CN106290221A - A kind of Chinese traditional medicine mirabilite Quality evaluation based on FT IR fingerprint chromatogram method - Google Patents
A kind of Chinese traditional medicine mirabilite Quality evaluation based on FT IR fingerprint chromatogram method Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 47
- 239000003814 drug Substances 0.000 title claims abstract description 40
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 title claims abstract description 10
- 239000010446 mirabilite Substances 0.000 title claims abstract description 7
- 238000013441 quality evaluation Methods 0.000 title claims abstract description 7
- RSIJVJUOQBWMIM-UHFFFAOYSA-L sodium sulfate decahydrate Chemical compound O.O.O.O.O.O.O.O.O.O.[Na+].[Na+].[O-]S([O-])(=O)=O RSIJVJUOQBWMIM-UHFFFAOYSA-L 0.000 claims abstract description 78
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 claims abstract description 29
- 238000002329 infrared spectrum Methods 0.000 claims abstract description 27
- 229940079593 drug Drugs 0.000 claims abstract description 26
- 229910052500 inorganic mineral Inorganic materials 0.000 claims abstract description 24
- 239000011707 mineral Substances 0.000 claims abstract description 24
- 239000012567 medical material Substances 0.000 claims abstract description 13
- 238000012360 testing method Methods 0.000 claims abstract description 5
- 239000000470 constituent Substances 0.000 claims description 19
- 238000004458 analytical method Methods 0.000 claims description 16
- 150000003467 sulfuric acid derivatives Chemical class 0.000 claims description 12
- 238000001228 spectrum Methods 0.000 claims description 9
- 238000007639 printing Methods 0.000 claims description 8
- 239000003085 diluting agent Substances 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 5
- 239000004570 mortar (masonry) Substances 0.000 claims description 5
- 230000009466 transformation Effects 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 4
- 238000005259 measurement Methods 0.000 claims description 4
- 238000000227 grinding Methods 0.000 claims description 3
- 238000002203 pretreatment Methods 0.000 claims description 3
- 238000000513 principal component analysis Methods 0.000 claims description 3
- 230000008859 change Effects 0.000 claims description 2
- 239000004615 ingredient Substances 0.000 claims description 2
- 239000011159 matrix material Substances 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 230000003595 spectral effect Effects 0.000 claims description 2
- 238000012544 monitoring process Methods 0.000 abstract description 4
- 238000003908 quality control method Methods 0.000 abstract description 4
- 238000011194 good manufacturing practice Methods 0.000 abstract description 2
- IOLCXVTUBQKXJR-UHFFFAOYSA-M potassium bromide Chemical compound [K+].[Br-] IOLCXVTUBQKXJR-UHFFFAOYSA-M 0.000 description 8
- 238000004519 manufacturing process Methods 0.000 description 5
- 238000011160 research Methods 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 3
- 238000011156 evaluation Methods 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 206010010774 Constipation Diseases 0.000 description 2
- 239000007832 Na2SO4 Substances 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 2
- 229910052938 sodium sulfate Inorganic materials 0.000 description 2
- 238000012935 Averaging Methods 0.000 description 1
- 238000004566 IR spectroscopy Methods 0.000 description 1
- 206010061218 Inflammation Diseases 0.000 description 1
- 208000002193 Pain Diseases 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- 206010042674 Swelling Diseases 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 238000007621 cluster analysis Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000012850 discrimination method Methods 0.000 description 1
- 208000014617 hemorrhoid Diseases 0.000 description 1
- 238000001095 inductively coupled plasma mass spectrometry Methods 0.000 description 1
- 230000004054 inflammatory process Effects 0.000 description 1
- 208000004396 mastitis Diseases 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000010355 oscillation Effects 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- PANBYUAFMMOFOV-UHFFFAOYSA-N sodium;sulfuric acid Chemical compound [Na].OS(O)(=O)=O PANBYUAFMMOFOV-UHFFFAOYSA-N 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N21/3563—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing solids; Preparation of samples therefor
-
- 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
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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 invention discloses a kind of Chinese traditional medicine mirabilite Quality evaluation based on FT IR fingerprint chromatogram method.The Natrii Sulfas sample being collected different batches by market carries out IR spectrum scanning, it is thus achieved that Fourier transform infrared spectroscopy spectrogram (FT IR), according to peak position, the transmitance at total peak, sets up the infrared spectrum average fingerprint collection of illustrative plates of Natrii Sulfas medical material.By testing sample scanned infrared spectrum in mid-infrared light spectrometer, measure Fourier transform infrared spectroscopy figure, compared with the average fingerprint collection of illustrative plates of described Natrii Sulfas, the contrast total peak position at peak, peak number, carry out the calculating of similarity, the true and false of this sample is identified with this, and judge whether mineral drug Natrii Sulfas meets " Chinese Pharmacopoeia " requirement, " Good Manufacturing Practice and Quality Control of Drug ", the GSP and clinical practice, for the authentication method that the quality examination offer of Natrii Sulfas is new, the scientific basis certain to the quality monitoring offer of market mineral drug.
