CN113391003B - Method for simultaneously detecting content of active ingredients in pulse-activating decoction - Google Patents
Method for simultaneously detecting content of active ingredients in pulse-activating decoction Download PDFInfo
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- 239000004480 active ingredient Substances 0.000 title claims abstract description 13
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- G—PHYSICS
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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
- G01N30/86—Signal analysis
- G01N30/8675—Evaluation, i.e. decoding of the signal into analytical information
- G01N30/8679—Target compound analysis, i.e. whereby a limited number of peaks is analysed
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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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Abstract
The invention relates to a method for simultaneously detecting the content of active ingredients in Shengmai decoction, which comprises the steps of preparing a sample solution, preparing a reference substance solution and detecting a sample to obtain the active ingredients of 5-hydroxymethylfurfural, protocatechuic acid, syringin, geniposide, codonopsis pilosula acetylenic glycoside, schisandrin A and schisandrin B in Shengmai decoction. The invention detects index components in the Shengmai drink for the first time and quantitatively analyzes the content of 5-hydroxymethylfurfural components so as to ensure the use safety of medicines and realize more comprehensive evaluation and control of the quality of the Shengmai drink. The detection indexes selected by the invention are all components with higher content in the pulse-activating drink and pharmacological activity. Can provide basis for the safety, effectiveness and accuracy of the clinical application of the pulse generating decoction. The detection time and the cost are saved, and the method is accurate, simple and easy to implement. The invention has good stability, good repeatability, high recovery rate and stronger specificity.
Description
Technical Field
The invention relates to a method for simultaneously detecting the content of active ingredients, in particular to a method for simultaneously detecting the content of active ingredients in Shengmai decoction, belonging to the field of quality detection of traditional Chinese medicine preparations.
Background
Shengmai decoction (Codonopsis pilosula prescription) has the effects of strengthening spleen, tonifying lung, nourishing blood and promoting fluid production, and can be clinically used for deficiency of both qi and yin, palpitation, shortness of breath and slight spontaneous perspiration. The radix codonopsis is sweet in taste and flat in nature, enters spleen and lung channels, and modern pharmacological researches show that the radix codonopsis has the functions of strengthening physique, improving human immunity, resisting aging, oxidization, fatigue, inflammation, tumor, memory and cognition and the like, so that the radix codonopsis is widely used as a substitute of ginseng in clinic and widely used in a prescription preparation of ginseng originally used. The pulse-activating decoction (dangshen prescription) has mild medicine property, is not dry and greasy, has the effects of restoring pulse and relieving depletion, does not help fire to block qi after long-term administration, can be widely applied to chronic cardiovascular disease patients with sub-health and lighter illness, is collected in a tenth book of Chinese medicinal prescription preparations in medicine Standard of Ministry of health, and has only one relative density test item except for conventional test of mixture.
The recipe of Shengmai decoction consists of three kinds of Chinese medicinal materials including pilose asiabell root, schisandra fruit, ophiopogon root, etc. and the chemical components of pilose asiabell root include phenylpropanoids, sesquiterpene lactones, nucleosides, amino acids and polyacetylene. The phenylpropanoid compound comprises syringin, codonopsis pilosula glycoside I, codonopsis pilosula acetylenic glycoside and the like, is the main component in codonopsis pilosula, has the highest content of the codonopsis pilosula acetylenic glycoside and the most representative, has pharmacological activities of resisting cancer, resisting bacteria, resisting inflammation, calming, reducing blood pressure, regulating prostaglandin metabolism and the like, has better protection effect on gastric mucosal injury and various experimental gastric ulcers, and has obvious antiulcer effect. Geniposide belongs to iridoid glycoside compounds, has quite wide pharmacological actions, and has various effects of anti-inflammatory, antioxidant stress, blood sugar regulation, anti-tumor and the like; protocatechuic acid is common organic acid compound in fructus Schisandrae, and has antibacterial, phlegm eliminating and asthma relieving effects. Is clinically used for treating chronic tracheitis. The schisandrin A and the schisandrin B belong to lignans, are effective components for playing various effects of schisandra, can improve the space exploration memory capacity of rats and have obvious central inhibition effect, and also have obvious nervous system effect.
