CN109596733A - The detection method of Yellow Red coloring agent in a kind of medicinal material - Google Patents
The detection method of Yellow Red coloring agent in a kind of medicinal material Download PDFInfo
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- CN109596733A CN109596733A CN201811571412.5A CN201811571412A CN109596733A CN 109596733 A CN109596733 A CN 109596733A CN 201811571412 A CN201811571412 A CN 201811571412A CN 109596733 A CN109596733 A CN 109596733A
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- 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
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- 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
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- G01N30/74—Optical detectors
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- 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
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Abstract
The invention discloses a kind of detection methods of Yellow Red coloring agent in medicinal material, comprising the following steps: 1) takes II standard reagent of gold orange, auramine O standard reagent and Basic Orange standard reagent respectively, add 40-60vt% ethyl alcohol to dissolve, obtain standard solution；2) sample to be tested is taken, is dispersed with step 1) with the ethyl alcohol of concentration, filters, obtains solution to be measured；3) solution and standard solution to be measured are quantitatively pipetted, injection liquid chromatograph is eluted；4) solution to be measured is compared the retention time at tracer signal peak with the HPLC map of standard solution.Whether this method can be contains Yellow Red coloring agent in fast qualitative detection medicinal material, each echo signal peak sharply without support tail, noiseless, reduces the requirement to equipment, improves detector efficiency, has more optimistic market prospects.
Description
Technical field
The present invention relates to a kind of a kind of detection methods of Yellow Red coloring agent in analysis method more particularly to medicinal material.
Background technique
Chinese medicine dyeing belongs to a kind of illegal addition behavior.For this purpose, Yao Jian general bureau, country has issued the dye of multiple Chinese medicines
The detection method of color, currently, Chinese medicine detection orange series coloring agent mainly has: gold orange II coloring agent, auramine O coloring agent,
Basic Orange coloring agent.
Following table is common coloring agent ingredient and suspicious addition medicinal material and corresponding detection method list:
1 coloring agent of table and detection method
But above-mentioned detection method is mostly single coloring agent detection, and detection efficiency is lower, for this reason, it may be necessary to orange to Chinese medicine
The method that serial coloring agent multicomponent is detected with the time is groped, and is established one kind and is able to carry out Chinese medicine orange series coloring agent
The universal test method that multicomponent is detected with the time.
Summary of the invention
For overcome the deficiencies in the prior art, the purpose of the present invention is to provide in a kind of high-throughput, efficient medicinal material
The detection method of Yellow Red coloring agent.
The purpose of the present invention adopts the following technical scheme that realization:
The detection method of Yellow Red coloring agent in a kind of medicinal material, comprising the following steps:
1) II standard reagent of gold orange, auramine O standard reagent and Basic Orange standard reagent are taken respectively, add 40-60vt% ethyl alcohol
Dissolution, obtains standard solution；
2) sample to be tested is taken, is dispersed with step 1) with the ethyl alcohol of concentration, filters, obtains solution to be measured；
3) solution and standard solution to be measured are quantitatively pipetted, liquid chromatograph is injected separately into and is eluted；
The parameter of the liquid chromatograph are as follows:
Chromatographic column: C18Reverse-phase chromatographic column；
Mobile phase: A acetonitrile；
B 0.05mol/L ammonium acetate solution；
Elution program: t0-25min, mobile phase A is gradually increased to 50-60vt% by 2vt%；
t25-35min, the proportions constant of mobile phase A and Mobile phase B；
t35-37min, mobile phase A is gradually decreased to 2vt% by 50-60vt%；
t37-40min, the proportions constant of mobile phase A and Mobile phase B；
4) retention time at tracer signal peak solution to be measured is compared with the HPLC map of standard solution, doubtful peak
Uv-visible absorption spectra using the more corresponding chromatographic peak of diode array detector in 260-500nm wave-length coverage is examined and determine,
Determine that signal peak belongs to.
Further, in step 1), using the ethyl alcohol of 50vt%.
Further, in step 1), dispersing mode is shaking.
Further, it in step 2), is filtered using 0.45 μm of filter membrane.
Further, in step 2), the filter membrane is Teflon filtration film.
Further, in step 3), solution is by 0.45 μm of filter membrane filtering before sample introduction.
Further, in step 3), glacial acetic acid containing 0.5vt% in Mobile phase B.
Further, in step 3), t0-25min, mobile phase A is gradually increased to 55vt% by 2vt%；t35-37min, mobile phase A
2vt% is gradually decreased to by 55vt%.
Further, in step 3), the detector of liquid chromatograph is DAD detector.
Further, in step 3), Detection wavelength 420nm.
