CN114235980A - Method for detecting content of flavonoid compounds in desmodium styracifolium extract - Google Patents
Method for detecting content of flavonoid compounds in desmodium styracifolium extract Download PDFInfo
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- CN114235980A CN114235980A CN202111355625.6A CN202111355625A CN114235980A CN 114235980 A CN114235980 A CN 114235980A CN 202111355625 A CN202111355625 A CN 202111355625A CN 114235980 A CN114235980 A CN 114235980A
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- vicenin
- schaftoside
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- 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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- G01N30/00—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
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- 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
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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Abstract
The invention provides a method for detecting the content of flavonoid compounds in a desmodium styracifolium extract, wherein the flavonoid compounds are selected from vicenin-2, vicenin-1, schaftoside, new schaftoside, isovitexin and vicenin-3, and the method comprises the following steps: performing liquid chromatography detection on the desmodium styracifolium extract, and determining the content of vicenin-2, vicenin-1, schaftoside, new schaftoside, 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 content of vicenin-2, vicenin-1, schaftoside, new schaftoside, isovitexin and vicenin-3 in the 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 promotes development and research of herba Desmodii Styracifolii medicinal value.
Description
Technical Field
The present invention relates to the field of medicine. Specifically, the invention relates to a method for detecting the content of flavonoid compounds in a 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 the desmodium styracifolium extract.
Background
Desmodium styracifolium is a leguminous plant, and dried overground part of Desmodium styracifolium (Osb.) Merr, is a traditional Chinese medicine collected in the first part of the 2020 edition of Chinese pharmacopoeia, and has the effects of promoting diuresis, removing jaundice, and inducing diuresis for treating stranguria. The main component of the collected formulated preparation, namely the herba Desmodii Styracifolii, is used for treating damp-heat in bladder, stranguria with stone, lithangiuria and urinary system infection which belong to damp-heat in liver, gall and bladder. The herba Desmodii Styracifolii extract is rich in flavonoids, and the flavonoids have extensive physiological activities of resisting oxidation, allergy, bacteria, mutation and tumor, protecting cardiovascular and cerebrovascular systems, resisting viruses and the like. The action characteristics of multiple components and multiple effects of the traditional Chinese medicine determine that the inherent quality of the traditional Chinese medicine is difficult to express by a single component. In the herba Desmodii Styracifolii extract, the main active ingredients of the flavonoid components are schaftoside, neoschaftoside vicenin-2, vicenin-1, vicenin-3 and isovitexin. Schaftoside can effectively produce anti-inflammatory effect; the vicenin-2, vicenin-1 and vicenin-3 have good antioxidant activity, and the pharmacological effects are greatly related to the components contained in the same. Therefore, at present, methods for determining the content of vicenin-2, vicenin-1, schaftoside, neoschaftoside, isovitexin and vicenin-3 in the desmodium styracifolium extract are still to be researched.
Disclosure of Invention
The present invention aims to solve at least to some extent at least one of the technical problems of the prior art. Therefore, the invention provides a method for detecting the content of vicenin-2, vicenin-1, schaftoside, new schaftoside, isovitexin and vicenin-3 in the desmodium styracifolium extract and a quality control method of the desmodium styracifolium extract or a medicine containing the desmodium styracifolium extract, and the method can be used for accurately determining the content of vicenin-2, vicenin-1, schaftoside, new schaftoside, isovitexin and vicenin-3 in the 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 promotes 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 a desmodium styracifolium extract. According to an embodiment of the invention, the method comprises: performing liquid chromatography detection on the desmodium styracifolium extract, and determining the content of vicenin-2, vicenin-1, schaftoside, new schaftoside, 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.
Researches find that the composition of the desmodium styracifolium extract (especially the extract rich in flavonoids) is dozens of complex, the characteristics of the substances are different, and how to effectively separate vicenin-2, vicenin-1, schaftoside, neoschaftoside, isovitexin and vicenin-3 from numerous components and know the content of the vicenin-2, the vicenin-1, the schaftoside, the isovitexin and the vicenin-3 is difficult. Therefore, the inventor of the invention finds that through a large number of experiments, when the detection is carried out by adopting liquid chromatography, the separation effect of vicenin-2, vicenin-1, schaftoside, new schaftoside, isovitexin and vicenin-3 can be obviously influenced by the types of mobile phases, and the problems of no peak appearance, improper peak appearance time, low separation degree with other components and the like easily occur due to improper mobile compatibility, so that the content determination of the 6 components is inaccurate. Furthermore, the inventor screens out the optimal mobile phase-trifluoroacetic acid aqueous solution and methanol as a mobile phase A and methanol as a mobile phase B through a large number of experiments, thereby being capable of accurately determining the content of vicenin-2, vicenin-1, schaftoside, new schaftoside, isovitexin and vicenin-3 in the desmodium styracifolium extract, having 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 promotes development and research of herba Desmodii Styracifolii medicinal value.
