CN111579693A - Method for measuring content of main effective components in antiviral cold traditional Chinese medicine preparation - Google Patents
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Abstract
The invention relates to a method for measuring the content of main effective components in an antiviral cold traditional Chinese medicine preparation, wherein the antiviral cold traditional Chinese medicine preparation comprises scutellaria baicalensis, honeysuckle, fructus forsythiae, folium isatidis, lophatherum gracile, liquorice extract, dextrin, burdock, peppermint oil, calculus bovis factitius and auxiliary materials, and the method for measuring the content comprises the following steps: s1, preparing a reference solution, S2, preparing a test solution, S3 and measuring the content. The method for measuring the contents of the baicalin and the chlorogenic acid has the advantages of simple pretreatment, simplicity, convenience, sensitivity, stability, reliability and the like, and the obtained ultra-high performance liquid chromatogram calculates the concentrations of the baicalin and the chlorogenic acid through a regression equation, so that the quality information of the product is reflected, and the method is favorable for monitoring the quality of the product and identifying the authenticity.
Description
Technical Field
The invention relates to the technical field of drug analysis and detection, in particular to a method for measuring the content of main effective components in a traditional Chinese medicine preparation for resisting viral influenza.
Background
The prescription of the Chinese medicinal preparation for resisting the viral cold consists of 9 Chinese medicaments such as scutellaria baicalensis, honeysuckle and the like, wherein the scutellaria baicalensis and the honeysuckle are monarch medicaments of the prescription, and the baicalin and the chlorogenic acid are respectively main effective components of the scutellaria baicalensis and the honeysuckle, but a simple, convenient, sensitive, stable and reliable method for measuring the content of the baicalin or the chlorogenic acid is not provided at present. Therefore, the method for measuring the content of the baicalin and the chlorogenic acid by the ultra-high performance liquid chromatography is simple, convenient, sensitive, stable and reliable, and can be used as the quality control standard of the antiviral cold traditional Chinese medicine preparation.
Disclosure of Invention
The invention aims to provide a method for measuring the content of main effective components in a traditional Chinese medicine preparation for resisting viral cold, aiming at the defects in the prior art.
In order to achieve the purpose, the invention adopts the technical scheme that:
the method for measuring the content of main effective components in the antiviral cold traditional Chinese medicine preparation is provided, the antiviral cold traditional Chinese medicine preparation comprises scutellaria baicalensis, honeysuckle, fructus forsythiae, folium isatidis, lophatherum gracile, liquorice extract, dextrin, fructus arctii, peppermint oil, calculus bovis factitius and auxiliary materials, and the method for measuring the content comprises the following steps:
s1, preparing a reference solution: precisely weighing a reference substance, adding 50-100% methanol, and shaking up to obtain a reference substance solution with the concentration of 45-70 μ g/mL;
s2, preparing a test solution: precisely weighing the antiviral cold traditional Chinese medicine preparation, adding 50-70% methanol, performing ultrasonic extraction for 15-60min, cooling, adding 50-70% methanol, shaking, filtering, and collecting the filtrate to obtain a sample solution with concentration of 2-5 mg/mL;
s3, content determination: respectively and precisely sucking 10 mu L of the reference solution and the test solution respectively, and injecting the reference solution and the test solution into an ultra-high performance liquid chromatograph for measurement.
Preferably, when the main effective ingredient is baicalin, step S3 of the method for measuring baicalin content includes:
respectively and precisely sucking 10 mu L of each of the reference solution and the test solution, and injecting the reference solution and the test solution into an ultra-high performance liquid chromatograph for measurement, wherein the chromatographic measurement conditions are as follows: adopting welchrom-C18 chromatographic column, 4.6mm × 250mm, 5 μm, and the number of theoretical plates is 1000 according to baicalin peak; methanol-0.4% phosphoric acid solution is used as a mobile phase; the flow rate is 1.0 mL/min; the detection wavelength was 280 nm.
Preferably, the mobile phase volume is 48% of the methanol and 52% of the 0.4% phosphoric acid.
Preferably, the ultrasound extraction time is 30 min.
