CN105651722B - A kind of public English ultramarine mixture method of quality control based on ultraviolet fingerprint - Google Patents
A kind of public English ultramarine mixture method of quality control based on ultraviolet fingerprint Download PDFInfo
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- CN105651722B CN105651722B CN201610186558.2A CN201610186558A CN105651722B CN 105651722 B CN105651722 B CN 105651722B CN 201610186558 A CN201610186558 A CN 201610186558A CN 105651722 B CN105651722 B CN 105651722B
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- 239000000203 mixture Substances 0.000 title claims abstract description 65
- IRERQBUNZFJFGC-UHFFFAOYSA-L azure blue Chemical compound [Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Al+3].[Al+3].[Al+3].[Al+3].[Al+3].[Al+3].[S-]S[S-].[O-][Si]([O-])([O-])[O-].[O-][Si]([O-])([O-])[O-].[O-][Si]([O-])([O-])[O-].[O-][Si]([O-])([O-])[O-].[O-][Si]([O-])([O-])[O-].[O-][Si]([O-])([O-])[O-] IRERQBUNZFJFGC-UHFFFAOYSA-L 0.000 title claims abstract description 60
- 238000000034 method Methods 0.000 title claims abstract description 31
- 238000003908 quality control method Methods 0.000 title claims abstract description 16
- 238000002835 absorbance Methods 0.000 claims abstract description 25
- 238000004458 analytical method Methods 0.000 claims abstract description 13
- 238000003113 dilution method Methods 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 22
- 239000008213 purified water Substances 0.000 claims description 21
- 238000012360 testing method Methods 0.000 claims description 13
- 230000003595 spectral effect Effects 0.000 claims description 12
- 238000010790 dilution Methods 0.000 claims description 9
- 239000012895 dilution Substances 0.000 claims description 9
- 239000012085 test solution Substances 0.000 claims description 8
- 238000004364 calculation method Methods 0.000 claims description 5
- 238000012797 qualification Methods 0.000 claims description 4
- 239000003795 chemical substances by application Substances 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 2
- 239000003814 drug Substances 0.000 description 7
- 230000000694 effects Effects 0.000 description 7
- CWVRJTMFETXNAD-FWCWNIRPSA-N 3-O-Caffeoylquinic acid Natural products O[C@H]1[C@@H](O)C[C@@](O)(C(O)=O)C[C@H]1OC(=O)\C=C\C1=CC=C(O)C(O)=C1 CWVRJTMFETXNAD-FWCWNIRPSA-N 0.000 description 6
- PZIRUHCJZBGLDY-UHFFFAOYSA-N Caffeoylquinic acid Natural products CC(CCC(=O)C(C)C1C(=O)CC2C3CC(O)C4CC(O)CCC4(C)C3CCC12C)C(=O)O PZIRUHCJZBGLDY-UHFFFAOYSA-N 0.000 description 6
- CWVRJTMFETXNAD-KLZCAUPSSA-N Neochlorogenin-saeure Natural products O[C@H]1C[C@@](O)(C[C@@H](OC(=O)C=Cc2ccc(O)c(O)c2)[C@@H]1O)C(=O)O CWVRJTMFETXNAD-KLZCAUPSSA-N 0.000 description 6
- CWVRJTMFETXNAD-JUHZACGLSA-N chlorogenic acid Chemical compound O[C@@H]1[C@H](O)C[C@@](O)(C(O)=O)C[C@H]1OC(=O)\C=C\C1=CC=C(O)C(O)=C1 CWVRJTMFETXNAD-JUHZACGLSA-N 0.000 description 6
- 229940074393 chlorogenic acid Drugs 0.000 description 6
- FFQSDFBBSXGVKF-KHSQJDLVSA-N chlorogenic acid Natural products O[C@@H]1C[C@](O)(C[C@@H](CC(=O)C=Cc2ccc(O)c(O)c2)[C@@H]1O)C(=O)O FFQSDFBBSXGVKF-KHSQJDLVSA-N 0.000 description 6
- 235000001368 chlorogenic acid Nutrition 0.000 description 6
- BMRSEYFENKXDIS-KLZCAUPSSA-N cis-3-O-p-coumaroylquinic acid Natural products O[C@H]1C[C@@](O)(C[C@@H](OC(=O)C=Cc2ccc(O)cc2)[C@@H]1O)C(=O)O BMRSEYFENKXDIS-KLZCAUPSSA-N 0.000 description 6
- 238000007865 diluting Methods 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- 238000001228 spectrum Methods 0.000 description 4
- 239000000273 veterinary drug Substances 0.000 description 4
- 239000000243 solution Substances 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 229940079593 drug Drugs 0.000 description 2
- 238000004445 quantitative analysis Methods 0.000 description 2
- 241000205585 Aquilegia canadensis Species 0.000 description 1
- 240000001949 Taraxacum officinale Species 0.000 description 1
- 235000005187 Taraxacum officinale ssp. officinale Nutrition 0.000 description 1
- 244000299492 Thespesia populnea Species 0.000 description 1