Description
Technical field
The invention belongs to Chinese medicine detection technique field.More particularly, to a kind of Chinese medicine based on FT-IR fingerprint chromatogram method
Saltcake quality authentication method.
Background technology
Natrii Sulfas, a kind of Chinese medicine, for Sulfates mineral drug Natrii Sulfas race Natrii Sulfas, processed refined crystalline solid, main contain
Aqueous sulfuric acid sodium (Na2SO4·10H2O), character is sheet-pile shape, water white transparency and in hyaloid gloss, easy air slaking.Have and rush down
Lower relieving constipation, moistening for dryness and softening hard mass, detumescence of relieving inflammation or internal heat etc. acts on, clinically, constipation due to dry stool, acute mastitis, swelling and pain of hemorrhoid stagnant for excess-heat.
At present, compared to research and the quality control of plant amedica, the mineral drug quality on market is uneven, the place of production and batch
Number smudgy, store of long duration, easy air slaking produce white powder state, and professional skill and the specialty of pharmacy staff are known
Know weakness, mislead client sometimes and buy adulterant, if only judging by white powder appearance character, even pharmacy's work
The most fubaritic true and false of the professionals such as personnel, there is certain blind area in the quality monitoring of mineral drug.
Natrii Sulfas belongs to the common medicine of mineral drug, and modern study is concentrated mainly in the pharmacology study of compound prescription of Natrii Sulfas, and analyzes
Being concentrated mainly on X-ray diffraction and ICP-MS research, both instrument usage amounts are little, and conventional Chinese medicine company there is no outfit phase
The instrument and equipment closed, if being equipped with will also result in certain financial burden.
Summary of the invention
The technical problem to be solved in the present invention overcomes existing above-mentioned existing Sulfates mineral drug Natrii Sulfas authentication method
Defect and deficiency, it is provided that the real and fake discrimination of Sulfates mineral drug Natrii Sulfas and Quality evaluation, specifically a kind of mineral drug awns
The Fourier transform infrared spectroscopy of nitre combines the authentication method of average fingerprint collection of illustrative plates, and the average fingerprint figure set up by the method
Spectrum, evaluates average fingerprint collection of illustrative plates by similarity evaluation, comparison and classified analysis on major constituents, further for the quality of Natrii Sulfas
Monitoring provides the new method of practicality.
It is an object of the invention to provide a kind of Chinese traditional medicine mirabilite Quality evaluation based on FT-IR fingerprint chromatogram method, specifically
Be a kind of Fourier transform infrared spectroscopy combine average fingerprint collection of illustrative plates identify Natrii Sulfas true or false method.