Compared with prior art, the beneficial effects of the present invention are:
Method provided by the invention rapidly can carry out qualitative detection, gold orange II, auramine O and alkali to the coloring agent in medicine
Property orange retention time interval it is long, each signal peak is sharply without support tail, noiseless, by carrying out ultraviolet-ray visible absorbing to doubtful peak
Spectrum reinspection, reduces the requirement to equipment, improves detector efficiency, has more optimistic market prospects.
Detailed description of the invention
Fig. 1 is the HPLC figure of the standard solution of the embodiment of the present invention 1；
Fig. 2 is that the ultraviolet of signal peak 2 is shown in visible light spectrogram in Fig. 1；
Fig. 3 is that the ultraviolet of signal peak 3 is shown in visible light spectrogram in Fig. 1；
Fig. 4 is the HPLC figure of 20180503 corydalis tuber medicinal material in embodiment 2；
Fig. 5 is that the ultraviolet of signal peak 2 is shown in visible light spectrogram in Fig. 4；
Fig. 6 is that the ultraviolet of signal peak 3 is shown in visible light spectrogram in Fig. 4；
Fig. 7 is the HPLC figure of 20180620 corydalis tuber medicinal material in embodiment 2；
Fig. 8 is that the ultraviolet of signal peak 2 is shown in visible light spectrogram in Fig. 7；
Fig. 9 is that the ultraviolet of signal peak 3 is shown in visible light spectrogram in Fig. 7；
Figure 10 is the HPLC figure of 20180815 corydalis tuber medicinal material in embodiment 2；
Figure 11 is that the ultraviolet of signal peak 2 is shown in visible light spectrogram in Figure 10；
Figure 12 is that the ultraviolet of signal peak 3 is shown in visible light spectrogram in Figure 10.
Specific embodiment
In the following, being described further in conjunction with attached drawing and specific embodiment to the present invention, it should be noted that not
Under the premise of conflicting, new implementation can be formed between various embodiments described below or between each technical characteristic in any combination
Example.
The detection method of Yellow Red coloring agent in a kind of medicinal material, comprising the following steps:
1) II standard reagent of gold orange, auramine O standard reagent and Basic Orange standard reagent are taken respectively, add 40-60vt% ethyl alcohol
Dissolution, obtains standard solution；
2) sample to be tested is taken, is dispersed with step 1) with the ethyl alcohol of concentration, filters, obtains solution to be measured；
3) solution and standard solution to be measured are quantitatively pipetted, injection liquid chromatograph is analyzed；
The parameter of the liquid chromatograph are as follows:
Chromatographic column: C18Reverse-phase chromatographic column；
Mobile phase: A acetonitrile；
The 0.05mol/L ammonium acetate solution of B glacial acetic acid containing 0.5vt%；
Elution program: t0-25min, mobile phase A is gradually increased to 55vt% by 2vt%；
t25-35min, the proportions constant of mobile phase A and Mobile phase B；
t35-37min, mobile phase A is gradually decreased to 2vt% by 55vt%；
t37-40min, the proportions constant of mobile phase A and Mobile phase B；
4) solution to be measured is compared the retention time at tracer signal peak with the HPLC map of standard solution, doubtful to adopt
With the more corresponding chromatographic peak of diode array detector in the uv-visible absorption spectra of 260-500nm wave-length coverage, determines and return
Belong to.
The detection method be by gradient elution so as in 40min to gold orange II, auramine O and the Basic Orange in medicinal material
Qualitative detection is carried out, the retention time of gold orange II is near 24.4min, the retention time point of two isomers of auramine O
Not near 25.4min and 27.3min, the retention time of Basic Orange is 34.8min.
Embodiment 1:
A kind of production of the standard diagram of gold orange II, auramine O and Basic Orange, comprising the following steps:
1) II standard reagent of gold orange, auramine O standard reagent and the Basic Orange standard reagent of 5mg or so are accurately weighed respectively,
Add the dissolution of 50% ethyl alcohol to shake up, is settled to 25mL, obtains standard solution；
2) aspiration step 1) 10 μ L of standard solution, inject liquid chromatograph, Detection wavelength be 420nm under washed
It is de-；
The parameter of the liquid chromatograph are as follows:
Chromatographic column: C18Reverse-phase chromatographic column；
Mobile phase: A acetonitrile；
The 0.05mol/L ammonium acetate solution of B glacial acetic acid containing 0.5vt%；
Elution program: t0-25min, mobile phase A is gradually increased to 55vt% by 2vt%；
t25-35min, the proportions constant of mobile phase A and Mobile phase B；
t35-37min, mobile phase A is gradually decreased to 2vt% by 55vt%；
t37-40min, the proportions constant of mobile phase A and Mobile phase B；
3) column temperature of liquid chromatograph is 20 DEG C, flow velocity 0.7mL/min；The retention time at tracer signal peak is using
Uv-visible absorption spectra of the more corresponding chromatographic peak of diode array detector in 260-500nm wave-length coverage, confirmation signal
Peak ownership.
