CN109596735A - A kind of detection method of Chinese medicine yellow class coloring agent - Google Patents
A kind of detection method of Chinese medicine yellow class coloring agent Download PDFInfo
- Publication number
- CN109596735A CN109596735A CN201811571469.5A CN201811571469A CN109596735A CN 109596735 A CN109596735 A CN 109596735A CN 201811571469 A CN201811571469 A CN 201811571469A CN 109596735 A CN109596735 A CN 109596735A
- Authority
- CN
- China
- Prior art keywords
- chinese medicine
- coloring agent
- solution
- test solution
- detection method
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/62—Detectors specially adapted therefor
- G01N30/74—Optical detectors
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/86—Signal analysis
- G01N30/8624—Detection of slopes or peaks; baseline correction
- G01N30/8631—Peaks
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/86—Signal analysis
- G01N30/8675—Evaluation, i.e. decoding of the signal into analytical information
- G01N30/8679—Target compound analysis, i.e. whereby a limited number of peaks is analysed
Landscapes
- Physics & Mathematics (AREA)
- Analytical Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Library & Information Science (AREA)
- Engineering & Computer Science (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Investigating Or Analysing Materials By The Use Of Chemical Reactions (AREA)
Abstract
The invention discloses a kind of detection methods of Chinese medicine yellow class coloring agent, comprising: the preparation step of test solution: taking sample powder, ethyl alcohol is added, filters to take filtrate, obtains test solution；The preparation step of contrast solution: taking lemon yellow, sunset yellow and bright orange coloring agent, and ethyl alcohol is added, contrast solution is made；Chromatographic determination step: taking contrast solution and test solution, and injection liquid chromatograph is measured；Judgment step: if in the chromatogram of test solution, chromatographic peak not identical with the chromatography main peak retention time of contrast solution, then it is assumed that coloring agent is free of in Chinese medicine；If in the chromatogram of test solution, there is chromatographic peak identical with the chromatography main peak retention time of contrast solution, then compare the uv-visible absorption spectra of contrast solution and test solution using diode array detector；Detection method of the invention solves Chinese medicine detection method problem that is different, and keeping detection efficiency slow in different cultivars.
Description
Technical field
The present invention relates to a kind of detection methods of Chinese medicine yellow class coloring agent, belong to detection technique field.
Background technique
In recent years, the case where Chinese medicine dyes is very serious.National Yao Jian general bureau has issued the inspection of the dyeing of multiple Chinese medicines
Survey method, this method are mostly to be directed to unit Chinese medicine to be detected, and safflower Chinese medicine, west safflower Chinese medicine need to detect lemon yellow,
Safflower Chinese medicine, dark plum Chinese medicine and cordyceps sinensis need to detect sunset yellow, because of the diversity of method, lead to pre-treatment, upper machine point
The complexity of analysis process, detection efficiency are slow, it is therefore necessary to a kind of detection method of Yellow colorant in Chinese medicine groped,
Find general detection method.
Summary of the invention
For overcome the deficiencies in the prior art, the first purpose of this invention is to provide a kind of Chinese medicine yellow class dyeing
The detection method of agent, to solve the Chinese medicine detection method problem that is different, and keeping detection efficiency slow of different cultivars.
Achieving the object of the present invention can be reached by adopting the following technical scheme that: a kind of Chinese medicine yellow class coloring agent
Detection method, comprising:
The preparation step of test solution: taking sample powder, and ethyl alcohol is added and filters to take filtrate after shaking is extracted, is supplied
Test sample solution；
The preparation step of contrast solution: taking lemon yellow, sunset yellow and bright orange coloring agent, and ethyl alcohol is added, and mixing control is made
Solution；
Chromatographic determination step: taking contrast solution and test solution, and injection liquid chromatograph is measured, and records liquid phase color
Spectrogram；
Judgment step: if in the chromatogram of test solution, it is not identical as the chromatography main peak retention time of contrast solution
Chromatographic peak, then it is assumed that in Chinese medicine be free of coloring agent；If in the chromatogram of test solution, there is the chromatography with contrast solution
The identical chromatographic peak of main peak retention time then compares the purple of contrast solution and test solution using diode array detector
Outside-visible absorption spectra, absorption spectrum is not identical, thinks that absorption spectrum is identical, thinks Chinese medicine without coloring agent in Chinese medicine
Material contains coloring agent.
Further, in the preparation step of test solution, sample powder 2g is taken.
Further, in the preparation step of test solution, sample powder is placed in conical flask.
