CN108693140A - A kind of method of muskone content in quick detection Xingnaojing oral preparation - Google Patents
A kind of method of muskone content in quick detection Xingnaojing oral preparation Download PDFInfo
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- CN108693140A CN108693140A CN201810692594.5A CN201810692594A CN108693140A CN 108693140 A CN108693140 A CN 108693140A CN 201810692594 A CN201810692594 A CN 201810692594A CN 108693140 A CN108693140 A CN 108693140A
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- ALHUZKCOMYUFRB-UHFFFAOYSA-N muskone Natural products CC1CCCCCCCCCCCCC(=O)C1 ALHUZKCOMYUFRB-UHFFFAOYSA-N 0.000 title claims abstract description 62
- 238000000034 method Methods 0.000 title claims abstract description 55
- 239000008918 xingnaojing Substances 0.000 title claims abstract description 31
- 238000002360 preparation method Methods 0.000 title claims abstract description 30
- 238000001514 detection method Methods 0.000 title claims abstract description 12
- 238000002329 infrared spectrum Methods 0.000 claims abstract description 38
- 238000012360 testing method Methods 0.000 claims abstract description 8
- 238000012545 processing Methods 0.000 claims abstract description 6
- 241000972155 Moschus Species 0.000 claims abstract 3
- 238000001228 spectrum Methods 0.000 claims description 44
- 238000012937 correction Methods 0.000 claims description 12
- 230000003595 spectral effect Effects 0.000 claims description 12
- 238000013178 mathematical model Methods 0.000 claims description 11
- 238000000862 absorption spectrum Methods 0.000 claims description 8
- 238000007781 pre-processing Methods 0.000 claims description 7
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 6
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 6
- 238000004458 analytical method Methods 0.000 claims description 6
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Inorganic materials [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 claims description 6
- 238000005259 measurement Methods 0.000 claims description 6
- 239000000126 substance Substances 0.000 claims description 6
- 230000000694 effects Effects 0.000 claims description 5
- 239000000284 extract Substances 0.000 claims description 5
- 238000012795 verification Methods 0.000 claims description 5
- 238000004364 calculation method Methods 0.000 claims description 4
- 238000004587 chromatography analysis Methods 0.000 claims description 4
- 239000010453 quartz Substances 0.000 claims description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 4
- 239000000243 solution Substances 0.000 claims description 4
- 239000002775 capsule Substances 0.000 claims description 3
- 238000011156 evaluation Methods 0.000 claims description 3
- 238000004817 gas chromatography Methods 0.000 claims description 3
- 230000009466 transformation Effects 0.000 claims description 3
- 230000005526 G1 to G0 transition Effects 0.000 claims description 2
- 238000000205 computational method Methods 0.000 claims description 2
- 239000000470 constituent Substances 0.000 claims description 2
- 238000002790 cross-validation Methods 0.000 claims description 2
- 150000002148 esters Chemical class 0.000 claims description 2
- 238000001914 filtration Methods 0.000 claims description 2
- 238000009472 formulation Methods 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 230000003287 optical effect Effects 0.000 claims description 2
- 238000010238 partial least squares regression Methods 0.000 claims description 2
- -1 polysiloxane Polymers 0.000 claims description 2
- 229920001296 polysiloxane Polymers 0.000 claims description 2
- 238000012628 principal component regression Methods 0.000 claims description 2
- 238000004445 quantitative analysis Methods 0.000 claims description 2
- 239000013558 reference substance Substances 0.000 claims description 2
- 239000012085 test solution Substances 0.000 claims description 2
- 238000002604 ultrasonography Methods 0.000 claims description 2
- 238000010792 warming Methods 0.000 claims description 2
- 238000012935 Averaging Methods 0.000 claims 2
- 238000007689 inspection Methods 0.000 claims 2
- 150000002576 ketones Chemical class 0.000 claims 1
- 239000007788 liquid Substances 0.000 claims 1
- 238000000691 measurement method Methods 0.000 claims 1
- 238000004611 spectroscopical analysis Methods 0.000 claims 1
- 239000000523 sample Substances 0.000 description 86
- 239000012071 phase Substances 0.000 description 6