For the separation chromatogram of the HPLC of embodiment 1 as shown in Figure 1, signal peak 1 is impurity peaks, signal peak 2 is gold orange II's
Signal peak, retention time are 24.4min or so, and the uv-visible absorption spectra of 2 component of signal peak is as shown in Fig. 2, signal peak 3
It is the signal peak of a pair of of isomer of auramine O with 4, retention time is respectively 25.4min and 27.3min or so, wherein believing
The uv-visible absorption spectra at number peak 3 is as shown in figure 3, signal 5 is the signal peak of Basic Orange.
Embodiment 2:
The detection method of Yellow Red coloring agent in a kind of corydalis tuber medicinal material, comprising the following steps:
1) take 2g sample to be tested, add the 50vt% ethyl alcohol of 25mL, be uniformly dispersed, filtered through 0.45 μm of filter membrane, obtain to
Survey solution；
2) through 0.45 μm of Teflon filtration film aspiration step 1) 10 μ L of standard solution, inject liquid chromatograph,
Detection wavelength is to be eluted under 420nm；
Chromatographic column: C18Reverse-phase chromatographic column；
Mobile phase: A acetonitrile；
The 0.05mol/L ammonium acetate solution of B glacial acetic acid containing 0.5vt%；
Elution program: t0-25min, mobile phase A is gradually increased to 55vt% by 2vt%；
t25-35min, the proportions constant of mobile phase A and Mobile phase B；
t35-37min, mobile phase A is gradually decreased to 2vt% by 55vt%；
t37-40min, the proportions constant of mobile phase A and Mobile phase B；
3) it is compared with the HPLC map of embodiment 1, if discovery absorbs in ± the 0.2min of standard reagent signal peak
Peak is checked using uv-visible absorption spectra.
In the corydalis tuber medicinal material that lot number is 20180503, the map of HPLC is excluded as shown in figure 4, signal peak 1 is impurity peaks
It is the suspicion of target coloration agent.Close signal peak 2 appears in 24.4min or so with the retention time of the gold orange II of embodiment 1,
Close signal peak 3 is in 25.5min or so with auramine O (1), and uv-visible absorption spectra is respectively shown in Fig. 5 and Fig. 6, by
The comparison of Fig. 5 and Fig. 2 is not it is found that the signal peak 2 of the corydalis tuber medicinal material of 20180503 batches is gold orange II；By the ratio of Fig. 6 and Fig. 3
Compared with it is found that uv-visible absorption spectra is different, the signal peak 3 of the corydalis tuber medicinal material of 20180503 batches is not auramine O, i.e. Fig. 4
In, absorption peak 1,2 and 3 is impurity peaks.
I.e. the corydalis tuber medicinal material of 20180503 batches is free of gold orange II, auramine O or Basic Orange.
In the corydalis tuber medicinal material that lot number is 20180620, the map of HPLC is excluded as shown in fig. 7, signal peak 1 is impurity peaks
It is the suspicion of target coloration agent.Close signal peak 2 appears in 24.4min or so with the retention time of the gold orange II of embodiment 1,
Close signal peak 3 is in 25.5min or so with the retention time of auramine O (1), uv-visible absorption spectra be respectively Fig. 8 and
Shown in Fig. 9, by the comparison of Fig. 8 and Fig. 2 it is found that the signal peak 2 of 20180620 batch corydalis tuber medicinal materials is not gold orange II；By Fig. 9
It is found that uv-visible absorption spectra is different compared with Fig. 3, the signal peak 3 of 20180620 batch corydalis tuber medicinal materials is not auramine
In O, Fig. 7, absorption peak 1,2 and 3 is impurity peaks.
I.e. the corydalis tuber medicinal material of 20180620 batches is free of gold orange II, auramine O or Basic Orange.
In the corydalis tuber medicinal material that lot number is 20180815, the map of HPLC is as shown in Figure 10, and signal peak 1 is impurity peaks, row
Except the suspicion for being target coloration agent.Close signal peak 2 appears in the left side 24.4min with the retention time of the gold orange II of embodiment 1
The right side, for close signal peak 3 in 25.5min or so, uv-visible absorption spectra is respectively to scheme with the retention time of auramine O (1)
Shown in 11 and Figure 12, by the comparison of Figure 11 and Fig. 2 it is found that the signal peak 2 of 20180815 batch corydalis tuber medicinal materials is not gold orange II；
By Figure 12 it is found that uv-visible absorption spectra is different compared with Fig. 3, the signal peak 3 of 20180815 batch corydalis tuber medicinal materials is not
It is auramine O, Tu10Zhong, absorption peak 1,2 and 3 is impurity peaks.