- 235000009430 Thespesia populnea Nutrition 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 239000010231 banlangen Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 229940126678 chinese medicines Drugs 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 238000004811 liquid chromatography Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000013441 quality evaluation Methods 0.000 description 1
- 238000004153 renaturation Methods 0.000 description 1
- XDQITMCFPPPMBC-TUANDBMESA-N scutelloside Natural products OC[C@H]1O[C@@H](O[C@@H]2O[C@@H]3C[C@H]4[C@H](O)[C@@H](O)[C@@](O)(CO3)[C@@H]24)[C@H](O)[C@@H](O)[C@@H]1O XDQITMCFPPPMBC-TUANDBMESA-N 0.000 description 1
- 238000006467 substitution reaction Methods 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
- G01N21/33—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using ultraviolet light
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/38—Diluting, dispersing or mixing samples
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- Physics & Mathematics (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)
- Spectroscopy & Molecular Physics (AREA)
- Investigating Or Analysing Materials By Optical Means (AREA)
Abstract
The invention discloses a kind of public English ultramarine mixture method of quality control based on ultraviolet fingerprint solves the problems, such as that product quality is difficult to control.The present invention includes:(1)Compare the foundation of ultraviolet fingerprint;(2)Determine the range of absorbency value at the lower limiting value and wave crest and wave trough position of similarity:(3)By public English ultramarine mixture to be measured according to step(1)In dilution process and scan method obtain sample uv-spectrogram;(4)Sample uv-spectrogram is subjected to similarity analysis with the identical analysis method of ultraviolet fingerprint is compareed, is determined as certified products when similarity is not less than lower limiting value, and the absorbance at wave crest and wave trough position is in control value range.The method of the present invention has many advantages, such as high-accuracy, high precision, high stability and high duplication.
Description
Technical field
The present invention relates to quality control methods, and in particular to a kind of public English ultramarine mixture based on ultraviolet fingerprint
Method of quality control.
Background technology
Public English ultramarine mixture is made of the 9 taste medicinal material such as dandelion, folium isatidis, Radix Isatidis, honeysuckle, is had clearing heat and detoxicating
Effect is clinically used for the auxiliary treatment of gumboro disease.It now records in being write by Ministry of Agriculture veterinary drug evaluation center《Beast
Medicine national standard compilation-veterinary drug provincial standard rises national standard》Third volume, at present its quality standard have scutelloside, hydrochloric acid small
Bark of a cork tree alkali and the discriminating of the thin layer of Cortex Phellodendri, the quantitative determination of chlorogenic acid.
Since public English ultramarine mixture is made of 9 taste Chinese medicines, chemical composition is numerous, but the public affairs English ultramarine is closed in the prior art
Agent only has two thin layers discriminatings and a kind of Quantitative Analysis of Chemical Composition, cannot prevent to lack the case where taste feeds intake in production, it is difficult to control
Product quality processed.
Invention content
Only have two thin layers the technical problem to be solved by the present invention is to existing public English ultramarine mixture to differentiate and a kind of chemistry
Component quantifying measures, it is difficult to control product quality, and it is an object of the present invention to provide a kind of public English ultramarine mixture based on ultraviolet fingerprint
Method of quality control solves the problems, such as that product quality is difficult to control.