- 239000003814 drug Substances 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 4
- 238000000605 extraction Methods 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 244000153234 Hibiscus abelmoschus Species 0.000 description 2
- 239000004480 active ingredient Substances 0.000 description 2
- 230000001066 destructive effect Effects 0.000 description 2
- 229940079593 drug Drugs 0.000 description 2
- 239000013067 intermediate product Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000002203 pretreatment Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 238000011282 treatment Methods 0.000 description 2
- 239000012808 vapor phase Substances 0.000 description 2
- DTGKSKDOIYIVQL-WEDXCCLWSA-N (+)-borneol Chemical compound C1C[C@@]2(C)[C@@H](O)C[C@@H]1C2(C)C DTGKSKDOIYIVQL-WEDXCCLWSA-N 0.000 description 1
- REPVLJRCJUVQFA-UHFFFAOYSA-N (-)-isopinocampheol Natural products C1C(O)C(C)C2C(C)(C)C1C2 REPVLJRCJUVQFA-UHFFFAOYSA-N 0.000 description 1
- WXCMHFPAUCOJIG-UHFFFAOYSA-N 4'-tert-Butyl-2',6'-dimethyl-3',5'-dinitroacetophenone Chemical compound CC(=O)C1=C(C)C([N+]([O-])=O)=C(C(C)(C)C)C([N+]([O-])=O)=C1C WXCMHFPAUCOJIG-UHFFFAOYSA-N 0.000 description 1
- 206010048962 Brain oedema Diseases 0.000 description 1
- 208000014912 Central Nervous System Infections Diseases 0.000 description 1
- 206010008190 Cerebrovascular accident Diseases 0.000 description 1
- 206010010071 Coma Diseases 0.000 description 1
- 206010010904 Convulsion Diseases 0.000 description 1
- 244000111489 Gardenia augusta Species 0.000 description 1
- 235000018958 Gardenia augusta Nutrition 0.000 description 1
- 206010019196 Head injury Diseases 0.000 description 1
- 241001416180 Moschidae Species 0.000 description 1
- ALHUZKCOMYUFRB-OAHLLOKOSA-N Muscone Chemical compound C[C@@H]1CCCCCCCCCCCCC(=O)C1 ALHUZKCOMYUFRB-OAHLLOKOSA-N 0.000 description 1
- 208000007125 Neurotoxicity Syndromes Diseases 0.000 description 1
- 208000006011 Stroke Diseases 0.000 description 1
- 208000010513 Stupor Diseases 0.000 description 1
- 206010044221 Toxic encephalopathy Diseases 0.000 description 1
- 231100000076 Toxic encephalopathy Toxicity 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 238000013528 artificial neural network Methods 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 229940116229 borneol Drugs 0.000 description 1
- CKDOCTFBFTVPSN-UHFFFAOYSA-N borneol Natural products C1CC2(C)C(C)CC1C2(C)C CKDOCTFBFTVPSN-UHFFFAOYSA-N 0.000 description 1
- 208000006752 brain edema Diseases 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 208000026106 cerebrovascular disease Diseases 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000036461 convulsion Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- DTGKSKDOIYIVQL-UHFFFAOYSA-N dl-isoborneol Natural products C1CC2(C)C(O)CC1C2(C)C DTGKSKDOIYIVQL-UHFFFAOYSA-N 0.000 description 1
- 238000007917 intracranial administration Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 238000010606 normalization Methods 0.000 description 1
- 229940100691 oral capsule Drugs 0.000 description 1
- 229940096978 oral tablet Drugs 0.000 description 1
- 239000007935 oral tablet Substances 0.000 description 1
- 238000005220 pharmaceutical analysis Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 239000003826 tablet Substances 0.000 description 1
Classifications
-
- 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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- Physics & Mathematics (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analysing Materials By Optical Means (AREA)
Abstract
The present invention relates to a kind of methods of Moschus content in quick detection Xingnaojing oral preparation, the described method comprises the following steps:Step 1, the Xingnaojing oral preparation of the qualified known content of multiple batches is acquired;Step 2, it is scanned near infrared spectrometer, obtains spectrogram, the Xingnaojing oral preparation atlas of near infrared spectra and standard muskone content curve of standard are obtained by processing;Step 3, to the Xingnaojing oral preparation not after testing produced, it is scanned near infrared spectrometer using the same method of step 2, the atlas of near infrared spectra obtained according to scanning, the Xingnaojing oral preparation atlas of near infrared spectra of gained atlas of near infrared spectra and standard is subjected to control calculating, you can obtain muskone content in sample.