Further, in the preparation step of test solution, ethyl alcohol 25mL is added.
Further, in the preparation step of test solution, 5min is extracted in shaking.
Further, in chromatographic determination step, contrast solution and each 10 μ L of test solution are taken.
Further, in chromatographic determination step, using octadecylsilane chemically bonded silica as filler；Using acetonitrile as mobile phase
A carries out gradient elution by Mobile phase B of the ammonium acetate solution of 0.5% glacial acetic acid containing percent by volume；The wavelength of measurement is
420nm。
Further, in chromatographic determination step, 0-20min, with the mobile phase A and volume basis of percent by volume 2-55%
The mixed liquor of Mobile phase B than 98-45% carries out gradient elution；20-25min, with the mobile phase A and body of percent by volume 55%
The mixed liquor of the Mobile phase B of product percentage 45% is eluted.
Further, in chromatographic determination step, the acetic acid ammonium concentration in ammonium acetate solution is 0.05mol/L.
Further, in judgment step, contrast solution is compared using diode array detector and test solution exists
The uv-visible absorption spectra of 260-500nm wave-length coverage.
Compared with prior art, the beneficial effects of the present invention are:
1, detection method of the invention, the Chinese medicine detection method for solving different cultivars is different, and keeps detection efficiency slow
Problem；
2, the present invention is general multicomponent Yellow series coloring agent detection method, is individually carried out simultaneously to several kinds of Chinese medicinal materials
Detection, to improve detection efficiency；Detection limit, durability etc. meet the requirement of methodology validation.
Detailed description of the invention
Fig. 1 is the chromatogram of contrast solution；
Fig. 2 is the chromatogram of 20180115 medicinal material sample of Cortex Phellodendri；
Fig. 3 is the chromatogram of 20180817 medicinal material sample of Cortex Phellodendri；
Fig. 4 is the chromatogram of 20180913 medicinal material sample of Cortex Phellodendri.
Specific embodiment
In the following, being described further in conjunction with attached drawing and specific embodiment to the present invention:
Embodiment:
A kind of detection method of Chinese medicine yellow class coloring agent, comprising:
The preparation step of test solution: 20180913 sample powder of Cortex Phellodendri 20180115, Cortex Phellodendri 20180817 and Cortex Phellodendri is taken
Each 2g in end is placed in conical flask, and the ethyl alcohol 25mL of mass percent 50% is added and filters to take filtrate after 5min is extracted in shaking, obtains
To test solution 1,2 and 3；
The preparation step of contrast solution: lemon yellow, sunset yellow and the bright orange coloring agent of quality such as taking, and mass percent is added
The mixing contrast solution of total concentration 0.6mg/mL is made in 50% ethyl alcohol；
Chromatographic determination step: taking mixing contrast solution and each 10 μ L of test solution, and injection liquid chromatograph is measured；
Using octadecylsilane chemically bonded silica as filler；Using acetonitrile as mobile phase A, with the second of 0.5% glacial acetic acid containing percent by volume
Acid ammonium solution is Mobile phase B, and the acetic acid ammonium concentration in ammonium acetate solution is 0.05mol/L；0-20min, with percent by volume 2-
The mixed liquor of 55% mobile phase A and the Mobile phase B of percent by volume 98-45% carries out gradient elution；20-25min, with volume
The mixed liquor of the Mobile phase B of the mobile phase A and percent by volume 45% of percentage 55% is eluted；The wavelength of measurement is
420nm；Record liquid chromatogram；
Judgment step: mixing the chromatogram of contrast solution as shown in Figure 1, label 1 is the chromatographic peak of lemon yellow, and label 2 is
The chromatographic peak of sunset yellow, label 3 are bright orange chromatographic peak.The chromatogram of test solution 1,2 and 3 is as in Figure 2-4, does not have
The identical chromatographic peak of chromatography main peak retention time for occurring and mixing contrast solution, then it is assumed that Cortex Phellodendri 20180115, Cortex Phellodendri
20180817 and Cortex Phellodendri 20180913 in be free of coloring agent.
If in the chromatogram of test solution, there is chromatographic peak identical with the chromatography main peak retention time of contrast solution,
Contrast solution and test solution are then compared in the ultraviolet-visible of 260-500nm wave-length coverage using diode array detector
Absorption spectrum, absorption spectrum is not identical, thinks that absorption spectrum is identical, thinks that Chinese medicine contains without coloring agent in Chinese medicine
Coloring agent.