Above-mentioned purpose of the present invention is achieved through the following technical solutions:
The authentication method of the Fourier transform infrared spectroscopy average fingerprint collection of illustrative plates of a kind of mineral drug Natrii Sulfas, including following step
Rapid:
(1) in the Sulfates mineral drug Natrii Sulfas of market collection different batches scans acquisition Fu under middle infrared spectrum region
Leaf transformation infrared spectrogram, according to the total peak-to-peak number of measurement result gained, peak position, transmitance, the Fourier setting up Natrii Sulfas becomes
Changing infrared spectrum average fingerprint collection of illustrative plates, this finger printing is that average fingerprint collection of illustrative plates replaces standard finger-print, as follows:
Below the characteristic peak demarcation of Natrii Sulfas infrared spectrum average fingerprint collection of illustrative plates, 10 total peaks are as main analysis object,
Wave number is 3550,3477,3416,1637,1618,1112,637,616,478 and 448cm successively-1；
(2) with OPUS7.5 software collection image, so that the Fourier transform infrared spectroscopy spectrogram of sample to have passing through of peak
The average of rate is as reference, by the correlation coefficient of SPSS.20 computed in software each sample, included angle cosine value, similarity average, result
Showing, the correlation coefficient of each sample is more than 0.8900, and the included angle cosine value of sample is more than 0.9114, and similarity average is more than
0.9186.Through checking collection checking, the correlation coefficient of adulterant is less than 0.2845, and included angle cosine value is less than 0.8665, and average is similar
Degree is less than 0.5755, it was demonstrated that main component is similar, and Natrii Sulfas infrared average fingerprint collection of illustrative plates has good composition feature.
(3) using classified analysis on major constituents method to evaluate average fingerprint collection of illustrative plates further, this experiment is to principal component analysis
Feature spectral coverage primary election is the position at 10 total peaks, uses SPSS.20 to set up principal component model and is analyzed, carries from original index
Informational capacity in screen less quantity of information, it is desirable to the total variance contribution ratio of main constituent is more than 85%.Pass through contribution rate of accumulative total
Can learn, the eigenvalue of first principal component is 7.312, and contribution rate of accumulative total is 73.121, and the eigenvalue of the Second principal component, factor is
1.631, the contribution rate of accumulative total of the first and second main constituents is 89.434%, and the 3rd above contribution rate of main constituent is 95.163%,
By analysis ingredient coefficient matrix table, the wave number of available first principal component is S1618cm-1, S1637cm-1, Second principal component,
Wave number be S1112cm-1, the wave number of the 3rd main constituent is 478cm-1, 448cm-1。
Application SPSS.20 software system cluster, selects main constituent to represent peak, uses median clustering procedure, with cosine value be
Interval divides, and Natrii Sulfas medical material tentatively can be divided into 2 big classes, and adulterant is divided into a class, remaining sample to be a class automatically.
Wherein, the pre-treatment step of described Natrii Sulfas sample determination Fourier transform infrared spectroscopy figure is；After taking drying and crushing
Sample 10mg and 150mg diluent KBr abundant finely ground mix homogeneously in agate mortar, be placed in small-sized tablet machine and be pressed into
Transparent sheet, is subsequently placed in mid-infrared light spectrometer and measures in middle infrared spectrum region, sets scanning times as 16 times, diaphragm opening
Footpath is 6mm, and resolution is 4cm-1。
The requirement of step (2) uses included angle cosine value, correlation coefficient and averaging method to carry out fingerprint similarity comprehensively
Evaluate, and the average fingerprint collection of illustrative plates established is carried out similarity checking.
The requirement of step (3) be obtain main representative peak after principal component analysis after carry out cluster analysis again, evaluate further
The average fingerprint collection of illustrative plates of Natrii Sulfas.
It addition, the SO that infrared spectrum characteristic area is tetrahedral structure of Sulfates mineral drug Natrii Sulfas in step (1)4,
It is divided into 3 regions with infrared signature, respectively is antisymmetric stretching vibration (1112cm-1±) spike, asymmetric change
Angular oscillation (637cm-1± and 616cm-1±) spike and symmetric deformation vibration (478cm-1± and 448cm-1±) peak position, its
The peak position of middle symmetric deformation vibration is inconspicuous.It is positioned at 3400cm-1Neighbouring wide absworption peak (3550～3416cm-1) comprise knot
The antisymmetry of brilliant water and symmetrical stretching vibration, do not contain angle vibration and rocking vibration and frequency peak.Containing angle absorption of vibrations
Peak (1637cm-1And 1618cm-1), owing to participating in metal-complexing, there is no intermolecular hydrogen bond action, show as sharp-pointed absorption
Peak.