Description
One, technical field
The invention belongs to Pharmaceutical Analysis technical field, more particularly to a kind of near infrared spectrum quick nondestructive measures Xingnaojing mouth
The method of muskone content in formulation.
Two, background technology
" Xingnaojing oral preparation " is made of cape jasmine, Radix Curcumae, borneol and Moschus four traditional Chinese medicine object, as cerebrovascular accident,
It goes into a coma caused by central nervous system infection and takes out convulsion, toxic encephalopathy, brain edema caused by craniocerebral trauma, intracranial pressure raising causes
The diseases treatment such as stupor drug, clinically have a wide range of applications, there is extensive clinical application basis, and curative effect is aobvious
It writes.
A kind of green analytical technology of near-infrared (NIR) spectral technique as quick nondestructive has and quickly analyzes, at sample
The features such as reason is simple, without consuming reagent.In recent years, near-infrared spectrum technique has more and more been applied to Chinese medicine and has ground
Study carefully, including medicinal material place of production discriminating, the on-line checking of active principle assay and pharmacy procedure and monitoring.Near-infrared spectrum technique
Be introduced as solving the quality Fast Evaluation of complicated Chinese medicine system distillation process and on-line checking provides possibility.
The content of muskone is gas chromatography in Xingnaojing oral preparation at present, and this method sample pre-treatments are complicated, mistake
Journey is cumbersome, time-consuming, costly, pollution environment, cannot meet the needs of quick nondestructive on-line analysis.Therefore, we introduce closely
Infrared detection method controls intermediate products.
Three, invention content
For the above Xingnaojing oral preparation analytical technology present situation, near infrared spectrum quick nondestructive provided by the invention measures
The method of muskone content is not required to carry out sample pre-treatments, and high-throughput, online nondestructive analysis may be implemented, as a result accurately and reliably,
Error is less than 5%, solves the problems such as existing muskone detection is cumbersome time-consuming, and detection sample cannot utilize again.
Technical solution of the invention is as follows:
Using the main component and information to be measured for including in Xingnaojing oral preparation intermediate products near infrared spectrum, with
Near infrared spectrum scanning sample can obtain wherein active ingredient and their background information, using more in Chemical Measurement
The method of member correction realizes the content of the non-destructive determination active ingredient muskone from sample.
The suitable spectrum area of present invention selection and when preprocessing procedures, with the method for stechiometry Multivariate Correction
It establishes the near infrared light spectrum signature of sample and with the mathematical model between measurement, non-destructive determination sample is wanted using mathematical model
The content of middle muskone.
The Chemical Measurement Multivariate Correction used in the present invention, the algorithm to continuous wavelength near infrared spectrum are partially minimum two
Multiplication and artificial neural network algorithm.Preprocess method to spectrum includes first derivative, second dervative, Fourier transform, volume
The smooth and wavelet transformation of product.
