CN114235980B - Method for detecting flavonoid content in desmodium styracifolium extract - Google Patents
Method for detecting flavonoid content in desmodium styracifolium extract Download PDFInfo
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- schaftoside
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- 244000227573 Desmodium styracifolium Species 0.000 title claims abstract description 50
- 238000000034 method Methods 0.000 title claims abstract description 35
- 229930003935 flavonoid Natural products 0.000 title abstract description 12
- 235000017173 flavonoids Nutrition 0.000 title abstract description 12
- 150000002215 flavonoids Chemical class 0.000 title description 4
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- MMDUKUSNQNWVET-UHFFFAOYSA-N schaftozide Natural products OC1C(O)C(O)C(CO)OC1C1=C(O)C(C2C(C(O)C(O)CO2)O)=C(OC(=CC2=O)C=3C=CC(O)=CC=3)C2=C1O MMDUKUSNQNWVET-UHFFFAOYSA-N 0.000 claims abstract description 112
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- MYXNWGACZJSMBT-VJXVFPJBSA-N isovitexin Chemical compound O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@H]1C1=C(O)C=C(OC(=CC2=O)C=3C=CC(O)=CC=3)C2=C1O MYXNWGACZJSMBT-VJXVFPJBSA-N 0.000 claims abstract description 35
- MMDUKUSNQNWVET-MCIQUCDDSA-N vicenin-3 Chemical compound O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@H]1C1=C(O)C([C@H]2[C@@H]([C@@H](O)[C@H](O)CO2)O)=C(OC(=CC2=O)C=3C=CC(O)=CC=3)C2=C1O MMDUKUSNQNWVET-MCIQUCDDSA-N 0.000 claims abstract description 35
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- DTQVDTLACAAQTR-UHFFFAOYSA-N Trifluoroacetic acid Chemical compound OC(=O)C(F)(F)F DTQVDTLACAAQTR-UHFFFAOYSA-N 0.000 claims abstract description 28
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- G—PHYSICS
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- 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
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
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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
- G01N30/26—Conditioning of the fluid carrier; Flow patterns
- G01N30/28—Control of physical parameters of the fluid carrier
- G01N30/34—Control of physical parameters of the fluid carrier of fluid composition, e.g. gradient
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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
- G01N30/8675—Evaluation, i.e. decoding of the signal into analytical information
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Abstract
The invention provides a method for detecting the content of flavonoid compounds in desmodium styracifolium extract, wherein the flavonoid compounds are selected from vicenin-2, vicenin-1, schaftoside, neoschaftoside, isovitexin and vicenin-3, and the method comprises the following steps: detecting herba Desmodii Styracifolii extract by liquid chromatography, and determining vicenin-2, vicenin-1, schaftoside, neoschaftoside, isovitexin and vicenin-3 based on the detection result; wherein the mobile phase adopted in the liquid chromatography detection comprises a mobile phase A and a mobile phase B, and the mobile phase A is selected from trifluoroacetic acid aqueous solution and methanol; the mobile phase B is selected from methanol. The method can accurately determine the contents of vicenin-2, vicenin-1, schaftoside, neoschaftoside, isovitexin and vicenin-3 in desmodium styracifolium extract, and has the advantages of strong specificity, high accuracy, good reproducibility, high sensitivity, good durability and the like. The method can be used for quality control of herba Desmodii Styracifolii extract or medicine containing the same, and promote development and research of herba Desmodii Styracifolii medicinal value.
Description
Technical Field
The invention relates to the field of medicine. Specifically, the invention relates to a method for detecting the content of flavonoid compounds in desmodium styracifolium extract, and more specifically, the invention relates to a method for detecting the content of vicenin-2, vicenin-1, schaftoside, neoschaftoside, isovitexin and vicenin-3 in desmodium styracifolium extract.
