CN105651722A - Method for controlling quality of dandelion, Isatis leaf and Isatis root mixture based on ultraviolet fingerprint spectrum - Google Patents
Method for controlling quality of dandelion, Isatis leaf and Isatis root mixture based on ultraviolet fingerprint spectrum Download PDFInfo
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- CN105651722A CN105651722A CN201610186558.2A CN201610186558A CN105651722A CN 105651722 A CN105651722 A CN 105651722A CN 201610186558 A CN201610186558 A CN 201610186558A CN 105651722 A CN105651722 A CN 105651722A
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- 239000000203 mixture Substances 0.000 title claims abstract description 71
- 238000000034 method Methods 0.000 title claims abstract description 35
- 241000334160 Isatis Species 0.000 title abstract 6
- 238000001228 spectrum Methods 0.000 title abstract 4
- 241000245665 Taraxacum Species 0.000 title abstract 3
- 235000005187 Taraxacum officinale ssp. officinale Nutrition 0.000 title abstract 3
- 238000002835 absorbance Methods 0.000 claims abstract description 26
- 238000004458 analytical method Methods 0.000 claims abstract description 11
- 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 claims description 60
- 239000008213 purified water Substances 0.000 claims description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 22
- 238000012360 testing method Methods 0.000 claims description 21
- 238000003908 quality control method Methods 0.000 claims description 17
- 230000003595 spectral effect Effects 0.000 claims description 12
- 239000000243 solution Substances 0.000 claims description 10
- 238000003113 dilution method Methods 0.000 claims description 7
- 239000003085 diluting agent Substances 0.000 claims description 6
- 238000004364 calculation method Methods 0.000 claims description 4
- 238000007639 printing Methods 0.000 claims description 4
- 238000010790 dilution Methods 0.000 claims description 3
- 239000012895 dilution Substances 0.000 claims description 3
- 238000000746 purification Methods 0.000 claims description 2
- 238000000870 ultraviolet spectroscopy Methods 0.000 claims description 2
- 238000007865 diluting Methods 0.000 abstract description 4
- 238000002211 ultraviolet spectrum Methods 0.000 abstract 2
- 239000000047 product Substances 0.000 description 16
- 239000003814 drug Substances 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
- 230000000694 effects Effects 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- 239000000273 veterinary drug Substances 0.000 description 5
- 238000004445 quantitative analysis Methods 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 230000000630 rising effect Effects 0.000 description 2
- VKJGBAJNNALVAV-UHFFFAOYSA-M Berberine chloride (TN) Chemical compound [Cl-].C1=C2CC[N+]3=CC4=C(OC)C(OC)=CC=C4C=C3C2=CC2=C1OCO2 VKJGBAJNNALVAV-UHFFFAOYSA-M 0.000 description 1
- 208000027312 Bursal disease Diseases 0.000 description 1
- 241000628997 Flos Species 0.000 description 1
- 238000004566 IR spectroscopy Methods 0.000 description 1
- 241000245240 Lonicera Species 0.000 description 1
- IPQKDIRUZHOIOM-UHFFFAOYSA-N Oroxin A Natural products OC1C(O)C(O)C(CO)OC1OC(C(=C1O)O)=CC2=C1C(=O)C=C(C=1C=CC=CC=1)O2 IPQKDIRUZHOIOM-UHFFFAOYSA-N 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- IKIIZLYTISPENI-ZFORQUDYSA-N baicalin Chemical compound O1[C@H](C(O)=O)[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1OC(C(=C1O)O)=CC2=C1C(=O)C=C(C=1C=CC=CC=1)O2 IKIIZLYTISPENI-ZFORQUDYSA-N 0.000 description 1
- 229960003321 baicalin Drugs 0.000 description 1
- AQHDANHUMGXSJZ-UHFFFAOYSA-N baicalin Natural products OC1C(O)C(C(O)CO)OC1OC(C(=C1O)O)=CC2=C1C(=O)C=C(C=1C=CC=CC=1)O2 AQHDANHUMGXSJZ-UHFFFAOYSA-N 0.000 description 1
- 239000010231 banlangen Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 208000015181 infectious disease Diseases 0.000 description 1
- 230000002458 infectious effect Effects 0.000 description 1
- 238000004811 liquid chromatography Methods 0.000 description 1
- 239000012567 medical material Substances 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 238000013441 quality evaluation Methods 0.000 description 1
- 238000012207 quantitative assay Methods 0.000 description 1
- 239000003440 toxic substance Substances 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
- G01N21/33—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 method for controlling quality of dandelion, Isatis leaf and Isatis root mixture based on ultraviolet fingerprint spectrum and solves the problem that product quality is difficult to control. The method comprises: (1), establishing a control ultraviolet fingerprint spectrum; (2), determining a lower limit of similarity and absorbance range values at peaks and troughs; (3), treating dandelion, Isatis leaf and Isatis root mixture by a diluting method in step (1) and a scanning method to obtain a sample ultraviolet spectrum; (4), subjecting the sample ultraviolet spectrum and the control ultraviolet fingerprint spectrum to similarity analysis by a same analytical method, and determining a qualified product when similarity is not lower than the lower limit and the absorbance at the peaks and troughs are within a control range. The method has the advantages such as high accuracy, high precision, high stability and high repeatability.