The pulse-activating decoction (dangshen prescription) on the market has wide application and obvious curative effect, but has complex chemical components, numerous potential effective targets, various functional indications, numerous manufacturers and uneven quality, does not have relevant quality control standards, and cannot comprehensively analyze, evaluate and control the pulse-activating decoction (dangshen prescription), so that the pulse-activating decoction (dangshen prescription) lacks safety and effectiveness in the use process. The research on HPLC content detection of Shengmai decoction (dangshen prescription) is mainly focused on quantitative determination of schisandrin A in pharmacopoeia records, and also has the advantages of separately detecting the content of dangshen acetylenic glycoside in dangshen, establishing an HPLC multicomponent detection method, and simultaneously detecting the content of 5-hydroxymethyl furfural, protocatechuic acid, dangshen acetylenic glycoside and schisandrin A in Shengmai decoction, thereby providing a certain basis for quality control of Shengmai decoction (dangshen prescription). However, the active ingredients of Shengmai decoction (Codonopsis pilosula) are not only aldehydes, organic acids, polyacetylenes and lignans.
Therefore, on the basis of the existing research, the establishment of a rapid, comprehensive and highly-targeted quality detection method for Shengmai decoction (dangshen prescription) has important significance.
Disclosure of Invention
In order to comprehensively control the quality of the Shengmai decoction (dangshen prescription), the technical problem to be solved by the invention is that the detection index of the Shengmai decoction (dangshen prescription) in the prior art is single, which is not beneficial to the quality control of the Shengmai decoction (dangshen prescription), and further provides a rapid, comprehensive and highly-targeted detection method of the Shengmai decoction (dang prescription) preparation.
The technical scheme of the invention is as follows:
a method for simultaneously detecting the content of active ingredients in Shengmai decoction is carried out according to the following steps:
the effective components of the composition are 5-hydroxymethylfurfural, protocatechuic acid, syringin, geniposide, dangshen acetylenic glycoside, schizandrin A and schizandrin B in Shengmai drink through the preparation of a test solution, the preparation of a reference solution and the detection of a sample.
Further, the method comprises the steps of:
step (1), preparation of a sample solution:
taking the solution of the product, precisely measuring, spin-drying in a spin bottle, adding a proper amount of methanol, transferring to a volumetric flask, fixing the volume to a scale, performing ultrasonic treatment, cooling, shaking uniformly, standing, taking supernatant, filtering, and taking subsequent filtrate.
Step (2), preparation of a reference substance solution:
precisely weighing a proper amount of reference substance of the component to be measured, and adding 50% -100% methanol to prepare a reference substance solution;
step (3), sample detection:
the chromatographic conditions were as follows:
the chromatographic column takes octadecylsilane chemically bonded silica gel as a filler, the flow rate is 0.5-2 mL/min, and the column temperature is 20-35 ℃; the detection wavelength is one or two wavelengths from 220nm to 290 nm; the sample injection amount is 5-20 mu L; the mobile phase is a mixed solvent composed of methanol or acetonitrile and formic acid or phosphoric acid; the concentration of the formic acid or phosphoric acid contained in the formic acid or phosphoric acid aqueous solution is 0.01-0.5%; respectively sucking 5-20 μl of the mixed reference solution and the sample solution, and injecting into a liquid chromatograph for measurement.
Further, in the step (1), 0.2-5.0 mL of the product solution is taken, precisely weighed, placed in a spin bottle for spin drying, added with a proper amount of 50-100% methanol, transferred into a volumetric flask, fixed to a scale, ultrasonically extracted for 15-30 minutes, cooled, shaken uniformly, stood, filtered by a microporous filter membrane with the thickness of 0.45 mu m, and obtained as a subsequent filtrate.
Further, in the step (2), each 1mL of the reference solution contains 16.00-160.00 mug of 5-hydroxymethyl furfural, 2.52-25.20 mug of protocatechuic acid, 1.68-16.80 mug of syringin, 3.44-34.40 mug of geniposide, 16.12-161.20 mug of codonopsis pilosula acetylide, 51.96-519.60 mug of schisandrin and 5.80-58.00 mug of schisandrin.
Further, in the step (3), gradient elution is performed according to the following table;
| time min | Methanol or acetonitrile (A)% | Formic acid or phosphoric acid aqueous solution (B)% | Totals to |
| 0～78 | Any one of the |
Allowance of | 100％ |
| 79～93 | Any one of the values 20 to 60 | Allowance of | 100％ |
| 94～110 | Any one of the |
Allowance of | 100％ |
The invention is further illustrated by the following experimental study.