For those skilled in the art, it can make other each according to the above description of the technical scheme and ideas
Kind is corresponding to be changed and deforms, and all these change and deform the protection model that all should belong to the claims in the present invention
Within enclosing.
Claims (10)
1. a kind of detection method of Chinese medicine yellow class coloring agent, characterized by comprising:
The preparation step of test solution: taking sample powder, and ethyl alcohol is added and filters to take filtrate after shaking is extracted, obtains test sample
Solution；
The preparation step of contrast solution: taking lemon yellow, sunset yellow and bright orange coloring agent, and ethyl alcohol is added, mixing contrast solution is made；
Chromatographic determination step: taking contrast solution and test solution, and injection liquid chromatograph is measured, and records liquid chromatogram
Figure；
Judgment step: if in the chromatogram of test solution, color not identical with the chromatography main peak retention time of contrast solution
Spectral peak, then it is assumed that coloring agent is free of in Chinese medicine；If in the chromatogram of test solution, there is the chromatography main peak with contrast solution
The identical chromatographic peak of retention time, then using diode array detector compare contrast solution and test solution it is ultraviolet-can
See absorption spectrum, absorption spectrum is not identical, thinks that absorption spectrum is identical, thinks that Chinese medicine contains without coloring agent in Chinese medicine
There is coloring agent.
2. the detection method of Chinese medicine yellow class coloring agent as described in claim 1, which is characterized in that the system of test solution
In standby step, sample powder 2g is taken.
3. the detection method of Chinese medicine yellow class coloring agent as described in claim 1, which is characterized in that the system of test solution
In standby step, sample powder is placed in conical flask.
4. the detection method of Chinese medicine yellow class coloring agent as described in claim 1, which is characterized in that the system of test solution
In standby step, ethyl alcohol 25mL is added.
5. the detection method of Chinese medicine yellow class coloring agent as described in claim 1, which is characterized in that the system of test solution
In standby step, 5min is extracted in shaking.
6. the detection method of Chinese medicine yellow class coloring agent as described in claim 1, which is characterized in that chromatographic determination step
In, take contrast solution and each 10 μ L of test solution.
7. the detection method of Chinese medicine yellow class coloring agent as described in claim 1, which is characterized in that chromatographic determination step
In, using octadecylsilane chemically bonded silica as filler；Using acetonitrile as mobile phase A, with 0.5% glacial acetic acid containing percent by volume
Ammonium acetate solution is that Mobile phase B carries out gradient elution；The wavelength of measurement is 420nm.
8. the detection method of Chinese medicine yellow class coloring agent as claimed in claim 7, which is characterized in that chromatographic determination step
In, 0-20min, with the mixed liquor of the mobile phase A of percent by volume 2-55% and the Mobile phase B of percent by volume 98-45% into
Row gradient elution；20-25min, with the mixing of the mobile phase A of percent by volume 55% and the Mobile phase B of percent by volume 45%
Liquid is eluted.
9. the detection method of Chinese medicine yellow class coloring agent as claimed in claim 7, which is characterized in that chromatographic determination step
In, the acetic acid ammonium concentration in ammonium acetate solution is 0.05mol/L.
10. the detection method of Chinese medicine yellow class coloring agent as described in claim 1, which is characterized in that in judgment step, adopt
Compare contrast solution and test solution in the ultraviolet-ray visible absorbing of 260-500nm wave-length coverage with diode array detector
Spectrum.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811571469.5A CN109596735A (en) | 2018-12-21 | 2018-12-21 | A kind of detection method of Chinese medicine yellow class coloring agent |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811571469.5A CN109596735A (en) | 2018-12-21 | 2018-12-21 | A kind of detection method of Chinese medicine yellow class coloring agent |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN109596735A true CN109596735A (en) | 2019-04-09 |
Family
ID=65963142
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811571469.5A Pending CN109596735A (en) | 2018-12-21 | 2018-12-21 | A kind of detection method of Chinese medicine yellow class coloring agent |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109596735A (en) |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6451615B1 (en) * | 1998-12-16 | 2002-09-17 | Total Raffinage Distribution S. A. | Colored indicator to measure the distribution of the hydrocarbon families contained in a mixture, the procedure for obtaining it, and its uses |