For this purpose, the method that the present invention provides Moschus content in a kind of quick detection Xingnaojing oral preparation, the method packet
Include following steps:
Step 1, the Xingnaojing oral preparation of the qualified known content of multiple batches is acquired;
Step 2, it is scanned near infrared spectrometer, obtains spectrogram, the Xingnaojing of standard is obtained by processing
Oral preparation atlas of near infrared spectra and standard muskone content curve;
Step 3, to the Xingnaojing oral preparation not after testing produced, using the same method near-infrared of step 2
Spectrometer is scanned it, according to the atlas of near infrared spectra that scanning obtains, by the restoring consciouness of gained atlas of near infrared spectra and standard
Quiet oral preparation atlas of near infrared spectra carries out control calculating, you can obtains muskone content in sample.
Wherein, the sample containing muskone described in step 1 is particle, tablet or capsule.
Wherein, near infrared spectrometer described in step 2, spectral conditions are as follows:Integrating sphere diffusing reflection, resolution ratio 8cm-1,
Scanning times are 32 times, 4000~10000cm of scanning optical spectrum range-1。
Wherein, the calculating described in step 3, method be, using corrected atlas of near infrared spectra and muskone content
Between mathematical model.
Wherein the mathematical model, method for building up are as follows:
A. sample sets are obtained:Each n batches of Xingnaojing oral preparation are chosen, n is not less than 10, and it is not small that every batch of chooses sample number
In 6;
B. sample near infrared ray:Sample is directly embedded into blank plate center, with BaSO4As blank, it is placed in close
Infrared radiation detection apparatus integrating sphere sample cell obtains muskone abosrption spectrogram by computerized near infrared scan, and record each sample is close red
The absorption spectrum in external spectrum area;
C. sample effective constituent determination:Muskone content is measured by gas chromatography to sample.The specific method is as follows:Chromatography
Condition:Using (50%- phenyl)-methyl polysiloxane as capillary column (column length 30m, internal diameter 0.32mm, the film thickness of stationary phase
0.5Fm);Column temperature is temperature programming;100 DEG C of initial temperature is warming up to 200 DEG C with 10 DEG C of rate per minute, is kept for 20 minutes.
Number of theoretical plate is calculated by muskone peak should be not less than 20000.Sample preparation:Take sample appropriate, it is finely ground, take about 1.5g, precision to claim
It is fixed, it sets in conical flask with cover, ethyl acetate 5ml, weighed weight is added in precision, and ultrasound 30 minutes is placed to room temperature, with acetic acid second
Ester supplies the weight of less loss, shakes up, and centrifugation takes supernatant, filtration to get.
It measures:It is accurate respectively to draw reference substance solution and test solution, note popularity chromatography, measure to get.
D. calibration model is established:Data acquisition is carried out using near infrared spectrometer to each sample in sample sets, is obtained
The initial data of muskone content obtains muskone content characteristics spectral information, with gas by Pretreated spectra and the selection of spectrum area
The sample muskone content obtained in being measured in phase chromatography is corresponding, and calibration model is established using Multivariate Correction method;
E. the verification of model:It takes and the Xingnaojing oral preparation sample of known content, identical item is obtained by gas phase measuring method
Measure near infrared spectrum under part, according to established calibration model calculate sample size, judgement sample sets whether bounded exterior point, just
Confirm after determining, addition is out-of-bounds put re-establishes calibration model, such step, to straightening die by calibration model establishment step again
Type constantly improve is until error < 5%;
F. sample to be tested is analyzed:Sample to be tested scans near infrared spectrum, extracts characteristic spectrum, and input calibration model can be counted
Calculate the content of muskone in sample.
Wherein, the determination condition of standard sample spectral is:Integrating sphere diffusing reflection, resolution ratio 8cm-1, scanning times 32
Secondary, scanning range is 4000~10000cm-1;Data acquisition is carried out to sample using near infrared spectrometer, each sample repeats to adopt
Collection 3 times, takes average spectrum, using opus/quant-2 quantitative analysis softwares, area's selection is pre-processed and composed to spectrum, is removed
Scattering effect is eliminated in interference of the high frequency noise to signal, and the influence deducted instrumental background or drifted about to signal obtains musk deer in sample
Ketone musk content characteristics spectral information carries out mathematical model foundation using Multivariate Correction method.