(1) Selection of chromatographic columns: the detection index selected for the HPLC detection method established according to the present invention includes components of large polarity, medium polarity and small polarity, and contains water-soluble and fat-soluble compounds, so a reversed phase C18 chromatographic column is selected.
(2) Selection of detection wavelength: and (3) carrying out full-wavelength scanning on 7 components such as 5-hydroxymethylfurfural and the like, and finally determining to select one or two wavelengths from 220-290 nm as detection wavelengths.
(3) Selection of mobile phase system: taking the mobile phase systems of acetonitrile (A) -phosphoric acid (B) solution, acetonitrile (A) -formic acid (B), methanol (A) -phosphoric acid (B) solution and methanol (A) -formic acid (B) solution as factors for examination, the results show that the use of different mobile phase systems has different effects on the peak shape and the separation degree of each active ingredient, and can be used for the detection of the mobile phase system of the solution.
(4) The treatment mode of the test sample is selected: as the selected detection indexes comprise components with large polarity, medium polarity and small polarity, and also comprise water-soluble components, the chemical properties of the components are comprehensively considered, and three solvents of 50% methanol, 70% methanol and 100% methanol are initially selected for investigation. As a result, it was found that 7 components of 50% -100% methanol were extracted in the solvent, and 50% -100% methanol was used as the extraction solvent.
(5) Chromatographic conditions and system suitability test: octadecylsilane chemically bonded silica is used as a filler; acetonitrile is taken as a mobile phase A, 0.15% formic acid water solution is taken as a mobile phase B, and gradient elution is carried out according to the specification in the following table; the detection wavelength is 260nm; column temperature 20 ℃.
The theoretical plate number is not lower than 6000 calculated according to the Codonopsis pilosula alkyne glycoside peak.
| Time min | Methanol or acetonitrile (A)% | Formic acid or phosphoric acid aqueous solution (B)% | Totals to |
| 0～78 | Any one of the |
Allowance of | 100％ |
| 79～93 | Any one of the values 20 to 60 | Allowance of | 100％ |
| 94～110 | Any one of the |
Allowance of | 100％ |
(6) Specificity experiment: under the same test conditions, the mixed reference solution and the Shengmai drink test sample solution are used as a reference, and 100% methanol solution is used as a negative reference. The measurement was performed as described in step (5). As a result, peaks of each component of the mixed reference solution appear in the sample solution containing the Shengmai drink, but do not appear in the negative control solution, which indicates that the experimental method has specificity, the mixed reference solution results are shown in FIG. 1, the Shengmai drink sample solution results are shown in FIG. 2, and the negative control solution results are shown in FIG. 3.
(7) Linear relationship: taking a proper amount of each reference substance, precisely weighing, placing the reference substances into a brown measuring flask, adding methanol for dissolving, and preparing a solution containing 160.00 mug of 5-hydroxymethylfurfural, 25.20 mug of protocatechuic acid, 16.80 mug of syringin, 34.40 mug of geniposide, 161.20 mug of codonopsis pilosula acetylide, 519.60 mug of schisandrin and 58.00 mug of schisandrin per 1mL of the reference substance stock solution. Precisely sucking 1.0mL, 2.0mL, 4.0mL, 6.0mL, 8.0mL and 10mL of mixed reference substance stock solution respectively, placing into a 10mL volumetric flask, adding methanol to fix volume to scale, and shaking uniformly to obtain the final product. Precisely sucking 10 mu L of each mixed reference substance solution, injecting into a liquid chromatograph, and measuring by the method described in the reference (5), wherein the results of the measurement of 5-hydroxymethylfurfural, protocatechuic acid, syringin, geniposide, codonopsis pilosula acetylenic glycoside, schisandrin A and schisandrin B have good linear relations within the ranges of 16.00-160.00 mu g/mL, 2.52-25.20 mu g/mL, 1.68-16.80 mu g/mL, 3.44-34.40 mu g/mL, 16.12-161.20 mu g/mL, 51.96-519.60 mu g/mL and 5.80-58.00 mu g/mL; the results are shown in Table 1.