Description
Technical field
The present invention relates to a kind of method of quality control, be specifically related to a kind of Herba Taraxaci ultramarine mixture method of quality control based on ultraviolet fingerprint.
Background technology
Herba Taraxaci ultramarine mixture is made up of 9 taste medical materials such as Herba Taraxaci, Folium Isatidis, Radix Isatidis, Flos Loniceraes, has effect of heat-clearing and toxic substances removing, clinically for the auxiliary treatment of infectious bursal disease. Now recording in " the veterinary drug national standard compilation veterinary drug provincial standard rising national standard " write by Ministry of Agriculture veterinary drug evaluation center the 3rd, its quality standard has the thin layer of baicalin, berberine hydrochloride and Cortex Phellodendri to differentiate at present, the quantitative assay of chlorogenic acid.
Owing to Herba Taraxaci ultramarine mixture is made up of 9 taste Chinese crude drugs, chemical composition is numerous, but in prior art, this Herba Taraxaci ultramarine mixture only has two thin layers discriminatings and a kind of Quantitative Analysis of Chemical Composition, it is impossible to the prevention situation that in producing, scarce taste feeds intake, it is difficult to control product quality.
Summary of the invention
The technical problem to be solved is that existing Herba Taraxaci ultramarine mixture only has two thin layers discriminatings and a kind of Quantitative Analysis of Chemical Composition, it is difficult to control to product quality, purpose is in that to provide a kind of Herba Taraxaci ultramarine mixture method of quality control based on ultraviolet fingerprint, solves the unmanageable problem of product quality.
In order to be able to solve the unmanageable problem of product quality, the present invention realizes by adopting the method for this global quality control of Chinese medicine fingerprint. The concrete technical scheme realizing the object of the invention is as follows:
A kind of Herba Taraxaci ultramarine mixture method of quality control based on ultraviolet fingerprint, comprises the following steps:
(1) foundation of ultraviolet fingerprint is compareed: more than 3 batches qualified Herba Taraxaci ultramarine mixture are diluted more than 100 times by purified water respectively, shake up prepared test sample, again with purified water for blank school zero, ultraviolet-uisible spectrophotometer is utilized to be scanned obtaining ultraviolet superposition collection of illustrative plates, calculating the absorbance values in ultraviolet superposition collection of illustrative plates, the finger printing of this absorbance values composition is comparison ultraviolet fingerprint;
(2) lower limit of similarity is determined, and the range of absorbency value at crest and wave trough position place: adopt more than 3 batches qualified Herba Taraxaci ultramarine mixture, identical dilution process and scan method in step (1) is adopted to obtain certified products uv-spectrogram, respectively with the certified products uv-spectrogram of every batch of Herba Taraxaci ultramarine mixture with compare ultraviolet fingerprint and carry out comparing calculation and go out the similarity of every batch of Herba Taraxaci ultramarine mixture, and then obtain the lower limit of similarity;The absorbance of the crest and wave trough position place by adding up certified products uv-spectrogram obtains the comparison value range of absorbance simultaneously;
(3) Herba Taraxaci ultramarine mixture to be measured is obtained sample uv-spectrogram according to the dilution process in step (1) and scan method;
(4) the analysis method that sample uv-spectrogram is identical with comparison ultraviolet fingerprint being carried out similarity analysis, when similarity is not less than lower limit, and the absorbance at crest and wave trough position place is judged to certified products when compareing in value range.