Background
Herba Desmodii Styracifolii is a leguminous plant, and the dry aerial part of herba Desmodii Styracifolii Desmodium styracifolium (osb.) Merr. Is a traditional Chinese medicine loaded in the edition 2020 of Chinese pharmacopoeia, and has effects of promoting diuresis, removing jaundice, and inducing diuresis for treating strangurtia. The main component of the prescription preparation of the shilintong tablet is desmodium styracifolium which is used for treating damp-heat in bladder, stranguria and pain due to shilinding, urinary tract calculus and urinary infection which belongs to the damp-heat in liver and gall bladder. The desmodium styracifolium extract is rich in flavonoid compounds, and the flavonoid compounds have wide physiological activities of resisting oxidation, allergy, bacteria, mutation, tumor, heart and cerebral vascular system, virus, and the like. The multi-component and multi-effect characteristics of the traditional Chinese medicine determine that the inherent quality of the traditional Chinese medicine is difficult to express by a single component. For herba Desmodii Styracifolii extract, the main active ingredients of flavonoid components are schaftoside, neoschaftoside vicenin-2, vicenin-1, vicenin-3 and isovitexin. Schaftoside is effective in producing anti-inflammatory effects; vicenin-2, vicenin-1 and vicenin-3 have good antioxidant activity, and these pharmacological effects have a great relationship with the components contained therein. Thus, methods for the content of vicenin-2, vicenin-1, schaftoside, neoschaftoside, isovitexin and vicenin-3 in desmodium styracifolium extract are currently under investigation.
Disclosure of Invention
The present invention aims to solve at least one of the technical problems existing in the prior art to at least some extent. Therefore, the invention provides a method for detecting the contents of vicenin-2, vicenin-1, schaftoside, neoschaftoside, isovitexin and vicenin-3 in desmodium styracifolium extract and a quality control method of desmodium styracifolium extract or medicines containing desmodium styracifolium extract, and the contents of vicenin-2, vicenin-1, schaftoside, neoschaftoside, isovitexin and vicenin-3 in desmodium styracifolium extract can be accurately determined by using the method, so that the method has the advantages of strong specificity, high accuracy, good reproducibility, high sensitivity, good durability and the like. The method can be used for quality control of herba Desmodii Styracifolii extract or medicine containing the same, and promote development and research of herba Desmodii Styracifolii medicinal value.
In one aspect of the invention, the invention provides a method for detecting the content of vicenin-2, vicenin-1, schaftoside, neoschaftoside, isovitexin and vicenin-3 in desmodium styracifolium extract. According to an embodiment of the invention, the method comprises: detecting herba Desmodii Styracifolii extract by liquid chromatography, and determining vicenin-2, vicenin-1, schaftoside, neoschaftoside, isovitexin and vicenin-3 based on the detection result; wherein the mobile phase adopted in the liquid chromatography detection comprises a mobile phase A and a mobile phase B, and the mobile phase A is selected from trifluoroacetic acid aqueous solution and methanol; the mobile phase B is selected from methanol.
It was found that the components of desmodium styracifolium extract (especially flavonoid-rich extract) are as many as several tens, and are complex, and that there are differences in characteristics between the substances, and it is difficult to effectively separate vicenin-2, vicenin-1, schaftoside, neoschaftoside, isovitexin and vicenin-3 from the numerous components and to know the contents thereof. Therefore, the inventor of the invention finds that when liquid chromatography is adopted for detection, the types of mobile phases can obviously influence the separation effects of vicenin-2, vicenin-1, schaftoside, new schaftoside, isovitexin and vicenin-3, and the problems of no peak, improper peak time, low separation degree of other components and the like of the improper mobile phases easily occur, so that the content measurement of the 6 components is inaccurate. Furthermore, the inventor screens out the optimal mobile phase, namely trifluoroacetic acid aqueous solution and methanol as a mobile phase A and methanol as a mobile phase B through a large number of experiments, so that the contents of vicenin-2, vicenin-1, schaftoside, neoschaftoside, isovitexin and vicenin-3 in desmodium styracifolium extract can be accurately determined, and the method has the advantages of strong specificity, high accuracy, good reproducibility, high sensitivity, good durability and the like, and the detection limit can be as low as 0.5 mu g/ml-1.5 mu g/ml. The method can be used for quality control of herba Desmodii Styracifolii extract or medicine containing the same, and promote development and research of herba Desmodii Styracifolii medicinal value.
