CN108982727A - A method of using effective component protocatechuic acid in HPLC method detection bastard speedwell extracting solution - Google Patents
A method of using effective component protocatechuic acid in HPLC method detection bastard speedwell extracting solution Download PDFInfo
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- CN108982727A CN108982727A CN201810867160.4A CN201810867160A CN108982727A CN 108982727 A CN108982727 A CN 108982727A CN 201810867160 A CN201810867160 A CN 201810867160A CN 108982727 A CN108982727 A CN 108982727A
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- protocatechuic acid
- effective component
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/26—Conditioning of the fluid carrier; Flow patterns
- G01N30/28—Control of physical parameters of the fluid carrier
- G01N30/34—Control of physical parameters of the fluid carrier of fluid composition, e.g. gradient
Abstract
The invention discloses a kind of methods using effective component protocatechuic acid in HPLC method detection bastard speedwell extracting solution, using octadecylsilane chemically bonded silica as the filler of chromatographic column, using acetonitrile or methanol as mobile phase A, using 0.5 2.0% acetum of mass concentration or 0.1 1.0% phosphoric acid solution of mass concentration as Mobile phase B, gradient elution, Detection wavelength 255-265nm are carried out to chromatographic column, reference substance solution and test solution are drawn respectively, inject liquid chromatograph, measurement to get.The present invention can be very good to determine the amount of effective component in extract, and the effective extraction degree for controlling bastard speedwell controls extraction time and extraction time.Reach cost absorbing and benefit than maximizing, the quality of control " swelling and pain relieving patch " drug is safe and reliable from producing to using to reach drug.
Description
Technical field
The present invention relates to a kind of methods of effective component protocatechuic acid in detection bastard speedwell extracting solution, and in particular to one kind is adopted
With the method for effective component protocatechuic acid in HPLC method detection bastard speedwell extracting solution.
Background technique
Bastard speedwell belongs to Scrophulariaceae Scrophulariaceae Veronica Veronica, is a kind of perennial herb.It is high
50-90 centimetres, complete stool is by white pubescence.Bastard speedwell stem is upright, and slightly branch, leaf almost all drape over one's shoulders life, threadiness sometimes on top
Aciculiform is to ovum shape lanceolar or even oval, and base portion is narrow narrow at handle, and apex point, middle and upper part edge has triangular shape sawtooth, dilute to be
Full edge.Blue or bluish violet are spent, arranges the raceme of growth spike in stem top row.The month at florescence 7-8, the fruiting period 9-10 month.Overground part
Divide all herbal medicine, there is clearing lung-heat, resolving sputum, cough-relieving, the effect of removing toxic substances.Control chronic bronchitis, cough leaf purulence blood；Skin eczema is controlled in external application,
Furuncle ulcerative carbuncle ulcer.
According to research shows that the effective component of bastard speedwell is the compounds such as flavonoids, flavonoid glycoside and protocatechuic acid.Now
The extracting method of bastard speedwell be multiple water mention, alcohol precipitation.
The method that determination of total flavonoids in bastard speedwell active component is established using colorimetric method at present.Method: it is with rutin
Reference substance uses sodium hydroxide, sodium nitrite and aluminum nitrate for color developing agent, using ultraviolet spectrophotometry under 510 nm wavelength
Measure the content of general flavone in bastard speedwell active component.But this method is without preferably controlling extraction degree.
Summary of the invention
In order to solve the above technical problems, the present invention provide it is a kind of using HPLC method detection bastard speedwell extracting solution in effective component
The method of protocatechuic acid.
The technical solution adopted by the present invention:
A kind of method using effective component protocatechuic acid in HPLC method detection bastard speedwell extracting solution of the invention, with octadecyl
Silane group silica gel is the filler of chromatographic column, molten with 0.5 2.0% acetic acid of mass concentration using acetonitrile or methanol as mobile phase A
Liquid or 0.1 1.0% phosphoric acid solution of mass concentration are Mobile phase B, and the regulation according to the form below carries out gradient elution to chromatographic column；Inspection
Survey wavelength is 255-265nm；Column temperature: 30 DEG C.Number of theoretical plate is calculated by protocatechuic acid peak should be not less than 5000.
The preparation of reference substance solution:
Take protocatechuic acid or other flavonoids reference substances appropriate, it is accurately weighed, add 30% 80% ethanol solution system of volumetric concentration
At every 1ml containing 15 μ g solution to get.
The preparation of test solution:
It is appropriate that precision measures Veronica linariifolia extract, adds 30% 80% ethanol solution of volumetric concentration to scale, shake up to get.
Measuring method: accurate absorption reference substance solution and each 20 μ 1 of test solution respectively, injection liquid chromatograph, measurement,
To obtain the final product.