Wherein, computer calculation is the multivariate calibration methods using Chemical Measurement.The polynary school of Chemical Measurement of use
Just including to continuous wavelength near infrared spectrum be Partial Least Squares or principal component regression algorithm, preprocessing procedures include one
Order derivative, second dervative, Fourier transform, convolution be smooth and wavelet transformation.
Preferably, method of the present invention, steps are as follows:
It is determinand without processing to take, about 0.5~3g appropriate containing Xingnaojing oral preparation, sample;Directly it is laid in
In quartz specimen cup, it is uniformly mixed, gently flattens, be scanned near infrared spectrometer.Each sample multiple scanning 3 times, is asked
Averaged spectrum.Spectral conditions are as follows:Integrating sphere diffusing reflection, resolution ratio 8cm-1, scanning times are 32 times, scanning range 4000
~10000cm-1.Characteristic spectrum information is extracted with preprocessing procedures.The characteristic spectrum information input straightening die that will be obtained
Type calculates to obtain muskone content in sample.
It is compared with existing similar approach, advantages of the present invention:
1, the present invention nearly infrared on line analysis technology is used for Determination of Muscone, is used for Xingnaojing oral preparation for the first time
The content of principle active component monitors, to ensure that the validity of drug.
2, this method has found a kind of simple and effective, accurate sensitive determination sample by the foundation of the above mathematical model
The method of middle muskone content.
3, sample treatment complexity in the prior art is solved, process is cumbersome, time-consuming, costly, pollution environment, Bu Nengman
The defect of the needs of sufficient quick nondestructive on-line analysis.
Four, it illustrates:
Fig. 1 muskone content PLS calibration models reference values and predicted value correlativity figure
Five, specific implementation mode
The present invention is further described by following embodiment, is not limit the invention in any way, without departing substantially from this hair
Under the premise of bright technical solution, those of ordinary skill in the art made for the present invention any change easy to implement or
Change is fallen within scope of the presently claimed invention.
Embodiment 1
Step 1 collects 15 batch of Xingnaojing oral preparation particle, and every batch of acquires 20 samples, totally 300 sample conducts
Modeling sample can be directly as sample to be tested without handling sample.
Step 2 takes about 0.5~3g to be directly placed into quartz specimen cup, is uniformly mixed, gently flattens, with BaSO4As blank,
It is placed near infrared detection instrument integrating sphere sample cell, muskone abosrption spectrogram, test sample mode are obtained by computerized near infrared scan:Product
Bulb separation diffusing reflection, resolution ratio 8cm-1, scanning times are 32 times, and scanning range is 4000~10000cm-1, room temperature:18-25
DEG C, each sample multiple scanning 3 times, record each sample selects Firstderivative in the absorption spectrum of near infrared spectrum
+ Vector normalization carry out Pretreated spectra (table 1), extract characteristic spectrum information.This 300 are measured using gas phase
The muskone content of sample.Using Partial Least Squares, it is corresponding with characteristic spectrum data to establish muskone content in sample
Mathematic correction model.By constantly verifying and improving calibration model, determine that the best band range (table 2) of modeling is:5600-
8000cm-1.Illustrate that there are preferable correlations between muskone near infrared spectrum and its muskone content.
Influence of the different preprocessing procedures of table 1 to calibration model
Influence of the different Spectral ranges of table 2 to calibration model
| Wave band/cm-1 | R2 | RMSECV |
| 4200-5600 | 0.9536 | 0.0421 |
| 5600-8000 | 0.9724 | 0.0409 |
| 6100-10000 | 0.9439 | 0.0454 |
The verification of model:According to the selection of the representative sample of Calibration, 50 in addition to establishing Calibration
Part sample, measures the absorption spectrum of its near infrared region, according to established Partial Least Squares calibration model under the same conditions
The related coefficient of muskone content in calculating sample, obtained NIR predicted values and its content true value is 0.9812, RMSEP=
0.0190。
Step 3 predicts muskone content in unknown content sample:Its atlas of near infrared spectra is scanned by above-mentioned condition, by phase
Pretreated spectra and the selection of spectrum area are answered, the characteristic spectrum of extraction is inputted into calibration model, calculates muskone content in sample.Institute
The content of survey and the deviation of actual content are 1.32%.