According to an embodiment of the present invention, the above method for detecting the content of vicenin-2, vicenin-1, schaftoside, neoschaftoside, isovitexin and vicenin-3 in desmodium styracifolium extract may further have the following additional technical features:
according to an embodiment of the present invention, the concentration of trifluoroacetic acid in the aqueous trifluoroacetic acid solution is 0.3 to 0.7% by volume; in the mobile phase A, the volume ratio of the trifluoroacetic acid aqueous solution to the methanol is (70-95): 10. therefore, the separation degree of each component can be improved, the peak shape of each component is good, the peak outlet time is proper, and the accuracy of the detection result is further improved.
According to an embodiment of the present invention, the liquid chromatography detection is performed by using the following elution modes:
| Time (min) | Mobile phase a (%) | Mobile phase B (%) |
| 0～20 | 100→95 | 0→5 |
| 20～30 | 95→89 | 5→11 |
| 30～35 | 89 | 11 |
| 35～36 | 89→100 | 11→0 |
| 36～45 | 100 | 0 |
Compared with isocratic elution, the gradient elution mode can obtain better separation effect, and the indexes such as separation degree, retention time, accuracy and peak value are ideal. For example, 100-95% (i.e., any value within this range) mobile phase A and 0-5% mobile phase B are used for linear elution within 20 min; linearly eluting by adopting 95-89% of mobile phase A and 5-11% of mobile phase B within 20-30 min; isocratic elution is carried out by adopting 89% of mobile phase A and 11% of mobile phase B within 30-35 min; 89% -100% of mobile phase A and 11% -0% of mobile phase B are eluted linearly within 35 min-36 min; isocratic elution is carried out by adopting 100% of mobile phase A and 0% of mobile phase B within 36-45 min.
According to the embodiment of the invention, the flow rate adopted in the liquid chromatography detection is 0.1-0.3 mL/min. Thus, the method is favorable for separating the compounds, has good separation degree and good separation effect, and can play a role in the flow rate range better than other flow rate ranges.
According to the embodiment of the invention, the detection wavelength adopted in the liquid chromatography detection is 300-350 nm. The inventor finds that the wavelength is adopted for detection, the absorption intensity is high, the detection sensitivity is high, and the effect is good.
According to the embodiment of the invention, the column temperature adopted in the liquid chromatography detection is 50-70 ℃. Thus, in this temperature range, the degree of separation and the peak width, peak height, etc. are preferable, and the effect of too high or too low a temperature is not preferable.
According to an embodiment of the present invention, the chromatographic column used in the liquid chromatography detection is selected from Waters ACQUITY BEH C chromatographic columns. The inventor obtains the chromatographic column through a large number of experiments, thereby further improving the accuracy and the separation degree of the detection result, and having good peak shape and proper peak time of each component.
According to an embodiment of the present invention, the method of obtaining the desmodium styracifolium extract comprises: reflux-heating herba Desmodii Styracifolii with ethanol to obtain ethanol extractive solution of herba Desmodii Styracifolii; concentrating the alcohol extract to obtain a concentrate; and subjecting the concentrate to macroporous adsorbent resin column treatment to obtain the desmodium styracifolium extract. Therefore, the extract rich in flavonoid compounds can be obtained, the contents of vicenin-2, vicenin-1, schaftoside, neoschaftoside, isovitexin and vicenin-3 in the extract are higher, the impurity content is smaller, and further the chromatographic separation of the 6 components is facilitated, and the detection accuracy is improved.
According to an embodiment of the invention, the macroporous adsorbent resin is selected from AB-8 macroporous adsorbent resins. Therefore, a large amount of flavonoid compounds, especially vicenin-2, vicenin-1, schaftoside, neoschaftoside, isovitexin and vicenin-3 can be obtained, the impurity content is small, the chromatographic separation of the 6 components is facilitated, and the detection accuracy is improved.
According to an embodiment of the present invention, the method of obtaining the desmodium styracifolium extract comprises: weighing herba Desmodii Styracifolii, adding 50% -95% ethanol with an amount which is 8-14 times that of the herba Desmodii Styracifolii, heating and refluxing at 50-60 ℃, extracting for 1-3 times and 1-3 hours each time to obtain an alcohol extract of herba Desmodii Styracifolii, and then merging the alcohol extracts; concentrating the alcohol extract to 2-8 times of the volume of the medicinal materials, standing and filtering to obtain filtrate; passing the filtrate through an AB-8 macroporous adsorption resin column at a flow rate of 1-3 times of the volume of the column bed per hour, after adsorption, eluting with 8-12 times of resin by water to remove impurities, eluting with 40-95% ethanol at a flow rate of 2-4 times of the volume of the column bed per hour to obtain eluent; concentrating the eluent to a concentrated solution with the relative density of 1.10-1.30, and drying and crushing the concentrated solution to obtain the desmodium styracifolium extract. Therefore, a large amount of flavonoid compounds, especially vicenin-2, vicenin-1, schaftoside, neoschaftoside, isovitexin and vicenin-3 can be obtained, the impurity content is small, the chromatographic separation of the 6 components is facilitated, and the detection accuracy is improved.