It addition, the Fourier transform infrared spectroscopy average fingerprint of the Sulfates mineral drug Natrii Sulfas set up by said method
Collection of illustrative plates, also within protection scope of the present invention.
A kind of Chinese traditional medicine mirabilite Quality evaluation based on FT-IR fingerprint chromatogram method, is in mid-infrared light by testing sample
Scanned infrared spectrum in spectrometer, measures Fourier transform infrared spectroscopy figure, compared with the average fingerprint collection of illustrative plates of described Natrii Sulfas, right
Than peak position, the peak number at total peak, carry out the calculating of similarity, identify the true and false of this sample with this, and judge mineral drug Natrii Sulfas
Whether meeting " Chinese Pharmacopoeia " requirement, " Good Manufacturing Practice and Quality Control of Drug ", the GSP and clinic should
With.Wherein, use main constituent clustering method that the average fingerprint collection of illustrative plates of Natrii Sulfas is analyzed further.
Preferably, the pre-treatment step of described mensuration Fourier transform infrared spectroscopy figure is；Take the sample after drying and crushing
Be fully ground with diluent KBr, be placed in small-sized tablet machine and be pressed into transparent sheet, be subsequently placed in mid-infrared light spectrometer in
IR regions measures, and sets scanning times as 16 times, and the aperture of the diaphragm is 6mm, and resolution is 4cm-1。
Preferably, the mass ratio of described sample and diluent is 1:10～20.
It is highly preferred that the mass ratio of described sample and diluent is 1:15.
Preferably, described grinding is abundant finely ground mix homogeneously in agate mortar.
Specifically, the above-mentioned achievement of the present invention is drawn by following research contents:
1) the mineral drug Natrii Sulfas collecting 28 batches of different batches and the place of production is carried out under middle infrared spectrum region scanning acquisition Fu
In leaf transformation infrared spectrogram, according to the total peak-to-peak number of measurement result gained, peak position, transmitance, set up the Fourier of Natrii Sulfas
Transform infrared spectroscopy average fingerprint collection of illustrative plates, this finger printing is that average fingerprint collection of illustrative plates replaces standard finger-print, demarcates following 10
Individual total peak is as main analysis object, and wave number is 3550 successively, and 3477,3416,1637,1618,1112,637,616,
478 and 448cm-1；
2) with OPUS7.5 software collection image, with peak total in the Fourier transform infrared spectroscopy spectrogram of 28 batch samples
The average of transmitance is as reference, by the correlation coefficient of SPSS.20 computed in software each sample, included angle cosine value, similarity average,
Result shows, the correlation coefficient of each sample is more than 0.8900, and the included angle cosine value of sample is more than 0.9114, and similarity average is more than
0.9186。
3) as the requirement of the present invention, step 1) in take the sample 10mg after drying and crushing and 150mg diluent KBr in agate
In Nao mortar, abundant finely ground mix homogeneously, is placed in small-sized tablet machine and is pressed into transparent sheet, is subsequently placed in mid-infrared light spectrometer
In measure in middle infrared spectrum region, set scanning times as 16 times, the aperture of the diaphragm is 6mm, and resolution is 4cm-1。
4) as the further checking of the present invention, step 2) in use included angle cosine value, correlation coefficient process and both methods
The similarity of average fingerprint collection of illustrative plates of average overall merit Natrii Sulfas.
5) as the another kind of progress of the present invention, classified analysis on major constituents method is used to evaluate average fingerprint figure further
Spectrum, the wave number of available first principal component is S1618cm-1, S1637cm-1, the wave number of Second principal component, is S1112cm-1, the 3rd
The wave number of main constituent is 478cm-1, 448cm-1, select main constituent to represent peak, use median clustering procedure, with cosine value as interval
Dividing, Natrii Sulfas medical material tentatively can be divided into 2 big classes, and adulterant is divided into a class, remaining sample to be a class automatically.
