chai Hu granules effective component according to claim 1, which is characterized in that described effective
Ingredient is at least one of saikosaponin a, scutelloside.
3. the content assaying method of Xiao Chai Hu granules effective component according to claim 2, which is characterized in that described effective
Ingredient is saikosaponin a, then in step (2):
For the method that Pretreated spectra uses for multiplicative scatter correction, modeling wave band is 4083~7486cm-1；Alternatively,
For the method that Pretreated spectra uses for standard normalization, modeling wave band is 4138~7289cm-1；Alternatively,
For the method that Pretreated spectra uses for first derivative, modeling wave band is 4138~7289cm-1；Alternatively,
The method that Pretreated spectra uses adds vector to normalize for first derivative, and modeling wave band is 4200~7500cm-1；Alternatively,
For the method that Pretreated spectra uses for second dervative, modeling wave band is 4200~7500cm-1。
4. the content assaying method of Xiao Chai Hu granules effective component according to claim 3, which is characterized in that step (2)
In, for the method that Pretreated spectra uses for first derivative, modeling wave band is 4138~7289cm-1；Alternatively,
The method that Pretreated spectra uses adds vector to normalize for first derivative, and modeling wave band is 4200~7500cm-1；Alternatively,
For the method that Pretreated spectra uses for second dervative, modeling wave band is 4200~7500cm-1。
5. the content assaying method of Xiao Chai Hu granules effective component according to claim 4, which is characterized in that step (2)
In, the method that Pretreated spectra uses adds vector to normalize for first derivative, and modeling wave band is 4200~7500cm-1。
6. the content assaying method of Xiao Chai Hu granules effective component according to claim 2, which is characterized in that described effective
Ingredient is scutelloside, then in step (2):
For the method that Pretreated spectra uses for multiplicative scatter correction, modeling wave band is 4000~5500cm-1；Alternatively,
For the method that Pretreated spectra uses for standard normalization, modeling wave band is 4000~5500cm-1；Alternatively,
For the method that Pretreated spectra uses for first derivative, modeling wave band is 4138~5432cm-1；Alternatively,
The method that Pretreated spectra uses adds vector to normalize for first derivative, and modeling wave band is 4538~5294-1；Alternatively,
For the method that Pretreated spectra uses for second dervative, modeling wave band is 4538~5294cm-1。
7. the content assaying method of Xiao Chai Hu granules effective component according to claim 6, which is characterized in that step (2)
In:
For the method that Pretreated spectra uses for first derivative, modeling wave band is 4138~5432cm-1；Alternatively,
The method that Pretreated spectra uses adds vector to normalize for first derivative, and modeling wave band is 4538~5294-1；Alternatively,
For the method that Pretreated spectra uses for second dervative, modeling wave band is 4538~5294cm-1。
8. the content assaying method of Xiao Chai Hu granules effective component according to claim 7, which is characterized in that step (2)
In:
For the method that Pretreated spectra uses for second dervative, modeling wave band is 4538~5294cm-1。
9. the content assaying method of Xiao Chai Hu granules effective component according to any one of claims 1 to 8, feature exist
In step (5) also verifies gained normalization model, comprising:
Take multiple Xiao Chai Hu granules samples as verifying collection, computerized near infrared scan obtains the original spectral data of verifying collection；
The original spectral data of the verifying collection is poured into the normalization model, calculates, must verify through normalization model
Collect effective component predicted value；
It is detected using the effective component of the high performance liquid chromatography to verifying collection, collection effective component true value must be verified；
Analyze the verifying collection effective component predicted value and verifying collection effective component true value.
10. the content assaying method of Xiao Chai Hu granules effective component according to any one of claims 1 to 8, feature exist
In the condition using computerized near infrared scan includes: resolution ratio 8cm-1, 4000~10000cm of scanning optical spectrum range-1, scanning times
32 times, ambient temperature, relative humidity 30~40%.
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| CN1982874A (en) * | 2005-12-16 | 2007-06-20 | 天津天士力制药股份有限公司 | Near-infrared diffuse reflection spectral method for fastly inspecting drop effective ingredient content |
| CN101303294A (en) * | 2008-06-20 | 2008-11-12 | 河南中医学院 | Application method of near-infrared on-line test technology in Chinese medicine Yiqing granule production |
| CN104297198A (en) * | 2014-10-16 | 2015-01-21 | 广州白云山明兴制药有限公司 | Method for rapidly determining content of index components of Qingkailing oral solution |
| CN104359854A (en) * | 2014-10-16 | 2015-02-18 | 广州白云山明兴制药有限公司 | Method of quickly determining index component contents of Qingkailing granules |
| CN106138131A (en) * | 2016-06-20 | 2016-11-23 | 广东方制药有限公司 | A kind of bupleurum particles and Chinese medicine preparation thereof |
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| CN113156011A (en) * | 2021-04-20 | 2021-07-23 | 广州白云山光华制药股份有限公司 | Method for constructing active ingredient group of small bupleurum particles |
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