According to the embodiment of the invention, the method for detecting the content of vicenin-2, vicenin-1, schaftoside, new schaftoside, isovitexin and vicenin-3 in the desmodium styracifolium extract can also have the following additional technical characteristics:
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 the components can be improved, the peak shape of each component is good, the peak-off time is appropriate, and the accuracy of the detection result is further improved.
According to the embodiment of the invention, the liquid chromatography detection is carried out by adopting the elution mode of the following table:
| 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 indexes such as separation degree, retention time, accuracy, peak pattern and the like are ideal. For example, linear elution is carried out within 20min by using 100-95% (i.e., any value within the range) of mobile phase A and 0-5% of mobile phase B; 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 linearly eluted within 35-36 min; and isocratic elution is carried out within 36-45 min by adopting 100% of mobile phase A and 0% of mobile phase B.
According to the embodiment of the invention, the flow rate used in the liquid chromatography detection is 0.1-0.3 mL/min. Therefore, the separation of the compounds is facilitated, the separation degree is good, the separation effect is good, and the flow rate range can play a role 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, so that 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 ℃. Therefore, in the temperature range, the separation degree and the peak type such as half-peak width, peak height and the like are better, and the effect of overhigh temperature or overlow temperature is not ideal.
According to an embodiment of the present invention, the chromatographic column used in the liquid chromatography assay is selected from Waters acquisition BEH C18 chromatographic columns. The inventor obtains the chromatographic column through a large number of experiments, so that the accuracy and the separation degree of a detection result can be further improved, the peak types of the components are good, and the peak emergence time is appropriate.
According to an embodiment of the present invention, the method for obtaining the desmodium styracifolium extract comprises: heating and refluxing the desmodium styracifolium medicinal material by using ethanol so as to obtain an ethanol extract of the desmodium styracifolium; concentrating the alcohol extract to obtain a concentrate; and carrying out macroporous adsorption resin column treatment on the concentrated solution so as to obtain the desmodium styracifolium extract. Therefore, the extract rich in flavonoids can be obtained, the content of vicenin-2, vicenin-1, schaftoside, new schaftoside, isovitexin and vicenin-3 in the extract is high, the content of impurities is small, 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, particularly vicenin-2, vicenin-1, schaftoside, neoschaftoside, isovitexin and vicenin-3 can be obtained, and the impurity content is small, so that 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 for obtaining the desmodium styracifolium extract comprises: weighing a desmodium styracifolium medicinal material, adding 50-95% ethanol which is 8-14 times of the medicinal material, heating and refluxing at 50-60 ℃, extracting for 1-3 times for 1-3 hours each time to obtain an ethanol extract of the desmodium styracifolium, and then combining the ethanol extracts; concentrating the alcohol extract to 2-8 times of the medicinal material volume, standing and filtering to obtain a filtrate; enabling the filtrate to pass through an AB-8 macroporous adsorption resin column at a flow rate of 1-3 times of the volume of the bed per hour, after adsorption is finished, eluting with water with the amount of 8-12 times of the resin for removing impurities, and then eluting with ethanol with the amount of 40-95% of the volume of the bed of 6-10 times of the volume of the bed at a flow rate of 2-4 times of the volume of the bed per hour to obtain an eluent; and 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, particularly vicenin-2, vicenin-1, schaftoside, neoschaftoside, isovitexin and vicenin-3 can be obtained, and the impurity content is small, so that the chromatographic separation of the 6 components is facilitated, and the detection accuracy is improved.
According to the embodiment of the invention, before the liquid chromatography detection, an ethanol solution and the desmodium styracifolium extract are mixed and filtered by a filter membrane.
In another aspect of the present invention, the present invention provides a quality control method of desmodium styracifolium extract or a pharmaceutical composition containing the same. According to an embodiment of the invention, the method comprises: detecting the desmodium styracifolium extract by adopting the method for detecting the content of vicenin-2, vicenin-1, schaftoside, new schaftoside, isovitexin and vicenin-3 in the desmodium styracifolium extract to obtain the content of vicenin-2, vicenin-1, schaftoside, new schaftoside, isovitexin and vicenin-3; and respectively comparing and analyzing the contents of the vicenin-2, the vicenin-1, the schaftoside, the new schaftoside, the isovitexin and the vicenin-3 with respective corresponding threshold values to determine whether the quality of the desmodium styracifolium extract or the medicine reaches the standard.