Embodiment 2
Step 1 collects 15 batch of Xingnaojing oral tablet, and every batch of acquires 20 samples, and totally 300 samples are as modeling
Sample, sample are determinand without processing
Sample is directly placed fibre-optical probe front end by step 2, using BaSO4 as blank, is placed near infrared detection instrument integral
Ball sample cell obtains muskone abosrption spectrogram, test sample mode by computerized near infrared scan:Integrating sphere diffusing reflection, resolution ratio are
8cm-1, scanning times are 32 times, and scanning range is 4000~10000cm-1, room temperature:18-25 DEG C, each sample multiple scanning 3
Secondary, record each sample selects First derivative+ in the absorption spectrum of near infrared spectrum
Vectornormalization carries out Pretreated spectra (table 1), extracts characteristic spectrum information.This 300 are measured using vapor phase method
The muskone content of sample.Using Partial Least Squares, it is corresponding with characteristic spectrum data to establish muskone content in sample
Mathematic correction model.By constantly verifying and improving calibration model, determine that the best band range (table 2) of modeling is:5600-
8000cm-1.Illustrate that there are preferable correlations between muskone near infrared spectrum and its muskone content.
The verification of model:According to the selection of the representative sample of Calibration, 50 in addition to establishing Calibration
Part sample, measures the absorption spectrum of its near infrared region, according to established Partial Least Squares calibration model under the same conditions
The related coefficient of muskone content in calculating sample, obtained NIR predicted values and its content true value is 0.9921, RMSEP=
0.0185。
Step 3 predicts muskone content in unknown content sample:Its atlas of near infrared spectra is scanned by above-mentioned condition, by phase
Pretreated spectra and the selection of spectrum area are answered, the characteristic spectrum of extraction is inputted into calibration model, calculates muskone content in sample.Institute
The content of survey and the deviation of actual content are 1.22%.
Embodiment 3
Step 1 collects 15 batch of Xingnaojing oral capsule, and every batch of acquires 20 samples, and totally 300 samples are as modeling
Sample can be directly as sample to be tested without handling sample.
Step 2 capsule sample directly places fibre-optical probe front end, with BaSO4As blank, it is placed near infrared detection instrument product
Bulb separation sample cell obtains muskone abosrption spectrogram, test sample mode by computerized near infrared scan:Integrating sphere diffusing reflection, resolution ratio
For 8cm-1, scanning times are 32 times, and scanning range is 4000~10000cm-1, room temperature:18-25 DEG C, each sample multiple scanning
3 times, record each sample selects First derivative+ in the absorption spectrum of near infrared spectrum
Vectornormalization carries out Pretreated spectra (table 1), extracts characteristic spectrum information.This 300 are measured using vapor phase method
The muskone content of sample.Using Partial Least Squares, it is corresponding with characteristic spectrum data to establish muskone content in sample
Mathematic correction model.By constantly verifying and improving calibration model, determine that the best band range (table 2) of modeling is:5600-
8000cm-1.Illustrate that there are preferable correlations between muskone near infrared spectrum and its muskone content.
The verification of model:According to the selection of the representative sample of Calibration, 50 in addition to establishing Calibration
Part sample, measures the absorption spectrum of its near infrared region, according to established Partial Least Squares calibration model under the same conditions
The related coefficient of muskone content in calculating sample, obtained NIR predicted values and its content true value is 0.9895, RMSEP=
0.0119。
Step 3 predicts muskone content in unknown content sample:Its atlas of near infrared spectra is scanned by above-mentioned condition, by phase
Pretreated spectra and the selection of spectrum area are answered, the characteristic spectrum of extraction is inputted into calibration model, calculates muskone content in sample.Institute
The content of survey and the deviation of actual content are 1.03%.