In order to solve the problems, such as that product quality is difficult to control, the present invention is by using this whole matter of traditional Chinese medicine fingerprint
The method of amount control is realized.Realize that the specific technical solution of the object of the invention is as follows:
A kind of public English ultramarine mixture method of quality control based on ultraviolet fingerprint, includes the following steps:
(1) foundation of ultraviolet fingerprint is compareed:3 batches or more qualified public English ultramarine mixture are diluted with purified water respectively
100 times or more, obtained test sample is shaken up, then using purified water as blank school zero, be scanned using ultraviolet-uisible spectrophotometer
Ultraviolet superposition collection of illustrative plates is obtained, the absorbance values in ultraviolet superposition collection of illustrative plates, the fingerprint image of absorbance values composition are calculated
Spectrum is control ultraviolet fingerprint;
(2) the range of absorbency value at the lower limiting value and wave crest and wave trough position of similarity is determined:Using 3 batches or more
Qualified public affairs English ultramarine mixture obtains certified products uv-spectrogram, respectively using identical dilution process in step (1) and scan method
With the certified products uv-spectrogram of every batch of public affairs English ultramarine mixture with compare ultraviolet fingerprint and carry out comparing calculation to go out every batch of public affairs English green
The similarity of blue mixture, and then obtain the lower limiting value of similarity;Pass through the wave crest and trough of statistics certified products uv-spectrogram simultaneously
Absorbance at position obtains the control value range of absorbance;
(3) by public English ultramarine mixture to be measured according to the dilution process and the scan method acquisition ultraviolet figure of sample in step (1)
Spectrum;
(4) sample uv-spectrogram is subjected to similarity analysis with the identical analysis method of ultraviolet fingerprint is compareed, works as phase
It is not less than lower limiting value like degree, and the absorbance at wave crest and wave trough position is determined as certified products when compareing in value range.
Traditional Chinese medicine fingerprint is the understanding based on centering medicinal substances group's mass action, can more adequately reflect that Chinese medicine is multiple
The integral status of various chemical composition amount distributions in miscellaneous mixed system, it is one to carry out macroscopic comprehensive analysis to it using finger-print
The effective means of kind, are widely used in the quality evaluation of Chinese medicine.The method for establishing traditional Chinese medicine fingerprint at present mainly has purple
External spectrum method, infra-red sepectrometry, liquid chromatography, gas chromatography etc..But in not effective in public English ultramarine mixture
Medicine finger-print, and accuracy rate, precision, stability and repeatability that testing result cannot be effectively ensured can meet demands.
Public English ultramarine mixture method of quality control through the invention, and can effectively be demonstrate,proved by the experimental data of embodiment
It is bright:High-accuracy, precision, stability and the repeatability of testing result can be effectively ensured in the method for the present invention, and effect is very aobvious
It writes.
In order to the effect being optimal, wherein the spectral conditions of the scanning of ultraviolet-uisible spectrophotometer are:
Spectral bandwidth:2.00nm scanning range:200.00~900.00nm, luminosity pattern:Abs, sweep spacing:
1.00nm;
If the lower limiting value of similarity is V, the calculation formula of the V is as follows:
V=D* (1-3%), wherein D is the minimum of certified products uv-spectrogram.
Preferably, the sample uv-spectrogram passes through data processing software " IBM SPSS with ultraviolet fingerprint is compareed
Bivariate correlation " Kendall ' s tau-b " analysis calculates similarity in statistics ".
It is experimentally confirmed, when public English ultramarine mixture dilutes 10 and 100 times in the present invention, part absorbance value is more than
10Abs, collection of illustrative plates show it is imperfect, dilution 1000 times when, within the scope of 900~200nm, all absorbance values 0~1Abs it
Between, effect is more notable.Thus, it is 1000 times that heretofore described public affairs English ultramarine mixture, which purifies water-reducible multiple, specifically
Dilution step is:
Precision pipettes public English ultramarine mixture 1mL and purified water is added to be diluted to 10mL, shakes up and dilution is made, then precision pipettes
1mL dilutions add purified water to be diluted to 100mL, shake up obtained test solution.
It is obtained by above-mentioned detection method and computation rule, the lower limiting value of the similarity is 0.910.The wave crest
Wavelength is 317.00nm, 282.00nm, and the wavelength of trough is 259.00nm;Range of absorbency value at 317.00nm is 0.165
Range of absorbency value at~0.265,282.00nm is that the range of absorbency value at 0.162~0.285,259.00nm is
0.137~0.240.
Compared with prior art, the present invention having the following advantages and advantages:
1, the present invention provides a kind of methods controlled on the whole the quality of public English ultramarine mixture, solve existing
Public English ultramarine mixture only has two thin layers and differentiates and a kind of Quantitative Analysis of Chemical Composition, it is difficult to the problem of controlling product quality;
2, method of quality control of the invention is easy to operate, accuracy rate is high, and the precision of testing result, stability and again
Renaturation is very outstanding, and effect is very notable.