According to an embodiment of the present invention, the ethanol solution is mixed with the desmodium styracifolium extract and filtered through a filter membrane before the liquid chromatography detection is performed.
In another aspect of the invention, the invention provides a quality control method of desmodium styracifolium extract or a medicament containing desmodium styracifolium extract. According to an embodiment of the invention, the method comprises: detecting the desmodium styracifolium extract by adopting the method for detecting the vicenin-2, vicenin-1, schaftoside, neoschaftoside, isovitexin and vicenin-3 content in the desmodium styracifolium extract to obtain vicenin-2, vicenin-1, schaftoside, neoschaftoside, isovitexin and vicenin-3 content; and respectively comparing the vicenin-2, vicenin-1, schaftoside, neoschaftoside, isovitexin and vicenin-3 contents with respective corresponding thresholds, and determining whether the quality of the desmodium styracifolium extract or medicine meets the standard.
As described above, the method according to the embodiment of the present invention can accurately determine the contents of vicenin-2, vicenin-1, schaftoside, neoschaftoside, isovitexin and vicenin-3 in desmodium styracifolium extract or a drug containing the same, and compare the measurement results with respective corresponding thresholds for analysis, thereby realizing quality control of desmodium styracifolium extract or a drug containing the same.
It should be noted that, the "threshold value" described in the present invention, that is, the "quality control line", is a condition value that needs to be satisfied when the requirement is met, for example, vicenin-2, vicenin-1, schaftoside, neoschaftoside, isovitexin, vicenin-3, and the total content of these components is not less than 60%, 70%, 80%, 90%, etc., and specific parameters can be flexibly selected according to actual production requirements, and the present invention is not strictly limited.
In addition, in the medicine containing desmodium styracifolium extract, other auxiliary materials except desmodium styracifolium extract are not strictly limited, and can be flexibly selected according to actual needs, for example, lactose and microcrystalline cellulose.
Additional aspects and advantages of the invention will be set forth in part in the description which follows, and in part will be obvious from the description, or may be learned by practice of the invention.
Drawings
The foregoing and/or additional aspects and advantages of the invention will become apparent and may be better understood from the following description of embodiments taken in conjunction with the accompanying drawings in which:
FIG. 1 shows a chromatogram of a test solution according to example 1 of the present invention;
FIG. 2 shows a chromatogram of a control solution according to example 1 of the present invention;
FIG. 3 shows a localization solution chromatogram according to example 2 of the present invention;
FIG. 4 shows a chromatogram of a test solution according to example 2 of the present invention;
FIG. 5 shows a chromatogram of a test solution according to comparative example 1 of the present invention;
FIG. 6 shows a chromatogram of a test solution according to comparative example 2 of the present invention.
Detailed Description
The scheme of the present invention will be explained below with reference to examples. It will be appreciated by those skilled in the art that the following examples are illustrative of the present invention and should not be construed as limiting the scope of the invention. The examples are not to be construed as limiting the specific techniques or conditions described in the literature in this field or as per the specifications of the product. The reagents or apparatus used were conventional products commercially available without the manufacturer's attention.
Example 1
The invention provides a method for preparing the contents of vicenin-2, vicenin-1, schaftoside, neoschaftoside, isovitexin and vicenin-3 in desmodium styracifolium extract, which comprises the following steps:
1. Preparation of a control solution:
And respectively taking a proper amount of control substances of vicenin-2, vicenin-1, schaftoside, new schaftoside, vicenin-3 and isovitexin, precisely weighing, adding 25% of methanol for dissolving, and preparing mixed control substance solutions containing vicenin-2, vicenin-1, schaftoside, new schaftoside, vicenin-3 and isovitexin with mass concentrations of 10 mug/mL, 10 mug/mL and 10 mug/mL for later use.