Computational methods are as follows:
The evaluation parameter of mathematical model:R2, the specific formula for calculation of RMSECV, RMSEP:
1,R2:Related coefficient
R2Nearlyr 1, calibration model predicted value and actual value are closer;R2=1, predicted value is fitted completely with actual value;R2For
Negative, fitting effect are poor.
2,RMSECV:Cross validation error root mean square
RMSECV is smaller, and model prediction accuracy is higher
3,RMSEP:Predict error mean square root
The estimated performance of institute's established model is assessed, RMSEP is smaller, and model prediction accuracy is higher.
In various:
Ci--- traditional analysis measured value;
Ci'--- pass through calibration model predicted value;
Cm-CiAverage value;
N --- establish the sample number of calibration model;
The sample number of m --- testing model.
Claims (10)
1. a kind of method of Moschus content in quick detection Xingnaojing oral preparation, which is characterized in that realized by following steps:
Step 1, the Xingnaojing oral preparation of the qualified known content of multiple batches is acquired;
Step 2, it is scanned near infrared spectrometer, obtains spectrogram, the Xingnaojing that standard is obtained by processing is oral
Preparation atlas of near infrared spectra and standard muskone content curve;
Step 3, to the Xingnaojing oral preparation not after testing produced, using the same method near infrared spectrum of step 2
Instrument is scanned it, according to the atlas of near infrared spectra that scanning obtains, by the Xingnaojing mouth of gained atlas of near infrared spectra and standard
Formulation atlas of near infrared spectra carries out control calculating, you can obtains muskone content in sample.
2. according to the method described in claim 1, it is characterized in that, wherein, the sample containing muskone described in step 1 is
Grain, tablet or capsule.
3. according to the method described in claim 1, it is characterized in that, wherein, near infrared spectrometer described in step 2, spectrum item
Part is as follows:Integrating sphere diffusing reflection, resolution ratio 8cm-1, scanning times are 32 times, 4000~10000cm of scanning optical spectrum range-1。
4. according to the method described in claim 1, it is characterized in that, wherein, the calculating described in step 3, method is, using warp
Mathematical model between the atlas of near infrared spectra and muskone content of overcorrect.
5. according to the method described in claim 4, wherein the mathematical model, method for building up are as follows:
A. sample sets are obtained:Each n batches of Xingnaojing oral preparation are chosen, n is not less than 10, and every batch of chooses sample number and is not less than 6;
B. sample near infrared ray:Sample is directly embedded into blank plate center, with BaSO4As blank, it is placed in near-infrared inspection
Instrument integrating sphere sample cell is surveyed, muskone abosrption spectrogram is obtained by computerized near infrared scan, record each sample is near infrared spectrum
The absorption spectrum in area;
C. sample effective constituent determination:Muskone content is measured by gas chromatography to sample.The specific method is as follows:
Chromatographic condition:Using (50%- phenyl)-methyl polysiloxane as capillary column (column length 30m, the internal diameter of stationary phase
0.32mm, film thickness 0.5Fm);Column temperature is temperature programming;100 DEG C of initial temperature is warming up to 200 with 10 DEG C of rate per minute
DEG C, it is kept for 20 minutes.Number of theoretical plate is calculated by muskone peak should be not less than 20000.
Sample preparation:Take sample appropriate, it is finely ground, about 1.5g is taken, it is accurately weighed, it sets in conical flask with cover, acetic acid second is added in precision
Ester 5ml, weighed weight, ultrasound 30 minutes place to room temperature, the weight of less loss are supplied with ethyl acetate, is shaken up, and centrifuge, take
Clear liquid, filtration to get.
It measures:It is accurate respectively to draw reference substance solution and test solution, note popularity chromatography, measure to get.