Description of the drawings
Attached drawing described herein is used for providing further understanding the embodiment of the present invention, constitutes one of the application
Point, do not constitute the restriction to the embodiment of the present invention.In the accompanying drawings:
Fig. 1 is the ultraviolet superposition collection of illustrative plates in the embodiment of the present invention, and the curve for having 10 batches of public English ultramarine mixture is gathered in the Fig. 1
Figure, there are the part of coincidence, thus the display that can not be more clear;
Fig. 2 is the control ultraviolet fingerprint in the present invention;
Fig. 3 is uv-spectrogram when diluting 10 times in embodiment 3;
Fig. 4 is uv-spectrogram when diluting 100 times in embodiment 3;
Fig. 5 is uv-spectrogram when diluting 1000 times in embodiment 3.
Specific implementation mode
To make the objectives, technical solutions, and advantages of the present invention clearer, with reference to embodiment and attached drawing, to this
Invention is described in further detail, and exemplary embodiment of the invention and its explanation are only used for explaining the present invention, do not make
For limitation of the invention.
Embodiment 1
As shown in Figure 1, a kind of public English ultramarine mixture method of quality control based on ultraviolet fingerprint of the present invention, including with
Lower step:
(1) foundation of ultraviolet fingerprint is compareed
First, by 10 batches of qualified public English ultramarine mixture of chlorogenic acid content, 1000 times is diluted with purified water respectively, shakes up system
Test sample is obtained, then using purified water as blank school zero, it is ultraviolet to be scanned acquisition to test sample using ultraviolet-uisible spectrophotometer
It is superimposed collection of illustrative plates, as shown in Figure 1.
Wherein, the specific dilution step of the public English ultramarine mixture is:
Precision pipettes public English ultramarine mixture 1mL and purified water is added to be diluted to 10mL, shakes up and dilution is made, then precision pipettes
1mL dilutions add purified water to be diluted to 100mL, shake up obtained test solution;
The spectral conditions of ultraviolet-uisible spectrophotometer scanning are:
Spectral bandwidth:2.00nm scanning range:200.00~900.00nm, luminosity pattern:Abs, sweep spacing:
1.00nm;And the ultraviolet-uisible spectrophotometer uses TU-1810PC type ultraviolet-uisible spectrophotometers in the present embodiment.
Then the absorbance values in ultraviolet superposition collection of illustrative plates are calculated again, and the finger-print of absorbance values composition is
For control ultraviolet fingerprint, the respective value of the control ultraviolet fingerprint medium wavelength and absorbance is as shown in table 1.
Table 1
Control ultraviolet fingerprint corresponding with data in the table 1 is as shown in Figure 2.
(2) lower limiting value of similarity is determined
First, using other 10 batches qualified public English ultramarine mixture, using identical dilution process in step (1) and scanning side
Method obtain certified products uv-spectrogram, respectively use every batch of public affairs English ultramarine mixture certified products uv-spectrogram with compare ultraviolet fingerprint
It is compared, by bivariate correlation " Kendall ' s tau-b " point in data processing software " IBM SPSS statistics "
Analysis calculates the similarity of every batch of public affairs English ultramarine mixture.Meanwhile detecting the qualification of 10 batches of qualified public English ultramarine mixture in this step
Product uv-spectrogram is in the absorbance that wavelength is at 317.00nm, 282.00nm, 259.00nm, and the result of similarity and absorbance is such as
Shown in table 2.
Table 2
By similarity result in above-mentioned table 2, and the calculation formula of V=D* (1-3%) is combined to calculate under similarity
Limit value.Wherein V is the lower limiting value of similarity, and D is the minimum of certified products uv-spectrogram.The lower limit of the similarity in the present embodiment
Value V is 0.910.
Meanwhile by the result in above-mentioned table 2 it is found that range of absorbency value at 317.00nm is 0.165~0.265,
Range of absorbency value at 282.00nm be the range of absorbency value at 0.162~0.285,259.00nm be 0.137~
0.240。
(3) by public English ultramarine mixture to be measured according to the dilution process and the scan method acquisition ultraviolet figure of sample in step (1)
Spectrum;Using 8 batches of public English ultramarine mixture in the present embodiment, test sample is prepared according to the dilution process in step (1), and use step
(1) scan method in obtains sample uv-spectrogram, and passes through data processing software " the IBM SPSS in step (2)
Bivariate correlation " Kendall ' s tau-b " analysis calculates the similarity of every batch of public affairs English ultramarine mixture, tool in statistics "
The results are shown in Table 3 for body.