As described above, the method according to the embodiment of the present invention can accurately determine the content of vicenin-2, vicenin-1, schaftoside, neoschaftoside, isovitexin, and vicenin-3 in the desmodium styracifolium extract or the drugs containing the desmodium styracifolium extract, and compare the determination results with the respective corresponding thresholds for analysis, thereby achieving quality control of the desmodium styracifolium extract or the drugs containing the desmodium styracifolium extract.
It should be noted that the "threshold" described in the present invention, that is, the "quality control line", is a condition value that needs to be satisfied by the requirement, for example, the total content of vicenin-2, vicenin-1, schaftoside, new schaftoside, isovitexin and vicenin-3 is not less than 60%, 70%, 80%, 90%, etc., and the specific parameters may be flexibly selected according to the actual production requirement, which is not strictly limited in the present invention.
It should be noted that, in the drug containing desmodium styracifolium extract, the ingredients of the other excipients except desmodium styracifolium extract are not strictly limited, and can be flexibly selected according to the actual needs, for example, lactose or microcrystalline cellulose can be used.
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 above and/or additional aspects and advantages of the present invention will become apparent and readily appreciated from the following description of the embodiments, taken in conjunction with the accompanying drawings of 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 mapping 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 of comparative example 1 according to the present invention;
fig. 6 shows a chromatogram of a test solution of comparative example 2 according to the present invention.
Detailed Description
The scheme of the invention will be explained with reference to the examples. It will be appreciated by those skilled in the art that the following examples are illustrative of the invention only and should not be taken as limiting the scope of the invention. The examples, where specific techniques or conditions are not indicated, are to be construed according to the techniques or conditions described in the literature in the art or according to the product specifications. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products commercially available.
Example 1
The invention provides a method for determining the content of vicenin-2, vicenin-1, schaftoside, new schaftoside, isovitexin and vicenin-3 in a desmodium styracifolium extract, which comprises the following steps:
1. preparation of control solutions:
respectively taking a proper amount of vicenin-2, vicenin-1, schaftoside, new schaftoside, vicenin-3 and isovitexin reference substances, precisely weighing, adding 25% methanol for dissolving, and preparing into mixed reference substance solutions containing vicenin-2, vicenin-1, schaftoside, new schaftoside, vicenin-3 and isovitexin with mass concentrations of 10 μ g/mL, 10 μ g/mL and 10 μ g/mL respectively for later use.
2. Preparation of a test solution:
taking 200 g of desmodium styracifolium medicinal material, adding 95% ethanol 14 times of the medicinal material for the first time, heating and refluxing for extraction at 60 ℃ for 3 hours, adding 95% ethanol 12 times of the medicinal material for the second time, heating and refluxing for extraction at 50 ℃ for 2 hours, adding 80% ethanol 8 times of the medicinal material for the third time, heating and refluxing for extraction at 50 ℃ for 1 hour, and combining ethanol extract; concentrating the ethanol extractive solution to a volume 8 times the volume of the medicinal materials, standing, and filtering to obtain filtrate (as sample liquid). 400 g of medicinal AB-8 type macroporous resin is soaked in proper amount of ethanol, and is packed into a column by a wet method for later use after treatment.
Enabling the filtrate (sample liquid medicine) to pass through an AB-8 macroporous adsorption resin column at the flow rate of 3 times of the volume of the column bed per hour, eluting with water of 12 times of the resin amount to remove impurities after adsorption is finished, and then eluting with 95% ethanol of 10 times of the volume of the column bed at the flow rate of 3 times of the volume of the column bed per hour to obtain an eluent; recovering ethanol from the eluate, concentrating to obtain concentrated solution with relative density of 1.10, drying at 75 deg.C under reduced pressure, and pulverizing to obtain herba Desmodii Styracifolii extract.
Weighing herba Desmodii Styracifolii extract about 20mg, precisely weighing, placing in 50ml measuring flask, adding 25% ethanol about 40ml, ultrasonically treating for 20min, cooling, diluting with 25% ethanol to scale, shaking, filtering with polytetrafluoroethylene organic system 0.22 μm filter membrane, discarding at least 3ml of primary filtrate, and collecting subsequent filtrate.
3. Ultra high performance liquid chromatography assay
Precisely sucking 1 μ l of each of the reference solution and the sample solution, injecting into an ultra-high performance liquid chromatograph, and measuring to obtain an ultra-high performance liquid chromatogram;
wherein, the chromatographic conditions are as follows:
a chromatographic column: waters ACQUITY BEH C18, 2.1 mm. times.100 mm,1.7 μm.