In sum, the Natrii Sulfas sample that the present invention collects different batches by market carries out IR spectrum scanning, it is thus achieved that Fu
In leaf transformation infrared spectrum spectrogram (FT-IR), according to peak position, the transmitance at total peak, the infrared spectrum setting up Natrii Sulfas medical material is put down
All finger printing.Being contrasted by analysis, set up infrared spectrum average fingerprint collection of illustrative plates, demarcating following 10 total peaks is the red of Natrii Sulfas
The characteristic peak of external spectrum finger printing, wave number is 3550,3477,3416,1637,1618,1112,637,616,478 Hes successively
448cm-1, with correlation coefficient, included angle cosine value and average overall merit similarity, the correlation coefficient of each sample is more than 0.8900,
The included angle cosine value of sample is more than 0.9114.Two kinds of methods are carried out mean value computation, and the similarity average that can obtain each sample is more than
0.9186.Choose some batches of Natrii Sulfas medical material samples to collect as checking, the Natrii Sulfas infrared spectrum average fingerprint collection of illustrative plates set up is carried out
Checking, can distinguish true and false product, and the correlation coefficient of adulterant is less than 0.2845, and included angle cosine value is less than 0.8665, and average similarity is little
In 0.5755, the true or false to Natrii Sulfas, identify whether meet " Chinese Pharmacopoeia " requirement, for the mirror that the quality examination offer of Natrii Sulfas is new
Determine method, the scientific basis certain to the quality monitoring offer of market mineral drug.
The method have the advantages that
The invention provides that a kind of Fourier transform infrared spectroscopy combines average fingerprint collection of illustrative plates identifies Natrii Sulfas true or false
Method, based on current computer technology and the fast development of infrared spectrometer performance indications and raising, infrared spectrum is particularly suitable for
In the research of mineral drug, for the requirement of the needs and quality control meeting market surpervision, establish Natrii Sulfas Fourier transformation red
External spectrum combines the discrimination method of average fingerprint collection of illustrative plates, has easy to use, quick, sensitive advantage.
Accompanying drawing explanation
Fig. 1 is the Fourier transform infrared spectroscopy spectrogram of 28 batches of Natrii Sulfas medical materials.
Fig. 2 is Natrii Sulfas Fourier transform infrared spectroscopy average fingerprint collection of illustrative plates, wherein: 1:3550cm-1, 2:3477cm-1, 3:
3416cm-1, 4:1637cm-1, 5:1618cm-1, 6:1112cm-1, 7:637cm-1, 8:616cm-1, 9:478cm-1, 10:448cm-1。
Fig. 3 is that Natrii Sulfas similarity verifies infrared spectrum spectrogram.
Fig. 4 is Natrii Sulfas classified analysis on major constituents result figure.
Detailed description of the invention
Further illustrate the present invention below in conjunction with Figure of description and specific embodiment, but embodiment is not to the present invention
Limit in any form.Unless stated otherwise, the present invention uses reagent, method and apparatus are the examination of the art routine
Agent, method and apparatus.
Unless stated otherwise, following example agents useful for same and material are commercial.
The Fourier transform infrared spectroscopy of embodiment 1 Natrii Sulfas combines the foundation of average fingerprint atlas calculation
1, Sulfates mineral drug Natrii Sulfas medical material sample is that market is collected, all through Chinese medicine institute of Guangdong pharmaceutical university Lee's book deep pool
Professor identifies, in addition to M9 and M13, is Sulfates mineral drug Natrii Sulfas race's Natrii Sulfas (Natrii Fulfas).Natrii Sulfas medical material sample
Lot number, the place of production, note and content be shown in Table 1.
Table 1 Natrii Sulfas medical material sample lot number, the place of production, note and content.