Chinese medicine fingerprint is based on the understanding of centering medicinal substances group's mass action, the integral status of various chemical composition amounts distribution in Chinese medicine COMPLEX MIXED system can be reflected more fully, adopting finger printing that it is carried out macroscopic comprehensive analysis is a kind of effective means, is widely used in the quality evaluation of Chinese medicine. The method setting up Chinese medicine fingerprint at present mainly has ultraviolet spectroscopy, infrared spectrometry, liquid chromatography, gas chromatography etc. But not effective Chinese medicine fingerprint in Herba Taraxaci ultramarine mixture, and the accuracy rate of testing result, precision, stability and repeatability can not be effectively ensured all can meet demand.
By the Herba Taraxaci ultramarine mixture method of quality control of the present invention, and get final product valid certificates by the experimental data of embodiment: the method for the present invention can be effectively ensured the high-accuracy of testing result, precision, stability and repeatability, and effect is very notable.
In order to be able to reach the effect of optimum, wherein, the spectral conditions of the scanning of ultraviolet-uisible spectrophotometer is:
Spectral bandwidth: 2.00nm, sweep limits: 200.00��900.00nm, luminosity pattern: Abs, sweep spacing: 1.00nm;
If the computing formula that the lower limit of similarity is V, this V is as follows:
V=D* (1-3%), wherein, D is the minimum of certified products uv-spectrogram.
Preferably, described sample uv-spectrogram and comparison ultraviolet fingerprint bivariate in data processing software " IBMSPSSstatistics " relevant " Kendall ' stau-b " analytical calculation similarity.
Being experimentally confirmed, when in the present invention, Herba Taraxaci ultramarine mixture dilutes 10 and 100 times, part absorbance is more than 10Abs, and collection of illustrative plates shows imperfect, and when diluting 1000 times, within the scope of 900��200nm, all absorbances are between 0��1Abs, and effect is more significantly. Thus, the heretofore described Herba Taraxaci ultramarine water-reducible multiple of mixture purification is 1000 times, and concrete dilution step is:
Precision pipettes Herba Taraxaci ultramarine mixture 1mL and adds purified water and be diluted to 10mL, shakes up and makes diluent, then precision pipettes 1mL diluent and adds purified water and be diluted to 100mL, shakes up prepared need testing solution.
Being drawn by above-mentioned detection method and computation rule, the lower limit of described similarity is 0.910. The wavelength of described crest is 317.00nm, 282.00nm, and the wavelength of trough is 259.00nm; 317.00nm the range of absorbency value at place is 0.165��0.265, the range of absorbency value at 282.00nm place is 0.162��0.285, and the range of absorbency value at 259.00nm place is 0.137��0.240.
The present invention compared with prior art, has such advantages as and beneficial effect:
1, the invention provides a kind of method on the whole quality of Herba Taraxaci ultramarine mixture being controlled, solve existing Herba Taraxaci ultramarine mixture and only have two thin layers discriminatings and a kind of Quantitative Analysis of Chemical Composition, it is difficult to the problem controlling product quality;
2, the method for quality control of the present invention is easy and simple to handle, accuracy rate is high, and the precision of testing result, stability and repeatability are all very outstanding, and effect is very notable.
Accompanying drawing explanation
Accompanying drawing described herein is used for providing being further appreciated by the embodiment of the present invention, constitutes the part of the application, is not intended that 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 in this Fig. 1, set has the curve chart of 10 batches of Herba Taraxaci ultramarine mixture, there is the part of coincidence, thus cannot be carried out the display become apparent from;
Fig. 2 is the comparison ultraviolet fingerprint in the present invention;
Uv-spectrogram when Fig. 3 is dilute 10 times in embodiment 3;
Uv-spectrogram when Fig. 4 is dilute 100 times in embodiment 3;
Uv-spectrogram when Fig. 5 is dilute 1000 times in embodiment 3.
Detailed description of the invention
For making the object, technical solutions and advantages of the present invention clearly understand, below in conjunction with embodiment and accompanying drawing, the present invention is described in further detail, and exemplary embodiment and the explanation thereof of the present invention are only used for explaining the present invention, not as a limitation of the invention.
Embodiment 1
As it is shown in figure 1, a kind of Herba Taraxaci ultramarine mixture method of quality control based on ultraviolet fingerprint of the present invention, comprise the following steps:
(1) foundation of ultraviolet fingerprint is compareed
First, by 10 batches of qualified for chlorogenic acid content Herba Taraxaci ultramarine mixture, dilute 1000 times by purified water respectively, shake up prepared test sample, again with purified water for blank school zero, ultraviolet-uisible spectrophotometer is utilized to be scanned test sample obtaining ultraviolet superposition collection of illustrative plates, as shown in Figure 1.