Mobile phase: methanol (90: 10) as a mobile phase A and methanol as a mobile phase B were used as a 0.5 vol% aqueous trifluoroacetic acid solution.
And (3) an 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: 0.2 mL/min; the column temperature is 60 ℃; detection wavelength: 330 nm; operating time: and (4) 45 min.
The theoretical plate number is not less than 20000 calculated by schaftoside.
4. Calculation of the content of the target Compound
Calculating C according to the relative correction factor by using the ultra-high performance liquid chromatogram obtained in the step 3 and taking schaftoside as an internal reference substanceiThe concentration of the component to be measured is calculated by the following formula
In the formula
AiIs the peak area of the component i to be detected in the test sample;
Cithe concentration of the component i to be detected in the test sample;
Asis the peak area of the internal reference substance s in the test sample;
Csthe concentration of the reference substance s in the test sample;
fsiand the correction factor of the internal reference substance s to the component i to be detected is obtained.
The contents of vicenin-2, vicenin-1, neoschaftoside, vicenin-3 and isovitexin are calculated by formula respectively.
The results are shown in fig. 1, fig. 2, table 1 and table 2, and it can be seen that the chromatographic peaks of vicenin-2, vicenin-1, neoschaftoside, vicenin-3, isovitexin and schaftoside are completely separated, and have a large separation degree (greater than 1.5), symmetrical peak shapes, high sensitivity, small tailing, and all can meet the quantitative detection requirements.
TABLE 1 relative Retention time and Relative Correction Factor (RCF)
TABLE 2 chromatogram analysis
Example 2
The detection was carried out according to the method of example 1, except that the ultra performance liquid chromatography conditions were as follows:
a chromatographic column: waters ACQUITY BEH C18, 2.1 mm. times.100 mm,1.7 μm.
Mobile phase: methanol (90: 10) as a mobile phase A and methanol as a mobile phase B were used as a 0.5 vol% aqueous trifluoroacetic acid solution.
And (3) an elution mode: isocratic elution, the ratio of mobile phase a to mobile phase B was 90: 10.
Flow rate: 0.2 mL/min; the column temperature is 60 ℃; detection wavelength: 330 nm; operating time: and (4) 45 min.
The theoretical plate number is not less than 20000 calculated by schaftoside.
The results are shown in fig. 3 (positioning solution), fig. 4 (test solution), table 3 and table 4, which show that the chromatographic peaks of vicenin-1, neoschaftoside, vicenin-3 and schaftoside are completely separated, and have relatively large separation degree (greater than 1.5), symmetrical peak shape, high sensitivity and small tailing, and can meet the quantitative detection requirement, and the separation degree of vicenin-2 and isovitexin is less than 1.5 and greater than 1.2, which shows that the separation effect is inferior to that of example 1, and the separation effect is 6 components.
TABLE 3 relative Retention time and Relative Correction Factor (RCF)
TABLE 4 chromatogram analysis
Comparative example 1
The detection was carried out according to the method of example 1, except that the ultra performance liquid chromatography conditions were as follows:
a chromatographic column: waters ACQUITY BEH C18, 2.1 mm. times.100 mm,1.7 μm.
Mobile phase: 0.5 vol% aqueous trifluoroacetic acid-acetonitrile (90: 10) as mobile phase A and methanol as mobile phase B.
And (3) an 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: 0.2 mL/min; the column temperature is 60 ℃; detection wavelength: 330 nm; operating time: and (4) 45 min.
The theoretical plate number is not less than 20000 calculated by schaftoside.
As can be seen from FIG. 5, the chromatographic peaks of vicenin-1, schaftoside and new schaftoside are completely separated, and have higher separation degree, higher theoretical plate number and higher sensitivity; however, the baseline of the peak shape positions of vicenin-2, vicenin-3 and isovitexin is uneven, the peak shape is not completely symmetrical, the tailing factor is large, the reproducibility is poor, the method uses methanol as a solvent of the mobile phase A, the baseline of the peak shape positions of vicenin-1 and isovitexin is flat, the peak shape is completely symmetrical, the tailing factor meets the requirement, and the reproducibility is good, namely the method is better.
Comparative example 2
The detection was carried out according to the method of example 1, except that the ultra performance liquid chromatography conditions were as follows:
a chromatographic column: waters ACQUITY BEH C18, 2.1 mm. times.100 mm,1.7 μm.
Mobile phase: 0.1 vol% formic acid was used as mobile phase a and methanol as mobile phase B.