2, the Natrii Sulfas sample in 28 different batches and the place of production is taken, i.e. in table in addition to M9 and M13, the Natrii Sulfas sample of M1～M30
Each 10mg and 28 parts of 150mg dried potassium bromide reagent mixed grindings in agate mortar are the most finely ground, keep indoor temperature
Being 20 DEG C is 40% with indoor humidity, and the powder after mixing is laid in infrared compression mold and is placed in tablet machine with 20MPa
It is pressed into thin slice.Scanning area is 4000～400cm-1, resolution is 4cm-1, the aperture of the diaphragm is 6mm, and each sample is swept
Retouching number of times is 16 times.Result is as shown in Figure 1.
3, pass through the comparison to 28 batches of test sample infrared spectrograms, analysis, find that 28 batches of Natrii Sulfas medical materials are being respectively (3550
±3)cm-1、(3475±5)cm-1、(3417±3)cm-1、(1639±3)cm-1、(1617±4)cm-1、(1115±6)cm-1、
(638±2)cm-1、(616±4)cm-1、(476±8)cm-1、(448±8)cm-1There are stronger peak type and light transmittance, below demarcation
10 total peaks are the characteristic peak of the Infrared fingerprint spectra of Natrii Sulfas, and wave number is 3550 successively, 3477,3416,1637,1618,
1112,637,616,478 and 448cm-1, as shown in Figure 2.
The ownership at part peak is due to Sulfates mineral drug Natrii Sulfas (Na2SO4·10H2O) character of self composition, sulfate
The infrared spectrum characteristic area of class mineral drug Natrii Sulfas can be by the SO of tetrahedral structure4, it is divided into 3 regions with infrared signature,
It respectively is antisymmetric stretching vibration (1112cm-1±) spike, asymmetric angle vibration (637cm-1± and 616cm-1±)
Spike and symmetric deformation vibration (478cm-1± and 448cm-1±) peak position, wherein symmetric deformation vibration peak position inconspicuous.
The characteristic area of water of crystallization, is positioned at 3400cm-1Neighbouring wide absworption peak (3550～3416cm-1) comprise the opposition of water of crystallization
Claim and symmetrical stretching vibration, do not have angle vibration and rocking vibration and frequency peak.Containing angle vibration absorption peak (1637cm-1
And 1618cm-1), owing to participating in metal-complexing, there is no intermolecular hydrogen bond action, show as sharp-pointed absworption peak.
The checking of the Fourier transform infrared spectroscopy average fingerprint collection of illustrative plates of embodiment 2 Natrii Sulfas
1, the precision of Fourier transform infrared spectroscopy detection method, repeatability and stability
Sample has done precision (n=6), and precision has the RSD at peak and is respectively less than 0.23%, and the RSD of transmitance is the least
In 1.63%；Repeated experiment (n=6), the RSD at the total peak of repeatability is respectively less than 0.46%, and the RSD of transmitance is respectively less than
2.89%；The total peak RSD of repeatability 12h is respectively less than 0.36%, and the RSD of transmitance is respectively less than 2.72%.Illustrate that the method is accurate
The most reliable.
2, Fourier transform infrared spectroscopy average fingerprint collection of illustrative plates similarity evaluation
By SPSS.20 software, have an average of peak transmitance as reference with Natrii Sulfas sample average finger printing, count respectively
Calculating the correlation coefficient of each sample, included angle cosine value, both averages, analysis result is shown in Table 2.The correlation coefficient of result display Natrii Sulfas is big
In 0.8900, the included angle cosine value of sample is more than 0.9114, and similarity average is more than 0.9186, the main one-tenth of most of Natrii Sulfas samples
Seemingly, the similarity of average fingerprint collection of illustrative plates described above is good for split-phase.