Wherein, the concrete dilution step of described Herba Taraxaci ultramarine mixture is:
Precision pipettes Herba Taraxaci ultramarine mixture 1mL and adds purified water and be diluted to 10mL, shakes up and makes diluent, then precision pipettes 1mL diluent and adds purified water and be diluted to 100mL, shakes up prepared need testing solution;
The spectral conditions of described ultraviolet-uisible spectrophotometer scanning is:
Spectral bandwidth: 2.00nm, sweep limits: 200.00��900.00nm, luminosity pattern: Abs, sweep spacing: 1.00nm; And this ultraviolet-uisible spectrophotometer adopts TU-1810PC type ultraviolet-uisible spectrophotometer in the present embodiment.
Then calculating the absorbance values in ultraviolet superposition collection of illustrative plates again, the finger printing of this absorbance values composition is comparison ultraviolet fingerprint, and this comparison ultraviolet fingerprint medium wavelength is as shown in table 1 with the respective value of absorbance.
Table 1
The comparison ultraviolet fingerprint corresponding with data in this table 1 is as shown in Figure 2.
(2) lower limit of similarity is determined
First, adopt other 10 batches of qualified Herba Taraxaci ultramarine mixture, identical dilution process and scan method in step (1) is adopted to obtain certified products uv-spectrogram, contrasting with compareing ultraviolet fingerprint with the certified products uv-spectrogram of every batch of Herba Taraxaci ultramarine mixture respectively, in data processing software " IBMSPSSstatistics ", bivariate relevant " Kendall ' stau-b " analysis meter calculates the similarity of every batch of Herba Taraxaci ultramarine mixture. Meanwhile, detecting in this step that the certified products uv-spectrogram of 10 batches of qualified Herba Taraxaci ultramarine mixture is at the absorbance that wavelength is 317.00nm, 282.00nm, 259.00nm place, the result of similarity and absorbance is as shown in table 2.
Table 2
By similarity result in above-mentioned table 2, and calculate the lower limit of similarity in conjunction with the computing formula of V=D* (1-3%). Wherein V is the lower limit of similarity, and D is the minimum of certified products uv-spectrogram. In the present embodiment, the lower limit V of this similarity is 0.910.
Meanwhile, by the result in above-mentioned table 2 it can be seen that the range of absorbency value at 317.00nm place is 0.165��0.265, the range of absorbency value at 282.00nm place is 0.162��0.285, and the range of absorbency value at 259.00nm place is 0.137��0.240.
(3) Herba Taraxaci ultramarine mixture to be measured is obtained sample uv-spectrogram according to the dilution process in step (1) and scan method; The present embodiment adopts 8 batches of Herba Taraxaci ultramarine mixture, test sample is prepared according to the dilution process in step (1), and adopt the scan method in step (1) to obtain sample uv-spectrogram, and calculating the similarity of every batch of Herba Taraxaci ultramarine mixture by bivariate in the data processing software " IBMSPSSstatistics " in step (2) relevant " Kendall ' stau-b " analysis meter, concrete outcome is as shown in table 3.
(4) the analysis method that sample uv-spectrogram is identical with comparison ultraviolet fingerprint being carried out similarity analysis, when similarity is not less than lower limit, and the absorbance at crest and wave trough position place is judged to certified products when compareing in value range; In the present embodiment, the result of determination of these 8 batches of Herba Taraxaci ultramarine mixture samples is as shown in table 3.
Table 3
Heretofore described qualified Herba Taraxaci ultramarine mixture refers to the Herba Taraxaci ultramarine mixture that chlorogenic acid content is qualified.
Meanwhile, adopting above-mentioned 8 batches of Herba Taraxaci ultramarine mixture to measure the content of chlorogenic acid according to the quality standard of Herba Taraxaci ultramarine mixture in " veterinary drug national standard compilation veterinary drug provincial standard rising national standard " the 3rd, testing result is as shown in table 4.
Table 4
Quality standard specifies: the every 1mL of this product, must not less than 0.50mg in chlorogenic acid (C16H18O9).
Being contrasted it can be seen that the method for quality control testing result accuracy rate of the present invention can reach 100% with the result of determination in table 4 by table 3, effect is extremely notable.