Preferably, the concentration of baicalin is linear with the peak area; and taking the concentration of the baicalin as an abscissa, the area of the baicalin peak as an ordinate, and the regression equation of the baicalin concentration standard curve is that Y is 40787X-60834.
Preferably, when the main effective ingredient is chlorogenic acid, step S3 of the method for measuring a content of chlorogenic acid comprises:
respectively and precisely sucking 10 mu L of each of the reference solution and the test solution, and injecting the reference solution and the test solution into an ultra-high performance liquid chromatograph for measurement, wherein the chromatographic measurement conditions are as follows: adopting an Eilide C18 chromatographic column with the size of 4.6mm multiplied by 25cm and the size of 5 mu m, wherein the number of theoretical plates is 1000 according to the peak of chlorogenic acid; adopting acetonitrile-0.4% phosphoric acid solution as mobile phase; the flow rate is 1.0 mL/min; the detection wavelength was 327 nm.
Preferably, the volume of the mobile phase is 10% of the acetonitrile and 90% of the 0.4% phosphoric acid.
Preferably, the ultrasound extraction time is 30 min.
Preferably, the concentration of the chlorogenic acid is in a linear relation with the peak area thereof, the peak area of the chlorogenic acid is used as an abscissa, the concentration of the chlorogenic acid is used as an ordinate, and the regression equation of the standard curve of the concentration of the chlorogenic acid is that Y is 3.2605 × 10-7X-0.02946。
By adopting the technical scheme, compared with the prior art, the invention has the following technical effects:
the method for measuring the contents of the baicalin and the chlorogenic acid has the advantages of simple pretreatment, simplicity, convenience, sensitivity, stability, reliability and the like, and the obtained ultra-high performance liquid chromatogram calculates the concentrations of the baicalin and the chlorogenic acid through a regression equation, so that the quality information of the product is reflected, and the method is favorable for monitoring the quality of the product and identifying the authenticity.
Drawings
FIG. 1 is an ultra high performance liquid chromatogram of a baicalin control solution;
FIG. 2 is an ultra-high performance liquid chromatogram of baicalin in the test solution of the antiviral cold Chinese medicinal preparation;
FIG. 3 is an ultra-high performance liquid chromatogram of a solution without a negative control of Scutellaria baicalensis.
FIG. 4 is an ultra high performance liquid chromatogram of a chlorogenic acid control solution;
FIG. 5 is an ultra-high performance liquid chromatogram of chlorogenic acid in the test solution of the antiviral cold Chinese medicinal preparation;
FIG. 6 is an ultra-high performance liquid chromatogram of a solution without a negative control of Lonicera japonica;
FIG. 7 is a chlorogenic acid peak UV absorption spectrum in a chlorogenic acid reference solution ultra-high performance liquid chromatogram;
FIG. 8 is an ultraviolet absorption spectrum of a chlorogenic acid peak in an ultra-high performance liquid chromatogram of a test solution of the antiviral cold Chinese medicinal preparation;
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
It should be noted that the embodiments and features of the embodiments may be combined with each other without conflict.
The invention is further described with reference to the following drawings and specific examples, which are not intended to be limiting.
Example 1
The embodiment provides a method for measuring the content of main effective components in an antiviral cold traditional Chinese medicine preparation, wherein the antiviral cold traditional Chinese medicine preparation comprises scutellaria baicalensis, honeysuckle, fructus forsythiae, folium isatidis, lophatherum gracile, liquorice extract, dextrin, fructus arctii, peppermint oil, calculus bovis factitius and auxiliary materials, and the method for measuring the content comprises the following steps:
s1, preparing a reference solution: precisely weighing a reference substance, adding 50-100% methanol, and shaking up to obtain a reference substance solution with the concentration of 45-70 μ g/mL;
s2, preparing a test solution: precisely weighing the antiviral cold Chinese medicinal preparation, adding 50-70% methanol, ultrasonic extracting for 15-60min, cooling, adding 50-70% methanol, shaking, filtering, and collecting filtrate to obtain sample solution with concentration of 2-5 mg/mL;
s3, content determination: precisely sucking 10 μ L of each of the reference solution and the sample solution, and injecting into an ultra high performance liquid chromatograph for measurement.