2. Preparation of test solution:
taking 200 g of desmodium styracifolium, firstly adding 95% ethanol with the amount of 14 times that of the desmodium styracifolium, heating and reflux-extracting for 3 hours at 60 ℃, secondly adding 95% ethanol with the amount of 12 times that of the desmodium styracifolium, heating and reflux-extracting for 2 hours at 50 ℃, thirdly adding 80% ethanol with the amount of 8 times that of the desmodium styracifolium, heating and reflux-extracting for 1 hour at 50 ℃, and combining alcohol extracts; concentrating the ethanol extract to a certain volume to make the volume of the liquid medicine 8 times of the amount of the medicinal materials, standing and filtering to obtain filtrate (as sample liquid medicine) for standby. 400 g of medical AB-8 macroporous resin is soaked in proper amount of ethanol, packed by a wet method, and treated for standby.
Passing the filtrate (sample liquid medicine) through an AB-8 macroporous adsorption resin column at a flow rate of 3 times of the volume of the bed per hour, eluting with 12 times of water to remove impurities, eluting with 10 times of 95% ethanol at a flow rate of 3 times of the volume of the bed per hour after adsorption is finished, and obtaining eluent; recovering ethanol from the eluate, concentrating to obtain concentrated solution with relative density of 1.10, drying at 75deg.C under reduced pressure, and pulverizing to obtain herba Desmodii Styracifolii extract.
About 20mg of desmodium styracifolium extract is taken, precisely weighed, placed in a 50ml measuring flask, added with about 40ml of 25% ethanol, subjected to ultrasonic treatment for 20min, cooled, diluted to a scale with 25% ethanol, uniformly shaken, filtered by a polytetrafluoroethylene organic system 0.22 mu m filter membrane, and at least removed from 3ml of primary filtrate, and the subsequent filtrate is taken to obtain the desmodium styracifolium extract.
3. Ultra-high performance liquid chromatography assay
Precisely sucking 1 μl of each of the reference solution and the sample solution, and injecting into an ultra-high performance liquid chromatograph for measurement to obtain an ultra-high performance liquid chromatogram;
wherein, the chromatographic conditions are as follows:
Chromatographic column: waters ACQUITY BEH C18,2.1 mm. Times.100 mm,1.7 μm.
Mobile phase: 0.5% by volume aqueous trifluoroacetic acid in methanol (90:10) as mobile phase A and methanol as mobile phase B.
Elution mode: the following gradient elution conditions were used:
| Time (min) | Mobile phase a (%) | Mobile phase B (%) |
| 0～20 | 100→95 | 0→5 |
| 20～30 | 95→89 | 5→11 |
| 30～35 | 89 | 11 |
| 35～36 | 89→100 | 11→0 |
| 36～45 | 100 | 0 |
Flow rate: 0.2mL/min; column temperature is 60 ℃; detection wavelength: 330nm; run time: 45min.
The theoretical plate number should be not less than 20000 calculated as schaftoside.
4. Calculation of the content of the target Compound
Using the ultra-high performance liquid chromatogram obtained in step 3, and using schaftoside as internal reference, calculating C i as the concentration of the component to be detected according to the relative correction factor, wherein the calculation formula is as follows
In the middle of
A i is the peak area of the component i to be detected in the sample;
c i is the concentration of the component i to be detected in the sample;
A s is the peak area of the internal reference substance s in the sample;
C s is the concentration of the internal reference substance s in the sample;
And f si is the correction factor of the internal reference s to the component i to be detected.
The contents of vicenin-2, vicenin-1, new schaftoside, vicenin-3 and isovitexin are calculated according to the formula respectively.
The results are shown in fig. 1, fig. 2, table 1 and table 2, and can be seen that vicenin-2, vicenin-1, novel schaftoside, vicenin-3, isovitexin and schaftoside have chromatographic peaks which are completely separated, have larger separation degree (more than 1.5), symmetrical peak shape, high sensitivity and small tailing, and can meet the quantitative detection requirement.
TABLE 1 relative retention time and Relative Correction Factor (RCF)
Table 2 chromatogram analysis
Example 2
The test was performed as in example 1, except that the conditions of the ultra high performance liquid chromatography were as follows:
Chromatographic column: waters ACQUITY BEH C18,2.1 mm. Times.100 mm,1.7 μm.