3, Fourier transform infrared spectroscopy average fingerprint collection of illustrative plates evaluation methodology checking
For checking Natrii Sulfas Fourier transform infrared spectroscopy average fingerprint collection of illustrative plates method for evaluating similarity, with M9, M13, M31,
M32 verifies as checking collection, and result is shown in Fig. 3, shows that the infrared spectrum spectrogram of M9 and M13 is put down at the infrared spectrum with Natrii Sulfas
All finger printing have the most accordingly through peak on the position at peak, and correlation coefficient is less than 0.2845, and included angle cosine value is less than
0.8665, similarity average is less than 0.5755.M31 and M32 Natrii Sulfas sample is then corresponding with Natrii Sulfas infrared spectrum average fingerprint collection of illustrative plates
Position on occur corresponding through peak, correlation coefficient is more than 0.9432, and included angle cosine value is more than 0.9592, and similarity average is big
In 0.9476.Illustrate that Natrii Sulfas Fourier transform infrared spectroscopy combines the method for average fingerprint collection of illustrative plates and obtained preferable checking.
Embodiment 3 Fourier transform infrared spectroscopy combines the method that average fingerprint atlas analysis identifies sample
1, practical measurement
The sample measured by band, according to preparation method formation determination, scans a Fourier transform infrared spectroscopy figure, with awns
The average fingerprint collection of illustrative plates of nitre contrasts, the contrast total peak number at peak, wave number, peak position, similarity, identifies the ore deposit of this sample with this
Whether thing medicine is Sulfates mineral drug Natrii Sulfas.
2, result is as shown in table 2 and Fig. 4.
Table 2 Natrii Sulfas Infrared fingerprint spectra similarity analysis
Result above shows, the correlation coefficient in Natrii Sulfas medical material sample is more than 0.8900, and included angle cosine value is more than 0.9114,
By mean value computation, the similarity average of derived sample is more than 0.9186, illustrates that the Natrii Sulfas Infrared fingerprint spectra set up has good
Good representativeness, similarity is good, can help to the discriminatory analysis of Natrii Sulfas medical material.
Claims (10)
1. the method for building up of the Fourier transform infrared spectroscopy average fingerprint collection of illustrative plates of a Chinese traditional medicine mirabilite, it is characterised in that include
Following steps: the Sulfates mineral drug Natrii Sulfas of different batches is collected in market, under middle infrared spectrum region, scanning obtains Fu
Leaf transformation infrared spectrogram, according to the total peak-to-peak number of measurement result gained, peak position, transmitance, the Fourier setting up Natrii Sulfas becomes
Change infrared spectrum average fingerprint collection of illustrative plates；This finger printing is that average fingerprint collection of illustrative plates replaces standard finger-print, as follows: Natrii Sulfas is infrared
Following 10 the total peaks of characteristic peak demarcation of spectrum average fingerprint collection of illustrative plates are as main analysis object, and wave number is 3550 successively,
3477,3416,1637,1618,1112,637,616,478 and 448 cm-1。
Method the most according to claim 1, it is characterised in that further with OPUS7.5 software collection image, with sample
In Fourier transform infrared spectroscopy spectrogram, the average of the transmitance at total peak is as reference, by SPSS.20 computed in software each sample
Correlation coefficient, included angle cosine value, similarity average；Correlation coefficient according to result, i.e. each sample is more than 0.8900, sample
Included angle cosine value is more than 0.9114, and similarity average is more than 0.9186, and the correlation coefficient of adulterant is less than 0.2845, included angle cosine value
Less than 0.8665, average similarity is less than 0.5755, it was demonstrated that main component is similar, and Natrii Sulfas infrared spectrum average fingerprint collection of illustrative plates has
Good composition feature.
Method the most according to claim 2, it is characterised in that use classified analysis on major constituents method further further
Evaluate average fingerprint collection of illustrative plates, the position that feature spectral coverage primary election is 10 total peaks to principal component analysis, use SPSS.20 to set up
Principal component model is analyzed, filter information amount from the informational capacity that original index carries, it is desirable to the variance contribution that main constituent is total
Rate is more than 85%；By contribution rate of accumulative total, the eigenvalue of first principal component is 7.312, and contribution rate of accumulative total is 73.121, and second is main
The eigenvalue of components Factor is 1.631, and the contribution rate of accumulative total of the first and second main constituents is 89.434%, more than 3rd main constituent
Contribution rate is 95.163%, and by analysis ingredient coefficient matrix table, the wave number of first principal component is S1618cm-1, S1637cm-1,
The wave number of Second principal component, is S1112cm-1, the wave number of the 3rd main constituent is 478 cm-1, 448 cm-1。
Method the most according to claim 3, it is characterised in that application SPSS.20 software system cluster, selects main constituent generation
Table peak, uses median clustering procedure, divides for interval with cosine value, and Natrii Sulfas medical material tentatively can be divided into 2 big classes, and adulterant is certainly
It is dynamic that to be divided into a class, remaining sample be a class.