The content determination method has the advantages of simple pretreatment, simplicity, sensitivity, stability, reliability and the like.
Example 2
The embodiment provides a method for measuring the content of main effective components in a traditional Chinese medicine preparation for resisting viral cold, wherein the main effective component of the traditional Chinese medicine preparation for resisting viral cold is baicalin, and the method for measuring the content of the baicalin comprises the following steps:
s1, preparing a reference solution: accurately weighing baicalin reference substance, adding methanol, and shaking to obtain reference substance solution with concentration of 60 μ g/mL;
s2, preparing a test solution: precisely weighing the antiviral Chinese medicinal preparation for treating common cold, adding 70% methanol, ultrasonic extracting for 30min, cooling, adding 70% methanol, shaking, filtering, and collecting filtrate to obtain 3mg/mL test solution;
s3, content determination: precisely sucking 10 μ L of each of the reference solution and the sample solution, and injecting into an ultra high performance liquid chromatograph for measurement under the following chromatographic measurement conditions: adopting welchrom-C18 chromatographic column, 4.6mm × 250mm, 5 μm, and the number of theoretical plates is 1000 according to baicalin peak; methanol-0.4% phosphoric acid solution is used as a mobile phase; the flow rate is 1.0 mL/min; the detection wavelength was 280 nm.
Preferably, the mobile phase is 48% by volume of the methanol and 52% by volume of the 0.4% phosphoric acid.
Preferably, the concentration of the baicalin is in a linear relation with the peak area; and taking the concentration of the baicalin as an abscissa and the area of the baicalin peak as an ordinate, wherein the regression equation of the baicalin concentration standard curve is that Y is 40787X-60834.
Detection example 1
(1) Determination of extraction time
And comparing the extraction rates of the antiviral cold traditional Chinese medicine preparation obtained by ultrasonic and reflux extraction with 70% ethanol and ultrasonic and reflux extraction with methanol for 30 minutes and 60 minutes. The results are shown in table 1, and the ultrasonic extraction rate of 70% ethanol is high; the extraction rates of the ultrasonic extraction for 30 minutes and 60 minutes were substantially the same. Therefore, the preparation of the sample solution of the test sample is determined by ultrasonic extraction with 70% ethanol for 30 minutes.
TABLE 1 measurement results of different ultrasonic extraction times of test samples
(2) Precision test
According to the method, 0.30056g (batch number is S20090401) of the antiviral cold traditional Chinese medicine preparation is precisely weighed, a test sample solution is prepared according to the method, sample introduction is repeated for 6 times on an instrument, the peak area is measured, and the baicalin content result is calculated. The results of statistics of peak area and baicalin content are shown in table 2, the average value of peak area is 3225630.85, and RSD% is 0.66%.
TABLE 2 precision test
(3) Stability test
According to the method, 0.30056g of the antiviral cold traditional Chinese medicine preparation (batch number is S20090401) is precisely weighed, a sample solution is prepared according to the method, the sample is injected and measured for 1 time every 2 hours, the measurement is repeated for 6 times, the measurement lasts for 12 hours, the baicalin peak area is recorded, and the baicalin content result is calculated. The results of statistics of peak area and baicalin content are shown in table 3, the average value of peak area is 3225630.85, and RSD% is 2.1. The result shows that the sample solution is basically stable when the measurement is carried out for 12 hours.
TABLE 3 stability test
(4) Reproducibility test
According to the method, 6 parts of the antiviral cold traditional Chinese medicine preparation (batch number is S20090401) are precisely weighed, sample solutions are respectively prepared according to the method, and the sample injection is respectively carried out on an instrument for determination. The results of the content measurement of 6 samples are shown in table 4, where RSD% is 0.37 and the average peak area is 2656292.9.
TABLE 4 reproducibility test
(5) Investigation of linear relation and determination of measurement calculation method
Precisely weighing 0.01746g of baicalin reference substance, placing in a 100ml volumetric flask, adding methanol to scale, and shaking to obtain 174.6 μ g/ml reference substance solution. Diluting into baicalin reference substance solutions with different concentrations according to the proportion, and recording the peak areas of the baicalin reference substances with different concentrations according to the chromatographic conditions. The results are shown in Table 5, and the concentration of the control is plotted on the abscissa and the peak area is plotted on the ordinate to obtain a standard curve, wherein the regression equation is that Y is 40787X-60834, R20.9992, the baicalin concentration is better in linear relationship between 50. mu.g/mL and 160. mu.g/mL.