Embodiment 2
The present embodiment is the mensuration to the inventive method precision, stability and repeatability, and concrete assay method is as follows:
1. precision
Precision pipettes Herba Taraxaci ultramarine mixture 1mL and is placed in 10mL volumetric flask, adds purified water and is diluted to scale, shakes up, precision pipettes 1mL and is placed in 100mL volumetric flask again, adds purified water and is diluted to scale, shakes up, obtain need testing solution, scan 6 times continuously by the determined spectral scan condition of the present invention. Record crest 317.00,282.00nm, the RSD of trough 259.00nm place absorbance respectively 0.23%, 0.19%, 0.33%.
2. stability
Precision pipettes Herba Taraxaci ultramarine mixture (lot number: 151201) 1mL and is placed in 10mL volumetric flask, add purified water and be diluted to scale, shake up, precision pipettes 1mL and is placed in 100mL volumetric flask again, add purified water and be diluted to scale, shake up, obtain need testing solution, by " 1 " determined spectral scan condition respectively at 0,1,2,3,4,5h run-down. Record crest 317.00,282.00nm, the RSD of trough 259.00nm place absorbance respectively 0.41%, 0.61%, 1.07%.
3. repeatability
Precision pipettes with a collection of Herba Taraxaci ultramarine mixture (lot number: 151201) 1mL, 5 parts, it is placed in 10mL volumetric flask, adds purified water and be diluted to scale, shake up, precision pipettes 1mL and is placed in 100mL volumetric flask again, adds purified water and is diluted to scale, shakes up, obtain need testing solution, by the scanning of " 1 " determined spectral scan condition, record crest 317.00,282.00nm, the RSD of trough 259.00nm place absorbance respectively 1.74%, 1.98%, 2.51%.
In the present embodiment adopt Herba Taraxaci ultramarine mixture be all embodiment 1 step (2) is numbered 2 Herba Taraxaci ultramarine mixture. By above-mentioned crest 317.00,282.00nm, the RSD of trough 259.00nm place absorbance has high precision, stability and repeatability it can be seen that the method for the present invention can be effectively ensured testing result.
Embodiment 3
The present embodiment is that the extension rate to Herba Taraxaci ultramarine mixture is inquired into, and namely inquires into the impact on detection of the preparation method of test sample, and concrete operations are as follows:
1. precision pipettes Herba Taraxaci ultramarine mixture 1mL and is placed in 10mL volumetric flask, adds purified water and is diluted to scale, shake up, obtain need testing solution, scans by the spectral scan condition of the present invention, and result is shown in Fig. 3.
2. precision pipettes Herba Taraxaci ultramarine mixture 1mL and is placed in 100mL volumetric flask, adds purified water and is diluted to scale, shake up, obtain need testing solution, scans by the spectral scan condition of the present invention, and result is shown in Fig. 4.
3. precision pipettes Herba Taraxaci ultramarine mixture 1mL and is placed in 10mL volumetric flask, adds purified water and is diluted to scale, shakes up, precision pipettes 1mL and is placed in 100mL volumetric flask again, adds purified water and is diluted to scale, shakes up, obtaining need testing solution, scan by the spectral scan condition of the present invention, result is shown in Fig. 5.
By the collection of illustrative plates of Fig. 3 to Fig. 5 it can be seen that when diluting 10 and 100 times, part absorbance is more than 10Abs, and collection of illustrative plates shows imperfect, and when diluting 1000 times, within the scope of 900��200nm, all absorbances are between 0��1Abs, comparatively properly.
Above-described detailed description of the invention; the purpose of the present invention, technical scheme and beneficial effect have been further described; it is it should be understood that; the foregoing is only the specific embodiment of the present invention; the protection domain being not intended to limit the present invention; all within the spirit and principles in the present invention, any amendment of making, equivalent replacement, improvement etc., should be included within protection scope of the present invention.