(4) sample uv-spectrogram is subjected to similarity analysis with the identical analysis method of ultraviolet fingerprint is compareed, works as phase
It is not less than lower limiting value like degree, and the absorbance at wave crest and wave trough position is determined as certified products when compareing in value range;This reality
Applying the judgement of the public English ultramarine mixture sample of this in example 8 batches, the results are shown in Table 3.
Table 3
The public English ultramarine mixture of heretofore described qualification refers to the public English ultramarine mixture of chlorogenic acid content qualification.
Meanwhile using above-mentioned 8 batches public English ultramarine mixture according to《Veterinary drug national standard compilation-veterinary drug provincial standard rises state
Family's standard》The quality standard of public English ultramarine mixture measures the content of chlorogenic acid in third volume, and testing result is as shown in table 4.
Table 4
Quality standard provides:This product in terms of chlorogenic acid (C16H18O9), must not be less than 0.50mg per 1mL.
By the judgement Comparative result in table 3 and table 4 it is found that the method for quality control accuracy rate of testing result of the present invention can
Reach 100%, effect is extremely notable.
Embodiment 2
The present embodiment is to the measurement of the method for the present invention precision, stability and repeatability, and specific assay method is as follows:
1. precision
Precision pipettes public English ultramarine mixture 1mL and is placed in 10mL volumetric flasks, adds purified water to be diluted to scale, shakes up, then essence
The close 1mL that pipettes is placed in 100mL volumetric flasks, and purified water is added to be diluted to scale, is shaken up to get test solution, is pressed institute of the present invention
Determining spectral scan condition continuous scanning 6 times.Measure wave crest 317.00,282.00nm, absorbance value at trough 259.00nm
RSD be respectively 0.23%, 0.19%, 0.33%.
2. stability
Precision pipettes public English ultramarine mixture (lot number:151201) 1mL is placed in 10mL volumetric flasks, and purified water is added to be diluted to quarter
Degree, shakes up, then precision pipettes 1mL and is placed in 100mL volumetric flasks, adds purified water to be diluted to scale, shakes up molten to get test sample
Liquid, by spectral scan condition determined by " 1 " respectively at 0,1,2,3,4,5h run-downs.Measure wave crest 317.00,
The RSD of absorbance value is respectively 0.41%, 0.61%, 1.07% at 282.00nm, trough 259.00nm.
3. repeatability
Precision is pipetted with the public English ultramarine mixture (lot number of a batch:151201) 1mL 5 parts, is placed in 10mL volumetric flasks, adds pure
Change water and be diluted to scale, shakes up, then precision pipettes 1mL and is placed in 100mL volumetric flasks, adds purified water to be diluted to scale, shakes up, i.e.,
Test solution is obtained, by spectral scan condition scanning determined by " 1 ", measures wave crest 317.00,282.00nm, trough
The RSD of absorbance value is respectively 1.74%, 1.98%, 2.51% at 259.00nm.
The public English ultramarine mixture used in the present embodiment is that number is closed for 2 public English ultramarine in 1 step of embodiment (2)
Agent.By above-mentioned wave crest 317.00,282.00nm, at trough 259.00nm absorbance value RSD it is found that the present invention method energy
Testing result, which is effectively ensured, has high precision, stability and repeatability.
Embodiment 3
The present embodiment is inquired into the extension rate of public English ultramarine mixture, that is, inquires into the preparation method of test sample to inspection
The influence of survey, concrete operations are as follows:
1. precision pipettes public English ultramarine mixture 1mL and is placed in 10mL volumetric flasks, adds purified water to be diluted to scale, shake up, i.e.,
Test solution is obtained, by the spectral scan condition scanning of the present invention, as a result sees Fig. 3.
2. precision pipettes public English ultramarine mixture 1mL and is placed in 100mL volumetric flasks, adds purified water to be diluted to scale, shake up, i.e.,
Test solution is obtained, by the spectral scan condition scanning of the present invention, as a result sees Fig. 4.