TABLE 5 Linear relationship between baicalin peak area and baicalin concentration
| Control concentration (μ g/mL) | Peak area |
| 49.89 | 2019812.75 |
| 58.2 | 2341545.5 |
| 74.83 | 3039505.5 |
| 87.3 | 3481889 |
| 104.76 | 4227381 |
| 166.28 | 6736387.5 |
(6) Recovery test
Precisely weighing 6 parts of the antiviral cold traditional Chinese medicine preparation with the content of 42.22mg/g in the same batch (S20090401), respectively placing the 6 parts in 6 100ml volumetric flasks, respectively and precisely adding a proper amount of baicalin reference substance, respectively, preparing a test sample solution according to the preparation method of the test sample, and respectively calculating the sample adding recovery rate of the baicalin reference substance according to the method for measuring.
Percent recovery is measured-measured component content in sample/reference substance content × 100%
The results are shown in table 6, and the recovery rate of the baicalin loading RSD is 1.1%.
TABLE 6 sample recovery test
Application example 1
Sample content determination experiment:
the ten batches of the antiviral cold traditional Chinese medicine preparation are determined according to a content determination method established by standard research, and the results are shown in table 7.
TABLE 7 determination results of baicalin content in ten batches of the above antiviral cold Chinese medicinal preparation
Example 3
The embodiment provides a method for measuring the content of main effective components in an antiviral cold traditional Chinese medicine preparation, wherein the main effective component of the antiviral cold traditional Chinese medicine preparation is chlorogenic acid, and the method for measuring the content of baicalin comprises the following steps:
s1, preparing a reference solution: precisely weighing chlorogenic acid reference substance, adding 50% methanol, and shaking to obtain reference substance solution with concentration of 52 μ g/mL;
s2, preparing a test solution: precisely weighing the antiviral Chinese medicinal preparation for treating common cold, adding 50% methanol, ultrasonic extracting for 30min, cooling, adding 50% methanol, shaking, filtering, and collecting filtrate to obtain sample solution with concentration of 4 mg/mL;
s3, content determination: precisely sucking 10 μ L of each of the reference solution and the sample solution, and injecting into an ultra high performance liquid chromatograph for measurement under the following chromatographic measurement conditions: adopting an Eilide C18 chromatographic column with the size of 4.6mm multiplied by 25cm and the size of 5 mu m, wherein the number of theoretical plates is 1000 according to the peak of chlorogenic acid; adopting acetonitrile-0.4% phosphoric acid solution as mobile phase; the flow rate is 1.0 mL/min; the detection wavelength was 327 nm.
Preferably, the volume of the mobile phase is 10% of the acetonitrile and 90% of the 0.4% phosphoric acid.
Preferably, the concentration of chlorogenic acid is linearly related to its peak area, the peak area of chlorogenic acid is abscissa, the concentration of chlorogenic acid is ordinate, and the regression equation of the standard curve of the concentration of chlorogenic acid is Y-3.2605 × 10-7X-0.02946。
Detection example 2
(1) Determination of extraction time:
the extraction rates of the antiviral cold traditional Chinese medicine preparation with 50% methanol for ultrasonic extraction for 15 minutes, 30 minutes and 45 minutes are compared. The results are shown in table 8, the extraction rate of 15 minutes of ultrasonic extraction is slightly lower; the extraction rates of the ultrasonic extraction for 30 minutes and 45 minutes were substantially the same. Therefore, it was determined that the sample solution was prepared by ultrasonic extraction with 50% methanol for 30 minutes.
TABLE 8 measurement results of different ultrasonic extraction times of the test samples
(2) And (3) precision test:
according to the method, 0.1980g (lot number is 20021221) of the antiviral cold traditional Chinese medicine preparation is precisely weighed, a test solution is prepared according to the method, sample introduction is repeated for 6 times on an instrument, the peak area is measured, and the content result of chlorogenic acid is calculated. The results are shown in table 9, the peak area average is 1772831.5, the chlorogenic acid content average is 13.5047mg/g, and RSD% is 0.31.