D. calibration model is established:Data acquisition is carried out using near infrared spectrometer to each sample in sample sets, obtains Moschus
The initial data of ketone content obtains muskone content characteristics spectral information, with gas phase color by Pretreated spectra and the selection of spectrum area
The sample muskone content obtained in being measured in spectrometry is corresponding, and calibration model is established using Multivariate Correction method;
E. the verification of model:It takes and the Xingnaojing oral preparation sample of known content is obtained by gas phase measuring method, under the same terms
Measure near infrared spectrum, sample size calculated according to established calibration model, judgement sample sets whether bounded exterior point, it is positive to confirm
After fixed, addition is out-of-bounds put re-establishes calibration model by calibration model establishment step again, such step, not to calibration model
It is disconnected to improve until error < 5%;
F. sample to be tested is analyzed:Sample to be tested scans near infrared spectrum, extracts characteristic spectrum, and input calibration model can calculate
The content of muskone in sample.
6. according to the method described in claim 5, it is characterized in that the determination condition of standard sample spectral is:Integrating sphere is unrestrained anti-
It penetrates, resolution ratio 8cm-1, scanning times are 32 times, and scanning range is 4000~10000cm-1;Using near infrared spectrometer to sample
Product carry out data acquisition, and each sample repeated acquisition 3 times takes average spectrum, right using opus/quant-2 quantitative analysis softwares
Spectrum is pre-processed and is composed area's selection, removes interference of the high frequency noise to signal, eliminates scattering effect, deduct instrumental background or
The influence drifted about to signal, obtains muskone content characteristics spectral information in sample, and mathematical model is carried out using Multivariate Correction method
It establishes.
7. according to the method described in claim 5, it is characterized in that:Computer calculation is the Multivariate Correction using Chemical Measurement
Method.
8. according to the method described in claim 5, it is characterized in that:The Chemical Measurement Multivariate Correction of use includes to continuous wave
Long near infrared spectrum is Partial Least Squares or principal component regression algorithm, and preprocessing procedures include that first derivative, second order are led
Number, Fourier transform, convolution be smooth and wavelet transformation.
9. according to the method described in claim 1, it is characterized in that:Steps are as follows:
It is determinand without processing to take, about 0.5~3g appropriate containing Xingnaojing oral preparation, sample;Directly it is laid in quartz
In specimen cup, it is uniformly mixed, gently flattens, be scanned near infrared spectrometer.Each sample multiple scanning 3 times, is averaging
Spectrum.Spectral conditions are as follows:Integrating sphere diffusing reflection, resolution ratio 8cm-1, scanning times be 32 times, scanning range be 4000~
10000cm-1.Characteristic spectrum information is extracted with preprocessing procedures.The characteristic spectrum information input calibration model that will be obtained,
Calculate to obtain muskone content in sample.
10. according to the method described in claim 1, it is characterized in that:Steps are as follows:
Sample to be tested about 0.5~3g in right amount is taken, is directly laid in quartz specimen cup, is uniformly mixed, gently flattens, with near-infrared
Spectrometer is scanned.Each sample multiple scanning 3 times, is averaging spectrum.Spectral conditions are as follows:Integrating sphere diffusing reflection is differentiated
Rate is 8cm-1, scanning times are 32 times, and scanning range is 4000~10000cm-1.Characteristic light is extracted with preprocessing procedures
Spectrum information.The calibration model that characteristic spectrum incoming inspection is crossed calculates the content of muskone in sample to be tested.
Computational methods are as follows:
The evaluation parameter of mathematical model:R2, the specific formula for calculation of RMSECV, RMSEP:
1,R2:Related coefficient
R2Nearlyr 1, calibration model predicted value and actual value are closer;R2=1, predicted value is fitted completely with actual value;
R2For negative, fitting effect is poor.
2,RMSECV:Cross validation error root mean square
RMSECV is smaller, and model prediction accuracy is higher
3,RMSEP:Predict error mean square root
The estimated performance of institute's established model is assessed, RMSEP is smaller, and model prediction accuracy is higher.
In various:
Ci --- traditional analysis measured value;
Ci'--- pass through calibration model predicted value;
The average value of Cm-Ci;
N --- establish the sample number of calibration model;
The sample number of m --- testing model.
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