Mobile phase: 0.5% by volume aqueous trifluoroacetic acid in methanol (90:10) as mobile phase A and methanol as mobile phase B.
Elution mode: isocratic elution, mobile phase A and mobile phase B ratio of 90:10.
Flow rate: 0.2mL/min; column temperature is 60 ℃; detection wavelength: 330nm; run time: 45min.
The theoretical plate number should be not less than 20000 calculated as schaftoside.
The results are shown in FIG. 3 (positioning solution), FIG. 4 (sample solution), table 3 and Table 4, and can be seen that the chromatographic peaks of vicenin-1, novel schaftoside, vicenin-3 and schaftoside are completely separated, and the chromatographic peaks have larger separation degree (more than 1.5) and symmetrical peak shape, high sensitivity and small tailing, can meet the quantitative detection requirement, and the separation degree of vicenin-2 and isovitexin is lower than 1.5 and higher than 1.2, so that the purposes of detecting 6 components can be realized, but the separation effect is not as good as that of the embodiment 1.
TABLE 3 relative retention time and Relative Correction Factor (RCF)
Table 4 chromatogram analysis
Comparative example 1
The test was performed as in example 1, except that the conditions of the ultra high performance liquid chromatography were as follows:
Chromatographic column: waters ACQUITY BEH C18,2.1 mm. Times.100 mm,1.7 μm.
Mobile phase: 0.5% by volume aqueous trifluoroacetic acid in acetonitrile (90:10) as mobile phase A and methanol as mobile phase B.
Elution mode: the following gradient elution conditions were used:
| Time (min) | Mobile phase a (%) | Mobile phase B (%) |
| 0～20 | 100→95 | 0→5 |
| 20～30 | 95→89 | 5→11 |
| 30～35 | 89 | 11 |
| 35～36 | 89→100 | 11→0 |
| 36～45 | 100 | 0 |
Flow rate: 0.2mL/min; column temperature is 60 ℃; detection wavelength: 330nm; run time: 45min.
The theoretical plate number should be not less than 20000 calculated as schaftoside.
As can be seen from FIG. 5, the chromatographic peaks of vicenin-1, schaftoside and neoschaftoside are completely separated, and the chromatographic peaks have high separation degree, theoretical plate number and sensitivity; however, the base lines of the peak shapes of vicenin-2, vicenin-3 and isovitexin are uneven, the peak shapes are not completely symmetrical, the tailing factor is larger, the reproducibility is poor, methanol is used as a solvent of a mobile phase A, the base lines of the peak shapes of vicenin-1 and isovitexin are flat, the peak shapes are completely symmetrical, the tailing factor meets the requirements, and the reproducibility is good, namely the method is better.
Comparative example 2
The test was performed as in example 1, except that the conditions of the ultra high performance liquid chromatography were as follows:
Chromatographic column: waters ACQUITY BEH C18,2.1 mm. Times.100 mm,1.7 μm.
Mobile phase: 0.1% by volume of formic acid is mobile phase A and methanol is mobile phase B.
Elution mode: the following gradient elution conditions were used:
| Time (min) | Mobile phase a (%) | Mobile phase B (%) |
| 0～20 | 100→95 | 0→5 |
| 20～30 | 95→89 | 5→11 |
| 30～35 | 89 | 11 |
| 35～36 | 89→100 | 11→0 |
| 36～45 | 100 | 0 |
Flow rate: 0.2mL/min; column temperature is 60 ℃; detection wavelength: 330nm; run time: 45min.
The theoretical plate number should be not less than 20000 calculated as schaftoside.
As can be seen from FIG. 6, the chromatographic peaks of vicenin-2, vicenin-1, schaftoside and new schaftoside are not completely separated, the base line at the peak is uneven, the peak is not completely symmetrical, the tailing factor is larger, the reproducibility is poor, 0.5 volume of trifluoroacetic acid is used as the solvent of the mobile phase A, the base line at the peak of vicenin-2, vicenin-1, schaftoside and new schaftoside is flat, the peak is completely symmetrical, the tailing factor meets the requirements, and the reproducibility is good, namely the method is better.