TABLE 9 precision test
(3) And (3) stability test:
according to the method, 0.1960g (lot number is 20021221) of the antiviral cold traditional Chinese medicine preparation is precisely weighed, a test solution is prepared according to the method, the sample injection is carried out every 2-3 hours for measuring for 1 time, the measurement is repeated for 6 times, the measurement lasts for 12 hours, the peak area of chlorogenic acid is recorded, and the content result of chlorogenic acid is calculated. The results are shown in table 10, the peak area average is 1736766, the chlorogenic acid content average is 13.5291mg/g, and RSD% is 1.10. The result shows that the sample solution is basically stable when the measurement is carried out for 12 hours.
TABLE 10 stability test
(4) And (3) repeatability test:
6 parts of the antiviral cold traditional Chinese medicine preparation (lot number 20021221) are precisely weighed according to the method, test solution is respectively prepared according to the method, and the sample injection is respectively carried out on the instruments for measurement. The results of the content measurement of 6 samples are shown in table 11, with RSD% of 1.05 and the average content of 13.3994 mg/g.
TABLE 11 reproducibility test
| |
1 | 2 | 3 | 4 | 5 | 6 |
| Results of content measurement (mg/g) | 13.3462 | 13.5546 | 13.2286 | 13.2852 | 13.3610 | 13.6211 |
(5) Linear relation examination and determination of measurement calculation method:
precisely weighing 10.4mg of chlorogenic acid reference substance, placing into a 100mL brown volumetric flask, adding 50% methanol for dissolving, and diluting to scale to obtain a reference substance solution with a concentration of 104 μ g/mL. The control solutions were injected at 2.5. mu.L, 5.0. mu.L, 10.0. mu.L, 15.0. mu.L and 17.5. mu.L, respectively, corresponding to injection amounts of 0.26. mu.g, 0.52. mu.g, 1.04. mu.g, 1.56. mu.g and 1.82. mu.g, respectively, and peak areas were recorded. The results are shown in Table 12, the chlorogenic acid sample amount is between 0.13 μ g and 1.82 μ g, and the peak area (X) and the chlorogenic acid sample amount (Y) form a good linear relationship.
The regression equation is that Y is 3.2605 × 10-7X-0.02946，r＝0.9993。
And the standard curve is a straight line which basically passes through the origin, so the content of the chlorogenic acid can be measured and calculated by an external standard one-point method.
TABLE 12 Linear relationship between chlorogenic acid peak area and chlorogenic acid sample amount
| Sample injection volume (mu L) of chlorogenic acid reference substance | 2.5 | 5 | 10 | 15 | 17.5 |
| Chlorogenic acid reference sample amount C (mug) | 0.26 | 0.52 | 1.04 | 1.56 | 1.82 |
| Peak area (A) | 845670 | 1708473 | 3302715 | 4970809 | 5572681 |
(6) Recovery rate test:
precisely weighing 5 parts of the antiviral cold traditional Chinese medicine preparation with the content of 13.3994mg/g in the same batch (20021221), respectively placing the 5 parts in 5 25ml volumetric flasks, respectively and precisely adding 2.0ml of a chlorogenic acid reference substance 50% methanol solution with the concentration of 1.4mg/ml, equivalently adding 2.8mg of the chlorogenic acid reference substance, then adding 50% methanol to about 20ml, ultrasonically extracting for 30 minutes, cooling, diluting to scale with 50% methanol, shaking up, filtering, measuring by the method, and respectively calculating the sample addition recovery rate of the chlorogenic acid reference substance. The results are shown in table 13, and the mean recovery rate of chlorogenic acid sample is 99.80%, and RSD%.
TABLE 13 recovery test
Application example 2
Sample content determination experiment:
the above antiviral cold Chinese medicinal preparations are measured according to the above method, 2 parts of each batch are measured, and the results are shown in Table 14 by taking the average value.