And (3) an 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: 0.2 mL/min; the column temperature is 60 ℃; detection wavelength: 330 nm; operating time: and (4) 45 min.
The theoretical plate number is not less than 20000 calculated by 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 baselines of the peak shapes are uneven, the peak shapes are not completely symmetrical, the tailing factors are large, the reproducibility is poor, the method uses 0.5 volume of trifluoroacetic acid as the solvent of the mobile phase A, the baselines of the peak shapes of the vicenin-2, vicenin-1, schaftoside and new schaftoside are flat, the peak shapes are completely symmetrical, the tailing factors meet the requirements, and the reproducibility is good, namely the method is better.
In the description herein, references to the description of the term "one embodiment," "some embodiments," "an example," "a specific example," or "some examples," etc., mean 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 invention. In this specification, the schematic representations of the terms used above are not necessarily intended to refer 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, various embodiments or examples and features of different embodiments or examples described in this specification can be combined and combined by one skilled in the art without contradiction.
Although embodiments of the present invention have been shown and described above, it is understood that the above embodiments are exemplary and should not be construed as limiting the present invention, and that variations, modifications, substitutions and alterations can be made to the above embodiments by those of ordinary skill in the art within the scope of the present invention.
Claims (10)
1. A method for detecting the content of vicenin-2, vicenin-1, schaftoside, new schaftoside, isovitexin and vicenin-3 in a desmodium styracifolium extract is characterized by comprising the following steps of:
performing liquid chromatography detection on the desmodium styracifolium extract, and determining the content of vicenin-2, vicenin-1, schaftoside, new schaftoside, 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.
2. The method according to claim 1, wherein 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.
3. the method according to claim 1, wherein the liquid chromatography assay is performed using the following elution method:
。
4. The method according to claim 1, wherein the flow rate used in the liquid chromatography detection is 0.1-0.3 mL/min.
5. The method according to claim 1, wherein the detection wavelength used in the liquid chromatography detection is 300 to 350 nm.
6. The method according to claim 1, wherein the column temperature used in the liquid chromatography detection is 50 to 70 ℃.
7. The method according to claim 1, wherein the chromatographic column used in the liquid chromatography assay is selected from the group consisting of Waters acquisition BEH C18 chromatographic columns.
8. The method of claim 1, wherein obtaining the desmodium styracifolium extract comprises:
heating and refluxing the desmodium styracifolium medicinal material by using ethanol so as to obtain an ethanol extract of the desmodium styracifolium;
concentrating the alcohol extract to obtain a concentrate; and
subjecting the concentrated solution to macroporous adsorption resin column treatment so as to obtain the desmodium styracifolium extract;
optionally, the macroporous adsorbent resin is selected from AB-8 macroporous adsorbent resins;
optionally, the method of obtaining the desmodium styracifolium extract comprises:
weighing a desmodium styracifolium medicinal material, adding 50-95% ethanol which is 8-14 times of the medicinal material, heating and refluxing at 50-60 ℃, extracting for 1-3 times for 1-3 hours each time to obtain an ethanol extract of the desmodium styracifolium, and then combining the ethanol extracts;
concentrating the alcohol extract to 2-8 times of the medicinal material volume, standing and filtering to obtain a filtrate;
enabling the filtrate to pass through an AB-8 macroporous adsorption resin column at a flow rate of 1-3 times of the volume of the bed per hour, after adsorption is finished, eluting with water with the amount of 8-12 times of the resin for removing impurities, and then eluting with ethanol with the amount of 40-95% of the volume of the bed of 6-10 times of the volume of the bed at a flow rate of 2-4 times of the volume of the bed per hour to obtain an eluent;
and 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.
9. The method as claimed in claim 1, wherein the ethanol solution is mixed with the desmodium styracifolium extract and filtered with a filter membrane before the liquid chromatography detection is performed.
10. A quality control method of a desmodium styracifolium extract or a medicine containing the desmodium styracifolium extract is characterized by comprising the following steps:
detecting the desmodium styracifolium extract by using the method for detecting the content of vicenin-2, vicenin-1, schaftoside, new schaftoside, isovitexin and vicenin-3 in the desmodium styracifolium extract as claimed in any one of claims 1 to 9 to obtain the content of vicenin-2, vicenin-1, schaftoside, new schaftoside, isovitexin and vicenin-3;
and respectively comparing and analyzing the contents of the vicenin-2, the vicenin-1, the schaftoside, the new schaftoside, the isovitexin and the vicenin-3 with respective corresponding threshold values to determine whether the quality of the desmodium styracifolium extract or the medicine reaches the standard.
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