In the description of the present specification, a description referring to terms "one embodiment," "some embodiments," "examples," "specific examples," or "some examples," etc., means that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the present invention. In this specification, schematic representations of the above terms are not necessarily directed to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Furthermore, the different embodiments or examples described in this specification and the features of the different embodiments or examples may be combined and combined by those skilled in the art without contradiction.
While embodiments of the present invention have been shown and described above, it will be understood that the above embodiments are illustrative and not to be construed as limiting the invention, and that variations, modifications, alternatives and variations may be made to the above embodiments by one of ordinary skill in the art within the scope of the invention.
Claims (4)
1. A method for detecting the content of vicenin-2, vicenin-1, schaftoside, neoschaftoside, isovitexin and vicenin-3 in desmodium styracifolium extract, comprising:
detecting herba Desmodii Styracifolii extract by liquid chromatography, and determining vicenin-2, vicenin-1, schaftoside, neoschaftoside, isovitexin and vicenin-3 based on the detection result;
wherein the mobile phase adopted in the liquid chromatography detection comprises a mobile phase A and a mobile phase B,
The mobile phase A is selected from trifluoroacetic acid aqueous solution and methanol;
The mobile phase B is selected from methanol;
The concentration of trifluoroacetic acid in the aqueous trifluoroacetic acid solution is 0.5% by volume;
in the mobile phase A, the volume ratio of the trifluoroacetic acid aqueous solution to the methanol is 90:10;
the liquid chromatography detection is carried out by adopting the elution mode of the following table:
；
The chromatographic column adopted in the liquid chromatography detection is selected from Waters ACQUITY BEH C chromatographic columns, 2.1mm multiplied by 100mm and 1.7 mu m; the flow rate is 0.2mL/min; the detection wavelength is 330nm; column temperature is 60 ℃;
the method for obtaining the desmodium styracifolium extract comprises the following steps:
Reflux-heating herba Desmodii Styracifolii with ethanol to obtain ethanol extractive solution of herba Desmodii Styracifolii;
concentrating the alcohol extract to obtain a concentrate; and
Subjecting the concentrate to macroporous adsorbent resin column treatment to obtain the desmodium styracifolium extract;
The macroporous adsorption resin is selected from AB-8 macroporous adsorption resin, and in the macroporous adsorption resin column treatment, water is used for eluting and removing impurities, and 40% -95% of ethanol is used for eluting.
2. The method of claim 1, wherein the method of obtaining the desmodium styracifolium extract comprises:
Weighing herba Desmodii Styracifolii, adding 50% -95% ethanol with an amount which is 8-14 times that of the herba Desmodii Styracifolii, heating and refluxing at 50-60 ℃, extracting for 1-3 times and 1-3 hours each time to obtain an alcohol extract of herba Desmodii Styracifolii, and then merging the alcohol extracts;
concentrating the alcohol extract to 2-8 times of the volume of the medicinal materials, standing and filtering to obtain filtrate;
Passing the filtrate through an AB-8 macroporous adsorption resin column at a flow rate of 1-3 times of the volume of the column bed per hour, after adsorption, eluting with 8-12 times of resin by water to remove impurities, eluting with 40-95% ethanol at a flow rate of 2-4 times of the volume of the column bed per hour to obtain eluent;
Concentrating the eluent to a concentrated solution with the relative density of 1.10-1.30, and drying and crushing the concentrated solution to obtain the desmodium styracifolium extract.
3. The method of claim 1, wherein prior to performing the liquid chromatography test, an ethanol solution is mixed with the desmodium styracifolium extract and filtered through a filter.
4. A quality control method of desmodium styracifolium extract or a medicament containing desmodium styracifolium extract, comprising:
Detecting the desmodium styracifolium extract by the method for detecting the content of vicenin-2, vicenin-1, schaftoside, neoschaftoside, isovitexin and vicenin-3 in the desmodium styracifolium extract according to any one of claims 1-3 to obtain the content of vicenin-2, vicenin-1, schaftoside, neoschaftoside, isovitexin and vicenin-3;
And respectively comparing the vicenin-2, vicenin-1, schaftoside, neoschaftoside, isovitexin and vicenin-3 contents with respective corresponding thresholds, and determining whether the quality of the desmodium styracifolium extract or medicine meets the standard.
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