TABLE 14 determination of chlorogenic acid content in the above antiviral cold Chinese medicinal preparation
In conclusion, the method for determining the content of the baicalin and the chlorogenic acid has the advantages of simple pretreatment, simplicity, sensitivity, stability, reliability and the like, and the obtained ultra-high performance liquid chromatogram calculates the concentration of the baicalin and the chlorogenic acid through a regression equation, so that the quality information of the product is reflected, and the method is favorable for monitoring the quality of the product and identifying the authenticity.
While the invention has been described with reference to a preferred embodiment, it will be understood by those skilled in the art that various changes in form and detail may be made therein without departing from the spirit and scope of the invention.
Claims (9)
1. A method for measuring the content of main effective components in an antiviral cold traditional Chinese medicine preparation, wherein the antiviral cold traditional Chinese medicine preparation comprises scutellaria baicalensis, honeysuckle, fructus forsythiae, folium isatidis, lophatherum gracile, liquorice extract, dextrin, fructus arctii, peppermint oil, calculus bovis factitius and auxiliary materials, and is characterized in that the content measurement method comprises the following steps:
s1, preparing a reference solution: precisely weighing a reference substance, adding 50-100% methanol, and shaking up to obtain a reference substance solution with the concentration of 45-70 μ g/mL;
s2, preparing a test solution: precisely weighing the antiviral cold traditional Chinese medicine preparation, adding 50-70% methanol, performing ultrasonic extraction for 15-60min, cooling, adding 50-70% methanol, shaking, filtering, and collecting the filtrate to obtain a sample solution with concentration of 2-5 mg/mL;
s3, content determination: respectively and precisely sucking 10 mu L of the reference solution and the test solution respectively, and injecting the reference solution and the test solution into an ultra-high performance liquid chromatograph for measurement.
2. The content measuring method according to claim 1, wherein when the main active ingredient is baicalin, step S3 of the baicalin content measuring method comprises:
respectively and precisely sucking 10 mu L of each of the reference solution and the test solution, and injecting the reference solution and the test solution into an ultra-high performance liquid chromatograph for measurement, wherein the chromatographic measurement conditions are as follows: adopting welchrom-C18 chromatographic column, 4.6mm × 250mm, 5 μm, and the number of theoretical plates is 1000 according to baicalin peak; methanol-0.4% phosphoric acid solution is used as a mobile phase; the flow rate is 1.0 mL/min; the detection wavelength was 280 nm.
3. The method according to claim 2, wherein the volume of the mobile phase is 48% of the methanol and 52% of the 0.4% of the phosphoric acid.
4. The method according to claim 2, wherein the ultrasonic extraction time is 30 min.
5. The method according to claim 2, wherein the concentration of baicalin is linearly related to the peak area thereof; and taking the concentration of the baicalin as an abscissa, the area of the baicalin peak as an ordinate, and the regression equation of the baicalin concentration standard curve is that Y is 40787X-60834.
6. The content measuring method according to claim 1, wherein when the main effective ingredient is chlorogenic acid, step S3 of the chlorogenic acid content measuring method comprises:
respectively and precisely sucking 10 mu L of each of the reference solution and the test solution, and injecting the reference solution and the test solution into an ultra-high performance liquid chromatograph for measurement, wherein the chromatographic measurement conditions are as follows: adopting an Eilide C18 chromatographic column with the size of 4.6mm multiplied by 25cm and the size of 5 mu m, wherein the number of theoretical plates is 1000 according to the peak of chlorogenic acid; adopting acetonitrile-0.4% phosphoric acid solution as mobile phase; the flow rate is 1.0 mL/min; the detection wavelength was 327 nm.
7. The method according to claim 6, wherein the volume of the mobile phase is 10% of the acetonitrile and 90% of the 0.4% phosphoric acid.
8. The method according to claim 6, wherein the ultrasonic extraction time is 30 min.
9. The content determination method according to claim 6, wherein the concentration of chlorogenic acid is in a linear relationship with the peak area thereof, the peak area of chlorogenic acid is taken as an abscissa, the concentration of chlorogenic acid is taken as an ordinate, and the regression equation of the standard curve of the concentration of chlorogenic acid is that Y is 3.2605 × 10-7X-0.02946。
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