5. the Fourier transform infrared light of the Sulfates mineral drug Natrii Sulfas set up according to the arbitrary described method of claim 1 ~ 4
Spectrum average fingerprint collection of illustrative plates.
6. a Chinese traditional medicine mirabilite Quality evaluation based on FT-IR fingerprint chromatogram method, it is characterised in that by testing sample in
Scanned infrared spectrum in infrared spectrometer, measures Fourier transform infrared spectroscopy figure, with the average fingerprint collection of illustrative plates phase of described Natrii Sulfas
Relatively, the contrast total wave number at peak, peak number, peak position, carry out the calculating of similarity, identify the true and false of this testing sample with this.
Method the most according to claim 6, it is characterised in that use further average to Natrii Sulfas of main constituent clustering method
Finger printing is analyzed.
Method the most according to claim 6, it is characterised in that the pre-treatment of described mensuration Fourier transform infrared spectroscopy figure
Step is；Take the sample after drying and crushing and diluent KBr is fully ground, be pressed into transparent sheet, be subsequently placed in mid-infrared light
Measuring in middle infrared spectrum region in spectrometer, set scanning times as 16 times, the aperture of the diaphragm is 6mm, and resolution is 4cm-1。
Method the most according to claim 8, it is characterised in that the mass ratio of described sample and diluent is 1:10 ~ 20.
Method the most according to claim 8, it is characterised in that described grinding is abundant finely ground mixing in agate mortar
Uniformly.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107102015A (en) * | 2017-03-20 | 2017-08-29 | 西南民族大学 | The authentication method of paris polyphylla |
| CN110567907A (en) * | 2019-10-24 | 2019-12-13 | 大理大学 | Method for rapidly identifying authenticity of traditional Chinese medicine based on infrared spectrum technology |
| CN110749575A (en) * | 2019-10-17 | 2020-02-04 | 夏永刚 | Traditional Chinese medicine polysaccharide two-dimensional infrared spectrum identification prediction model and construction method and application thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102288571A (en) * | 2011-05-05 | 2011-12-21 | 大连民族学院 | Method for verifying young pilous antler |
| CN103983603A (en) * | 2014-05-29 | 2014-08-13 | 南京中医药大学 | Establishment method of fourier transform infrared spectrum fingerprint of mineral medicine limonitum, standard fingerprint and application thereof |
-
2016
- 2016-07-27 CN CN201610601627.1A patent/CN106290221A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102288571A (en) * | 2011-05-05 | 2011-12-21 | 大连民族学院 | Method for verifying young pilous antler |
| CN103983603A (en) * | 2014-05-29 | 2014-08-13 | 南京中医药大学 | Establishment method of fourier transform infrared spectrum fingerprint of mineral medicine limonitum, standard fingerprint and application thereof |
Non-Patent Citations (2)
| Title |
|---|
| 吴伟建 等: "基于聚类、主成分和判别分析的海龙红外指纹图谱研究", 《中国药学杂志》 * |
| 闫蔚 等: "6种硫酸盐类矿物药中红外鉴别", 《中国实验方剂学杂志》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107102015A (en) * | 2017-03-20 | 2017-08-29 | 西南民族大学 | The authentication method of paris polyphylla |
| CN110749575A (en) * | 2019-10-17 | 2020-02-04 | 夏永刚 | Traditional Chinese medicine polysaccharide two-dimensional infrared spectrum identification prediction model and construction method and application thereof |
| CN110567907A (en) * | 2019-10-24 | 2019-12-13 | 大理大学 | Method for rapidly identifying authenticity of traditional Chinese medicine based on infrared spectrum technology |
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