Claims (7)
1. the Herba Taraxaci ultramarine mixture method of quality control based on ultraviolet fingerprint, it is characterised in that comprise the following steps:
(1) foundation of ultraviolet fingerprint is compareed: more than 3 batches qualified Herba Taraxaci ultramarine mixture are diluted more than 100 times by purified water respectively, shake up prepared test sample, again with purified water for blank school zero, ultraviolet-uisible spectrophotometer is utilized to be scanned obtaining ultraviolet superposition collection of illustrative plates, calculating the absorbance values in ultraviolet superposition collection of illustrative plates, the finger printing of this absorbance values composition is comparison ultraviolet fingerprint;
(2) lower limit of similarity is determined, and the range of absorbency value at crest and wave trough position place: adopt more than 3 batches qualified Herba Taraxaci ultramarine mixture, identical dilution process and scan method in step (1) is adopted to obtain certified products uv-spectrogram, respectively with the certified products uv-spectrogram of every batch of Herba Taraxaci ultramarine mixture with compare ultraviolet fingerprint and carry out comparing calculation and go out the similarity of every batch of Herba Taraxaci ultramarine mixture, and then obtain the lower limit of similarity; The absorbance of the crest and wave trough position place by adding up certified products uv-spectrogram obtains the comparison value range of absorbance simultaneously;
(3) Herba Taraxaci ultramarine mixture to be measured is obtained sample uv-spectrogram according to the dilution process in step (1) and scan method;
(4) the analysis method that sample uv-spectrogram is identical with comparison ultraviolet fingerprint being carried out similarity analysis, when similarity is not less than lower limit, and the absorbance at crest and wave trough position place is judged to certified products when compareing in value range.
2. a kind of Herba Taraxaci ultramarine mixture method of quality control based on ultraviolet fingerprint according to claim 1, it is characterised in that the spectral conditions of described step (1) medium ultraviolet visible spectrophotometer scanning is:
Spectral bandwidth: 2.00nm, sweep limits: 200.00��900.00nm, luminosity pattern: Abs, sweep spacing: 1.00nm.
3. a kind of Herba Taraxaci ultramarine mixture method of quality control based on ultraviolet fingerprint according to claim 1, it is characterised in that the lower limit setting similarity is as follows as the computing formula of V, this V:
V=D* (1-3%), wherein, D is the minimum of certified products uv-spectrogram.
4. a kind of Herba Taraxaci ultramarine mixture method of quality control based on ultraviolet fingerprint according to claim 1 or 2 or 3, it is characterized in that, described sample uv-spectrogram and comparison ultraviolet fingerprint bivariate in data processing software " IBMSPSSstatistics " relevant " Kendall ' stau-b " analytical calculation similarity.
5. a kind of Herba Taraxaci ultramarine mixture method of quality control based on ultraviolet fingerprint according to claim 4, it is characterised in that the described Herba Taraxaci ultramarine water-reducible multiple of mixture purification is 1000 times, and concrete dilution step is:
Precision pipettes Herba Taraxaci ultramarine mixture 1mL and adds purified water and be diluted to 10mL, shakes up and makes diluent, then precision pipettes 1mL diluent and adds purified water and be diluted to 100mL, shakes up prepared need testing solution.
6. a kind of Herba Taraxaci ultramarine mixture method of quality control based on ultraviolet fingerprint according to claim 5, it is characterised in that the lower limit of described similarity is 0.910.
7. a kind of Herba Taraxaci ultramarine mixture method of quality control based on ultraviolet fingerprint according to claim 5, it is characterised in that the wavelength of described comparison ultraviolet fingerprint medium wave peak is 317.00nm, 282.00nm, and the wavelength of trough is 259.00nm; 317.00nm the range of absorbency value at place is 0.165 ~ 0.265, the range of absorbency value at 282.00nm place is 0.162 ~ 0.285, and the range of absorbency value at 259.00nm place is 0.137 ~ 0.240.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610186558.2A CN105651722B (en) | 2016-03-29 | 2016-03-29 | A kind of public English ultramarine mixture method of quality control based on ultraviolet fingerprint |
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| CN114414512A (en) * | 2022-01-20 | 2022-04-29 | 深圳开悦生命科技有限公司 | Spectral analysis method for identifying and quantitatively analyzing anti-cancer drugs |
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| CN109402924A (en) * | 2018-12-28 | 2019-03-01 | 浙江理工大学上虞工业技术研究院有限公司 | A method of improving dyeing process accuracy |
| CN113495110A (en) * | 2021-08-05 | 2021-10-12 | 魏秀丽 | Method for simultaneously measuring 4 effective components in dandelion bluish green blue particles |
| CN114137129A (en) * | 2021-12-16 | 2022-03-04 | 山东省饲料兽药质量检验中心 | Method for detecting 15 effective components in dandelion, green blue mixture by adopting HPLC-PDA method |
| CN114137129B (en) * | 2021-12-16 | 2023-06-20 | 山东省饲料兽药质量检验中心 | Method for detecting 15 effective components in dandelion bluish mixture by adopting HPLC-PDA method |
| CN114414512A (en) * | 2022-01-20 | 2022-04-29 | 深圳开悦生命科技有限公司 | Spectral analysis method for identifying and quantitatively analyzing anti-cancer drugs |
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