Compared with prior art, beneficial effects of the present invention: this method is using octadecylsilane chemically bonded silica column to not
Effective component in bastard speedwell is separated with reaching with the adsorption capacity difference of compound, so as to measure its it is each it is middle at
Point content control its quality, can be very good to determine the amount of effective component in extract, it is effective to control bastard speedwell
Extraction degree controls extraction time and extraction time.Reach cost absorbing and benefit than maximizing, controls " swelling and pain relieving patch " drug
Quality, it is safe and reliable from producing to using to reach drug.
Detailed description of the invention
Fig. 1 is that effective component is kept completely separate chromatogram in bastard speedwell.
Fig. 2 is the linear relationship chart of protocatechuic acid concentration and peak area.
Specific embodiment
In order to deepen the understanding of the present invention, it is described in detail below with reference to specific drawings and embodiments, this explanation
The examples are only for explaining the invention described in book, is not used to limit the present invention.
Embodiment 1
A kind of method using effective component protocatechuic acid in HPLC method detection bastard speedwell extracting solution of the invention, with octadecyl
Silane group silica gel is filler；Using acetonitrile or methanol as mobile phase A, using 1.0% acetum of mass concentration as Mobile phase B, press
Regulation in following table carries out gradient elution；Detection wavelength is 255nm；Column temperature: 30 DEG C.Number of theoretical plate is answered by the calculating of protocatechuic acid peak
Not less than 5000.
The preparation of reference substance solution: taking protocatechuic acid or other flavonoids reference substances appropriate, accurately weighed, adds volume dense
Spend 40% ethanol solution be made every 1ml containing 15 μ g solution to get.
The preparation of test solution: precision measurement Veronica linariifolia extract is appropriate, adds 40% ethanol solution of volumetric concentration to quarter
Degree, shake up to get.
Measuring method: accurate absorption reference substance solution and each 20 μ 1 of test solution respectively, injection liquid chromatograph, measurement,
To obtain the final product.
Embodiment 2
A kind of method using effective component protocatechuic acid in HPLC method detection bastard speedwell extracting solution of the invention, with octadecyl
Silane group silica gel is filler；Using acetonitrile or methanol as mobile phase A, using 2.0% acetum of mass concentration as Mobile phase B,
Regulation according to the form below carries out gradient elution；Detection wavelength is 258nm；Column temperature: 30 DEG C.Number of theoretical plate is calculated by protocatechuic acid peak
5000 should be not less than.
The preparation of reference substance solution: taking protocatechuic acid or other flavonoids reference substances appropriate, accurately weighed, adds volume dense
Spend 60% ethanol solution be made every 1ml containing 15 μ g solution to get.
The preparation of test solution: precision measurement Veronica linariifolia extract is appropriate, adds 60% ethanol solution of volumetric concentration to quarter
Degree, shake up to get.
Measuring method: accurate absorption reference substance solution and each 20 μ 1 of test solution respectively, injection liquid chromatograph, measurement,
To obtain the final product.
Embodiment 3
A kind of method using effective component protocatechuic acid in HPLC method detection bastard speedwell extracting solution of the invention, with octadecyl
Silane group silica gel is filler；Using acetonitrile or methanol as mobile phase A, using 0.4% phosphoric acid solution of mass concentration as Mobile phase B,
Regulation according to the form below carries out gradient elution；Detection wavelength is 260nm；Column temperature: 30 DEG C.Number of theoretical plate is calculated by protocatechuic acid peak
5000 should be not less than.
The preparation of reference substance solution: taking protocatechuic acid or other flavonoids reference substances appropriate, accurately weighed, adds volume dense
Spend 50% ethanol solution be made every 1ml containing 15 μ g solution to get.
The preparation of test solution: precision measurement Veronica linariifolia extract is appropriate, adds 50% ethanol solution of volumetric concentration to quarter
Degree, shake up to get.
Measuring method: accurate absorption reference substance solution and each 20 μ 1 of test solution respectively, injection liquid chromatograph, measurement,
To obtain the final product.
Embodiment 4
A kind of method using effective component protocatechuic acid in HPLC method detection bastard speedwell extracting solution of the invention, with octadecyl
Silane group silica gel is filler；Using acetonitrile or methanol as mobile phase A, using 0.8% phosphoric acid solution of mass concentration as Mobile phase B,
Regulation according to the form below carries out gradient elution；Detection wavelength is 265nm；Column temperature: 30 DEG C.Number of theoretical plate is calculated by protocatechuic acid peak
5000 should be not less than.
The preparation of reference substance solution: taking protocatechuic acid or other flavonoids reference substances appropriate, accurately weighed, adds volume dense
Spend 80% ethanol solution be made every 1ml containing 15 μ g solution to get.
The preparation of test solution: precision measurement Veronica linariifolia extract is appropriate, adds 80% ethanol solution of volumetric concentration to quarter
Degree, shake up to get.
Measuring method: accurate absorption reference substance solution and each 20 μ 1 of test solution respectively, injection liquid chromatograph, measurement,
To obtain the final product.