Table 1 results of linear relationship investigation
(8) Precision investigation: and (3) precisely measuring 10 mu L of the mixed reference substance solution under the specificity investigation item, injecting the mixed reference substance solution into a liquid chromatograph according to the method (5), and continuously injecting samples for 6 times for measurement. The results showed that the RSD% of each component was between 0.59 and 0.93. The results are shown in Table 2.
(9) Repeatability investigation: 6 parallel test solutions were prepared, 10. Mu.L of the test solution was precisely aspirated, and injected into a liquid chromatograph for measurement according to the method described in (5). The results show that: the RSD% of each component is between 0.59 and 2.63, and the repeatability is good. The results are shown in Table 2.
(10) Stability investigation: preparing a sample solution, precisely sucking 10 mu L of the solution at 0h,2h,4h,6h,8h,10h,12h and 24h respectively, and injecting into a liquid chromatograph. The test result shows that the test sample solution is stable in 24 hours at room temperature, and the RSD% is between 1.44 and 2.97. The results are shown in Table 2.
Table 2 table of experimental results
(11) Sample recovery rate test: 6 parts of pulse-activating drink (5-hydroxymethylfurfural 41.4634 mu g/mL, protocatechuic acid 3.9901 mu g/mL, syringin 19.5559 mu g/mL, geniposide 10.6206 mu g/mL, codonopsis pilosula acetylenic glycoside 64.7735 mu g/mL, schisandrin A129.5651 mu g/mL, schisandrin B17.6383 mu g/mL) are precisely measured, about 2.0mL of mixed reference substance stock solution is added in a ratio of 0.5:1, 1:1 and 1:1.5, the mixture is placed in a 10mL volumetric flask with a plug, 100% methanol is added for constant volume, a sealing plug is adopted, ultrasound is carried out for 15min, cooling is carried out, shaking is carried out, standing is carried out, supernatant fluid is taken and filtration is carried out, and subsequent filtrate is taken and filtered by a microporous filter membrane of 0.45 mu m, thus obtaining the pulse-activating drink. 6 parts of sample solution was taken, the peak areas of 7 components such as 5-hydroxymethylfurfural were measured under the conditions described in (5), and the content and recovery rate of each component were calculated.
As a result, the average recovery rate of each component is 97.32% -101.27%, and the RSD value is 1.90% -3.56%. The method shows that the added reference substance can be accurately recovered, and the determination method is accurate and reliable. The test results are shown in Table 3.
TABLE 3 sample recovery results Table
(12) Durability experiment: 3 parts of test solution is prepared, 10 mu L of the test solution is precisely sucked, and the test solution is respectively subjected to different fluctuation factors: and (3) respectively injecting samples at equipment, a chromatographic column and column temperature, recording peak areas of 7 components such as 5-hydroxymethylfurfural, calculating the content, and inspecting the durability of chromatographic conditions. As a result, the RSD% value of each component content was less than 3% under each condition, indicating that the durability of the chromatographic condition was good. The results are shown in Table 4.
Table 4 durability test results table
Compared with the prior art, the invention has the following beneficial effects:
(1) According to the HPLC content determination method for Shengmai decoction, index components of furans, organic acids, phenylpropanoids, iridoids, lignans and polyacetylenes in Shengmai decoction (dangshen prescription) are detected simultaneously for the first time, so that the quality of Shengmai decoction (dangshen prescription) preparation is evaluated and controlled more comprehensively. The invention has simple operation and good applicability, and can be stably used for measuring the content of pulse-activating decoction (dangshen prescription). The detection indexes selected by the invention are all components with higher content and pharmacological activity in the Shengmai decoction (dangshen prescription). Can provide the basis for the safety and effectiveness of the clinical application of the pulse generating decoction (dangshen prescription).
(2) The detection indexes selected by the invention are 5-hydroxymethylfurfural, protocatechuic acid, syringin, geniposide, dangshen acetylenic glycoside, schizandrin A and schizandrin B, which are representative chemical components of furans, organic acids, phenylpropanoids, iridoids, lignans and polyacetylenes in Shengmai decoction (dangshen prescription), and are also main pharmacological active components. According to the invention, the content of 7 components such as 5-hydroxymethylfurfural and the like is detected simultaneously by high performance liquid chromatography for the first time, so that the detection time and cost are saved, and the method is accurate, simple and easy to implement. The comprehensive evaluation and control of the quality of the Shengmai decoction (dangshen prescription) are realized, thereby providing guarantee for the effectiveness and the safety of clinical medication of the Shengmai decoction (dangshen prescription). The invention has good stability, good repeatability, high recovery rate and stronger specificity.