| CN102507798A (en) * | 2011-11-28 | 2012-06-20 | 福建出入境检验检疫局检验检疫技术中心 | Method for rapidly screening high throughputs of 36 artificial synthetic pigments in food |
| CN107037150A (en) * | 2017-04-11 | 2017-08-11 | 安徽省公众检验研究院有限公司 | It is a kind of at the same determine food in Determination of Preservatives, sweetener and colouring agent method |
| CN107748210A (en) * | 2017-09-14 | 2018-03-02 | 昌邑市检验检测中心 | The method that HPLC DAD detect a variety of synthetic dyestuffs in wheaten food simultaneously |
-
2018
- 2018-12-21 CN CN201811571469.5A patent/CN109596735A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6451615B1 (en) * | 1998-12-16 | 2002-09-17 | Total Raffinage Distribution S. A. | Colored indicator to measure the distribution of the hydrocarbon families contained in a mixture, the procedure for obtaining it, and its uses |
| CN102507798A (en) * | 2011-11-28 | 2012-06-20 | 福建出入境检验检疫局检验检疫技术中心 | Method for rapidly screening high throughputs of 36 artificial synthetic pigments in food |
| CN107037150A (en) * | 2017-04-11 | 2017-08-11 | 安徽省公众检验研究院有限公司 | It is a kind of at the same determine food in Determination of Preservatives, sweetener and colouring agent method |
| CN107748210A (en) * | 2017-09-14 | 2018-03-02 | 昌邑市检验检测中心 | The method that HPLC DAD detect a variety of synthetic dyestuffs in wheaten food simultaneously |
Non-Patent Citations (3)
| Title |
|---|
| NARUMOL VACHIRAPATAMA 等: "Identification and Determination of Seven Synthetic Dyes in Foodstuffs and Soft Drinks on Monolithic C18 Column by High Performance Liquid Chromatography", 《JOURNAL OF FOOD AND DRUG ANALYSIS》 * |
| 朱雪妍 等: "葛根芩连片中掺入染色剂的检测方法研究", 《药物分析杂志》 * |
| 罗轶 等: "蛤蚧定喘丸中十种非法染色物的检测", 《中国医药导报》 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104062374B (en) | The detection method of the Chinese medicine composition of invigorating Qi and tonifying kidney | |
| CN104198619B (en) | A kind of quality determining method of P-Cymene | |
| CN103197027A (en) | Quality control method of astragalus-leech capsules capable of regulating collaterals | |
| CN104391050A (en) | Method for simultaneously detecting 38 restricted coloring agents in cosmetic | |
| CN109490437B (en) | Fingerprint detection method of white peony root | |
| CN101444606A (en) | Quality control method for Liuwei Anxiao traditional Chinese medicine preparation | |
| CN106918667B (en) | Pressurized micro-extraction equipment, pressurized micro-extraction method and application thereof | |
| CN103575850B (en) | Detection method for Gymnadenia conopsea medicinal material | |
| CN109507343B (en) | UPLC method for rapidly determining content of effective components of saffron and identifying illegal dyeing | |
| CN103323558B (en) | Ginkgo biloba preparation analysis sample rapid preparation method based on solid phase extraction technology | |
| CN102662024B (en) | Method for simultaneously determining three alkaloids in granules for eliminating phlegm and stopping cough for children | |
| CN104833736A (en) | Fast qualitative and quantitative detection method for 25-ingredient coral pills through quantitative analysis of multi-components by single-marker | |
| CN108037200B (en) | Quality detection method of kidney nourishing and tranquilizing pills | |
| CN106814157A (en) | The preparation method of rascal reference extract | |
| CN103645251A (en) | Fingerprint spectrum detection method of compound donkey-hide gelatin preparation | |
| CN109596735A (en) | A kind of detection method of Chinese medicine yellow class coloring agent | |
| CN102636589B (en) | HPLC (High Performance Liquid Chromatography) quantitative method for cephaeline hydrochloride and ipecine hydrochloride in ipecacuanha medicinal material and preparation of ipecacuanha medicinal material | |
| CN101474274B (en) | Quality control method of Shensu Chinese medicine preparation | |
| CN103163272A (en) | Quality control method of infant spleen tonifying medicament | |
| CN103454374A (en) | Quality control method of bone rehabilitation medicine | |
| CN103063792B (en) | Quality test method of phlegm eliminating and cough stopping granules for children | |
| CN109557212A (en) | A kind of detection method of Chinese medicine red colour system coloring agent | |
| CN109752470A (en) | A kind of detection method of the multicomponent coloring agent of safflower | |
| CN103675192A (en) | Detection method of inflammation-diminishing compound pierasma quassioides benn capsule | |
| CN103487528A (en) | HPLC fingerprint determination method of cough relieving Bulbus fritillariae cirrhosae and loquat dripping pills |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20190409 |