I.e. the corydalis tuber medicinal material of 20180815 batches is free of gold orange II, auramine O or Basic Orange.
The above embodiment is only the preferred embodiment of the present invention, and the scope of protection of the present invention is not limited thereto,
The variation and replacement for any unsubstantiality that those skilled in the art is done on the basis of the present invention belong to institute of the present invention
Claimed range.
Claims (10)
1. the detection method of Yellow Red coloring agent in a kind of medicinal material, comprising the following steps:
1) II standard reagent of gold orange, auramine O standard reagent and Basic Orange standard reagent are taken respectively, and 40-60vt% ethyl alcohol is added to dissolve,
Obtain standard solution；
2) sample to be tested is taken, is dispersed with step 1) with the ethyl alcohol of concentration, filters, obtains solution to be measured；
3) solution and standard solution to be measured are quantitatively pipetted, liquid chromatograph is injected separately into and is eluted；
The parameter of the liquid chromatograph are as follows:
Chromatographic column: C18Reverse-phase chromatographic column；
Mobile phase: A acetonitrile；
B 0.05mol/L ammonium acetate solution；
Elution program: t0-25min, mobile phase A is gradually increased to 50-60vt% by 2vt%；
t25-35min, the proportions constant of mobile phase A and Mobile phase B；
t35-37min, mobile phase A is gradually decreased to 2vt% by 50-60vt%；
t37-40min, the proportions constant of mobile phase A and Mobile phase B；
4) solution to be measured is compared the retention time at tracer signal peak with the HPLC map of standard solution, and doubtful peak uses
The more corresponding chromatographic peak of diode array detector is examined and determine in the uv-visible absorption spectra of 260-500nm wave-length coverage, is determined
Signal peak ownership.
2. the detection method of Yellow Red coloring agent in medicinal material as described in claim 1, in step 1), using the second of 50vt%
Alcohol.
3. the detection method of Yellow Red coloring agent in medicinal material as described in claim 1, in step 1), dispersing mode is shaking.
4. the detection method of Yellow Red coloring agent in medicinal material as described in claim 1, in step 2), using 0.45 μm of filter membrane
Filtering.
5. the detection method of Yellow Red coloring agent in medicinal material as claimed in claim 4, in step 2), the filter membrane is poly- four
Vinyl fluoride filter membrane.
6. the detection method of Yellow Red coloring agent in medicinal material as described in claim 1, in step 3), solution passes through before sample introduction
0.45 μm of filter membrane filtering.
7. the detection method of Yellow Red coloring agent in medicinal material as described in claim 1, in step 3), contain in Mobile phase B
0.5vt% glacial acetic acid.
8. the detection method of Yellow Red coloring agent in medicinal material as described in claim 1, in step 3), t0-25min, mobile phase A by
2vt% is gradually increased to 55vt%；t35-37min, mobile phase A is gradually decreased to 2vt% by 55vt%.
9. the detection method of Yellow Red coloring agent in medicinal material as described in claim 1, in step 3), the detection of liquid chromatograph
Device is DAD detector.
10. the detection method of Yellow Red coloring agent in medicinal material as claimed in claim 9, in step 3), Detection wavelength is
420nm。
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Citations (4)
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|---|---|---|---|---|
| UA9689U (en) * | 2005-03-09 | 2005-10-17 | Taras Shevchenko Kyiv Nat Univ | Method for determining content of lead |
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| CN107831233A (en) * | 2017-11-27 | 2018-03-23 | 蒙小翠 | The method that a variety of colouring agents synchronously detect in Chinese medicine preparation |
| CN108508110A (en) * | 2018-04-02 | 2018-09-07 | 新疆出入境检验检疫局检验检疫技术中心 | The assay method of a variety of disperse dyes in a kind of edible packing material |
-
2018
- 2018-12-21 CN CN201811571412.5A patent/CN109596733A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| UA9689U (en) * | 2005-03-09 | 2005-10-17 | Taras Shevchenko Kyiv Nat Univ | Method for determining content of lead |
| CN104749307A (en) * | 2015-01-26 | 2015-07-01 | 舟山市质量技术监督检测研究院 | Screening method for 43 artificial synthetic pigments in aquatic product |
| CN107831233A (en) * | 2017-11-27 | 2018-03-23 | 蒙小翠 | The method that a variety of colouring agents synchronously detect in Chinese medicine preparation |
| CN108508110A (en) * | 2018-04-02 | 2018-09-07 | 新疆出入境检验检疫局检验检疫技术中心 | The assay method of a variety of disperse dyes in a kind of edible packing material |
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》 * |
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