Drawings
FIG. 1 is a liquid chromatogram of a mixed control solution in a specificity experiment;
FIG. 2 is a liquid chromatogram of a Shengmai decoction (Codonopsis pilosula) sample solution in a specific experiment;
fig. 3 is a liquid chromatogram of a negative control solution in a specificity experiment.
Detailed Description
The present invention will be described in further detail with reference to the drawings and examples, in order to make the objects, technical solutions and advantages of the present invention more apparent. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention. The specific techniques or conditions are not identified in the examples and are performed according to techniques or conditions described in the literature in this field or according to the product specifications. The reagents or apparatus used were conventional products available commercially without the manufacturer's attention.
Example 1
In the method for simultaneously detecting the content of the active ingredients in the Shengmai decoction (dangshen prescription), the content of 5-hydroxymethylfurfural, protocatechuic acid, syringin, geniposide, dangshen acetylenic glycoside, schizandrin A and schizandrin B in the self-made Shengmai decoction (dangshen prescription) in a laboratory is detected by HPLC. The method specifically comprises the following steps:
preparation of a reference substance solution in the step (1):
precisely weighing proper amounts of 5-hydroxymethylfurfural, protocatechuic acid, syringin, geniposide, codonopsis pilosula acetylenic glycoside, schizandrin A and schizandrin B, adding methanol to prepare a solution containing 16.00 mug of 5-hydroxymethylfurfural, 2.52 mug of protocatechuic acid, 1.68 mug of syringin, 3.44 mug of geniposide, 16.12 mug of codonopsis pilosula acetylenic glycoside, 51.96 mug of schizandrin A and 5.80 mug of schizandrin B per 1 mL.
Preparing a sample solution in the step (2):
taking a pulse-activating drink (codonopsis pilosula prescription) test sample, taking about 0.2mL of the sample, placing the sample into a rotary bottle for spin drying, precisely adding a proper amount of 50% methanol, transferring the sample into a 10mL volumetric flask, fixing the volume, sealing, performing ultrasonic treatment for 15 minutes, cooling, shaking uniformly, standing, taking supernatant, filtering the supernatant by using a microporous filter membrane with the thickness of 0.45 mu m, and taking a subsequent filtrate.
And (3) detecting a sample:
octadecylsilane chemically bonded silica is used as a filler; the flow rate is 0.5mL/min, acetonitrile is taken as a mobile phase A, 0.15% formic acid water solution is taken as a mobile phase B, and gradient elution is carried out according to the specification in the following table; the detection wavelength is 260nm; column temperature was 35 ℃. The theoretical plate number is not lower than 6000 calculated according to the Codonopsis pilosula alkyne glycoside peak.
| Time | Acetonitrile (A)% | 0.15% formic acid water (B)% | Totals to |
| 0 | 6 | 94 | 100％ |
| 11 | 6 | 94 | 100％ |
| 25 | 8 | 92 | 100％ |
| 26 | 12 | 88 | 100％ |
| 49 | 12 | 88 | 100％ |
| 51 | 19 | 81 | 100％ |
| 68 | 20 | 80 | 100％ |
| 78 | 28 | 72 | 100％ |
| 83 | 52 | 48 | 100％ |
| 93 | 52 | 48 | 100％ |
| 100 | 44 | 56 | 100％ |
| 105 | 6 | 94 | 100％ |
| 110 | 6 | 94 | 100％ |
Respectively sucking 10 μl of the mixed reference solution and the sample solution, and injecting into a liquid chromatograph for measurement.
The sample varieties and content measurement results of Shengmai decoction (Codonopsis pilosula) of this example are shown in Table 7.
TABLE 7 determination of sample content of Shengmai decoction (Codonopsis pilosula formula)
According to the content detection result, the method can be stably used for detecting the content of the pulse-activating decoction (dangshen prescription).