3. precision pipettes public English ultramarine mixture 1mL and is placed in 10mL volumetric flasks, adds purified water to be diluted to scale, shake up, then
Precision pipettes 1mL and is placed in 100mL volumetric flasks, and purified water is added to be diluted to scale, shakes up to get test solution, by the present invention
Spectral scan condition scanning, as a result see Fig. 5.
By the collection of illustrative plates of Fig. 3 to Fig. 5 it is found that when diluting 10 and 100 times, part absorbance value is more than 10Abs, and collection of illustrative plates is shown
Imperfect, when diluting 1000 times, within the scope of 900~200nm, all absorbance values are between 0~1Abs, more properly.
Above-described specific implementation mode has carried out further the purpose of the present invention, technical solution and advantageous effect
It is described in detail, it should be understood that the foregoing is merely the specific implementation mode of the present invention, is not intended to limit the present invention
Protection domain, all within the spirits and principles of the present invention, any modification, equivalent substitution, improvement and etc. done should all include
Within protection scope of the present invention.
Claims (5)
1. a kind of public English ultramarine mixture method of quality control based on ultraviolet fingerprint, which is characterized in that include the following steps:
(1) foundation of ultraviolet fingerprint is compareed:3 batches or more qualified public English ultramarine mixture are diluted 100 with purified water respectively
Times or more, obtained test sample is shaken up, then using purified water as blank school zero, acquisition is scanned using ultraviolet-uisible spectrophotometer
Ultraviolet superposition collection of illustrative plates, calculates the absorbance values in ultraviolet superposition collection of illustrative plates, and the finger-print of absorbance values composition is
To compare ultraviolet fingerprint;
(2) the range of absorbency value at the lower limiting value and wave crest and wave trough position of similarity is determined:Using 3 batches or more qualifications
Public English ultramarine mixture, certified products uv-spectrogram is obtained using identical dilution process in step (1) and scan method, is used respectively every
The certified products uv-spectrogram for criticizing public English ultramarine mixture goes out the conjunction of every batch of public affairs English ultramarine with ultraviolet fingerprint progress comparing calculation is compareed
The similarity of agent, and then obtain the lower limiting value of similarity;Pass through the wave crest and wave trough position of statistics certified products uv-spectrogram simultaneously
The absorbance at place obtains the control value range of absorbance;
(3) by public English ultramarine mixture to be measured according to the dilution process and scan method acquisition sample uv-spectrogram in step (1);
(4) sample uv-spectrogram is subjected to similarity analysis with the identical analysis method of ultraviolet fingerprint is compareed, works as similarity
Not less than lower limiting value, and the absorbance at wave crest and wave trough position is determined as certified products when compareing in value range;
The spectral conditions of ultraviolet-uisible spectrophotometer scanning are in the step (1):
Spectral bandwidth:2.00nm scanning range:200.00~900.00nm, luminosity pattern:Abs, sweep spacing:1.00nm;
If the lower limiting value of similarity is V, the calculation formula of the V is as follows:
V=D* (1-3%), wherein D is the minimum of certified products uv-spectrogram.
2. a kind of public English ultramarine mixture method of quality control based on ultraviolet fingerprint according to claim 1, special
Sign is that the sample uv-spectrogram passes through data processing software " IBM SPSS with ultraviolet fingerprint is compareed
Bivariate correlation " Kendall ' s tau-b " analysis calculates similarity in statistics ".
3. a kind of public English ultramarine mixture method of quality control based on ultraviolet fingerprint according to claim 2, special
Sign is that it is 1000 times that the public affairs English ultramarine mixture, which purifies water-reducible multiple, and specific dilution step is:
Precision pipettes public English ultramarine mixture 1mL and purified water is added to be diluted to 10mL, shakes up and dilution is made, then to pipette 1mL dilute for precision
Releasing liquid adds purified water to be diluted to 100mL, shakes up obtained test solution.
4. a kind of public English ultramarine mixture method of quality control based on ultraviolet fingerprint according to claim 3, special
Sign is that the lower limiting value of the similarity is 0.910.
5. a kind of public English ultramarine mixture method of quality control based on ultraviolet fingerprint according to claim 3, special
Sign is that the wavelength of the control ultraviolet fingerprint medium wave peak is 317.00nm, 282.00nm, and the wavelength of trough is
259.00nm;Range of absorbency value at 317.00nm is that the range of absorbency value at 0.165~0.265,282.00nm is
Range of absorbency value at 0.162~0.285,259.00nm is 0.137~0.240.
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