Example 2
In the method for simultaneously detecting the content of the active ingredients in the Shengmai decoction (dangshen prescription), the content of 5-hydroxymethylfurfural, protocatechuic acid, syringin, geniposide, dangshen acetylenic glycoside, schizandrin A and schizandrin B in the self-made Shengmai decoction (dangshen prescription) in a laboratory is detected by HPLC. The method specifically comprises the following steps:
preparation of a reference substance solution in the step (1):
precisely weighing appropriate amount of 5-hydroxymethylfurfural, protocatechuic acid, syringin, geniposide, radix Codonopsis alkynoside, schizandrin A and schizandrin B, adding methanol to prepare solution containing 64.00 μg of 5-hydroxymethylfurfural, 10.08 μg of protocatechuic acid, 6.72 μg of syringin, 13.76 μg of geniposide, 64.48 μg of radix Codonopsis alkynoside, 207.84 μg of schizandrin A and 58.00 μg of schizandrin B per 1 mL.
Preparing a sample solution in the step (2):
taking a pulse-activating drink (codonopsis pilosula prescription) test sample, taking about 2.0mL of the pulse-activating drink, placing the sample into a rotary bottle for spin drying, precisely adding a proper amount of 70% methanol, transferring the mixture into a 10mL volumetric flask, fixing the volume, sealing, performing ultrasonic treatment for 30 minutes, cooling, shaking uniformly, standing, taking supernatant, filtering the supernatant by using a microporous filter membrane with the thickness of 0.45 mu m, and taking a subsequent filtrate to obtain the pulse-activating drink.
And (3) detecting a sample:
octadecylsilane chemically bonded silica is used as a filler; the flow rate is 1.0mL/min, acetonitrile is taken as a mobile phase A, 0.01% formic acid water solution is taken as a mobile phase B, and gradient elution is carried out according to the specification in the following table; the detection wavelength is 250nm; column temperature was 30 ℃. The theoretical plate number is not lower than 6000 calculated according to the Codonopsis pilosula alkyne glycoside peak.
| Time | Acetonitrile (A)% | 0.01% formic acid water (B)% | Totals to |
| 0 | 2 | 98 | 100％ |
| 15 | 2 | 98 | 100％ |
| 25 | 10 | 90 | 100％ |
| 26 | 20 | 80 | 100％ |
| 49 | 20 | 80 | 100％ |
| 51 | 36 | 64 | 100％ |
| 68 | 36 | 64 | 100％ |
| 78 | 28 | 72 | 100％ |
| 83 | 42 | 58 | 100％ |
| 93 | 52 | 48 | 100％ |
| 100 | 20 | 80 | 100％ |
| 110 | 2 | 98 | 100％ |
Respectively sucking 5 μl of the mixed reference solution and the sample solution, and injecting into a liquid chromatograph for measurement.
The sample varieties and content measurement results of Shengmai decoction (Codonopsis pilosula) of this example are shown in Table 8.
Table 8 results of measuring the content of Shengmai decoction (Codonopsis pilosula)
According to the content detection result, the method can be stably used for detecting the content of the pulse-activating decoction (dangshen prescription).
Example 3
In the method for simultaneously detecting the content of the active ingredients in the Shengmai decoction (dangshen prescription), the content of 5-hydroxymethylfurfural, protocatechuic acid, syringin, geniposide, dangshen acetylenic glycoside, schizandrin A and schizandrin B in the self-made Shengmai decoction (dangshen prescription) in a laboratory is detected by HPLC. The method specifically comprises the following steps:
preparation of a reference substance solution in the step (1):
precisely weighing 5-hydroxymethylfurfural, protocatechuic acid, syringin, geniposide, codonopsis pilosula acetylenic glycoside, schizandrin A and schizandrin B, and adding methanol to prepare a solution containing 160.00 mug of 5-hydroxymethylfurfural, 25.20 mug of protocatechuic acid, 16.80 mug of syringin, 34.40 mug of geniposide, 161.20 mug of codonopsis pilosula acetylenic glycoside, 519.60 mug of schizandrin A and 58.00 mug of schizandrin B per 1 mL.
Preparing a sample solution in the step (2):
taking a pulse-activating drink (codonopsis pilosula prescription) test sample, taking about 5.0mL of the pulse-activating drink, placing the sample into a rotary bottle for spin drying, precisely adding a proper amount of 100% methanol, transferring the sample into a 10mL volumetric flask, fixing the volume, sealing, performing ultrasonic treatment for 30 minutes, cooling, shaking uniformly, standing, taking supernatant, filtering the supernatant by using a microporous filter membrane with the thickness of 0.45 mu m, and taking a subsequent filtrate.
And (3) detecting a sample:
octadecylsilane chemically bonded silica is used as a filler; the flow rate is 2.0mL/min, methanol is taken as a mobile phase A, 0.50% phosphoric acid aqueous solution is taken as a mobile phase B, and gradient elution is carried out according to the specification in the following table; the detection wavelength is 260nm; column temperature was 35 ℃. The theoretical plate number is not lower than 6000 calculated according to the Codonopsis pilosula alkyne glycoside peak.
| Time | Methanol (A)% | 0.15% formic acid water (B)% | Totals to |
| 0 | 36 | 64 | 100％ |
| 11 | 36 | 64 | 100％ |
| 49 | 12 | 88 | 100％ |
| 50 | 20 | 80 | 100％ |
| 68 | 20 | 80 | 100％ |
| 78 | 46 | 54 | 100％ |
| 83 | 58 | 42 | 100％ |
| 93 | 60 | 40 | 100％ |
| 105 | 36 | 64 | 100％ |
| 110 | 36 | 64 | 100％ |
Respectively sucking 20 μl of the mixed reference solution and the sample solution, and injecting into a liquid chromatograph for measurement.
The sample varieties and content measurement results of Shengmai decoction (Codonopsis pilosula) of this example are shown in Table 9.
Table 9 determination of the content of Shengmai decoction (Codonopsis pilosula)
According to the content detection result, the method can be stably used for detecting the content of the pulse-activating decoction (dangshen prescription).
The foregoing description of the preferred embodiments of the invention is not intended to be limiting, but rather is intended to cover all modifications, equivalents, alternatives, and improvements that fall within the spirit and scope of the invention.
Claims (3)
1. A method for simultaneously detecting the content of active ingredients in Shengmai decoction is characterized in that: the effective components detected by the preparation of the sample solution, the preparation of the reference substance solution and the sample detection are 5-hydroxymethylfurfural, protocatechuic acid, syringin, geniposide, dangshen acetylenic glycoside, schizandrin A and schizandrin B; the method comprises the following steps:
step (1), preparation of a sample solution:
taking the solution, precisely measuring, spin-drying in a spin bottle, adding a proper amount of methanol, transferring to a volumetric flask, fixing the volume to a scale, performing ultrasonic treatment, cooling, shaking uniformly, standing, filtering the supernatant, and taking the subsequent filtrate to obtain the product;
step (2), preparation of a reference substance solution:
precisely weighing a proper amount of reference substance of the component to be measured, and adding 50% -100% methanol to prepare a reference substance solution;
step (3), sample detection:
the chromatographic conditions were as follows:
the chromatographic column takes octadecylsilane chemically bonded silica gel as a filler, the flow rate is 0.5-2 mL/min, and the column temperature is 20-35 ℃; the detection wavelength is one or two wavelengths from 220nm to 290 nm; the sample injection amount is 5-20 mu L; the mobile phase is a mixed solvent composed of methanol or acetonitrile and formic acid; the concentration of the formic acid contained in the aqueous solution of the formic acid is 0.01 to 0.15 percent; respectively sucking 5-20 μl of the mixed reference solution and the sample solution, and injecting into a liquid chromatograph for measurement;
gradient elution was performed as follows:
Or:
or:
The linear relationship results are shown in the following table:
。
2. The method according to claim 1, characterized in that: in the step (1), 0.2-5.0 mL of the product solution is taken, precisely weighed, placed in a spin bottle for spin drying, added with a proper amount of 50-100% methanol, transferred into a volumetric flask, fixed to a scale, ultrasonically extracted for 15-30 minutes, cooled, shaken uniformly, stood, filtered by a microporous filter membrane with the thickness of 0.45 mu m, and obtained as a subsequent filtrate.
3. The method according to claim 1, characterized in that: in the step (2), each 1mL of reference solution contains 16.00-160.00 mug of 5-hydroxymethyl furfural, 2.52-25.20 mug of protocatechuic acid, 1.68-16.80 mug of syringin, 3.44-34.40 mug of geniposide, 16.12-161.20 mug of codonopsis pilosula acetylide, 51.96-519.60 mug of schizandrin and 5.80-58.00 mug of schizandrin.
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