Embodiment 5
A kind of method using effective component protocatechuic acid in HPLC method detection bastard speedwell extracting solution of the invention, with octadecyl
Silane group silica gel is filler；Using acetonitrile or methanol as mobile phase A, using 0.5% acetum of mass concentration as Mobile phase B,
Regulation according to the form below carries out gradient elution；Detection wavelength is 260nm；Column temperature: 30 DEG C.Number of theoretical plate is calculated by protocatechuic acid peak
5000 should be not less than.
The preparation of reference substance solution: taking protocatechuic acid or other flavonoids reference substances appropriate, accurately weighed, adds volume dense
Spend 30% ethanol solution be made every 1ml containing 15 μ g solution to get.
The preparation of test solution: precision measurement Veronica linariifolia extract is appropriate, adds 30% ethanol solution of volumetric concentration to quarter
Degree, shake up to get.
Measuring method: accurate absorption reference substance solution and each 20 μ 1 of test solution respectively, injection liquid chromatograph, measurement,
To obtain the final product.
Embodiment 6
A kind of method using effective component protocatechuic acid in HPLC method detection bastard speedwell extracting solution of the invention, with octadecyl
Silane group silica gel is filler；Using acetonitrile or methanol as mobile phase A, using 1.5% acetum of mass concentration as Mobile phase B,
Regulation according to the form below carries out gradient elution；Detection wavelength is 260nm；Column temperature: 30 DEG C.Number of theoretical plate is calculated by protocatechuic acid peak
5000 should be not less than.
The preparation of reference substance solution: taking protocatechuic acid or other flavonoids reference substances appropriate, accurately weighed, adds volume dense
Spend 80% ethanol solution be made every 1ml containing 15 μ g solution to get.
The preparation of test solution: precision measurement Veronica linariifolia extract is appropriate, adds 80% ethanol solution of volumetric concentration to quarter
Degree, shake up to get.
Measuring method: accurate absorption reference substance solution and each 20 μ 1 of test solution respectively, injection liquid chromatograph, measurement,
To obtain the final product.
Embodiment 7
A kind of method using effective component protocatechuic acid in HPLC method detection bastard speedwell extracting solution of the invention, with octadecyl
Silane group silica gel is filler；Using acetonitrile or methanol as mobile phase A, using 0.1% phosphoric acid solution of mass concentration as Mobile phase B,
Regulation according to the form below carries out gradient elution；Detection wavelength is 260nm；Column temperature: 30 DEG C.Number of theoretical plate is calculated by protocatechuic acid peak
5000 should be not less than.
The preparation of reference substance solution: taking protocatechuic acid or other flavonoids reference substances appropriate, accurately weighed, adds volume dense
Spend 30% ethanol solution be made every 1ml containing 15 μ g solution to get.
The preparation of test solution: precision measurement Veronica linariifolia extract is appropriate, adds 30% ethanol solution of volumetric concentration to quarter
Degree, shake up to get.
Measuring method: accurate absorption reference substance solution and each 20 μ 1 of test solution respectively, injection liquid chromatograph, measurement,
To obtain the final product.
Embodiment 8
A kind of method using effective component protocatechuic acid in HPLC method detection bastard speedwell extracting solution of the invention, with octadecyl
Silane group silica gel is filler；Using acetonitrile or methanol as mobile phase A, using 1% phosphoric acid solution of mass concentration as Mobile phase B, press
Regulation in following table carries out gradient elution；Detection wavelength is 260nm；Column temperature: 30 DEG C.Number of theoretical plate is answered by the calculating of protocatechuic acid peak
Not less than 5000.
The preparation of reference substance solution: taking protocatechuic acid or other flavonoids reference substances appropriate, accurately weighed, adds volume dense
Spend 60% ethanol solution be made every 1ml containing 15 μ g solution to get.
The preparation of test solution: precision measurement Veronica linariifolia extract is appropriate, adds 60% ethanol solution of volumetric concentration to quarter
Degree, shake up to get.
Measuring method: accurate absorption reference substance solution and each 20 μ 1 of test solution respectively, injection liquid chromatograph, measurement,
To obtain the final product.
1, above-mentioned implementation method is verified
(1) system suitability
Protocatechuic acid reference substance is taken respectively, adds ethanol water that the solution of each about 20 μ g/ml is made, and is compareed as protocatechuic acid molten
Liquid；Taking ethanol water is blank solvent；Precision measures swelling and pain relieving and pastes medical fluid 2ml, sets in 10ml measuring bottle, adds ethanol water
It to scale, shakes up, as test solution；Negative control swelling and pain relieving is prepared by production technology and pastes medical fluid, and precision measures detumescence
Pain relieving plaster medical fluid 2ml, sets in 10ml measuring bottle, adds ethanol water to scale, shakes up, as negative control solution.It is accurate respectively
20 μ l are measured, liquid chromatograph is injected, record chromatogram.
1 protocatechuic acid check experiment result of table
Conclusion: protocatechuic acid peak type is good, meets the requirements with adjacent peak separating degree, noiseless in negative control；Test solution
100min is acquired, is occurred after 45min without other peaks, each compound elutes completely in the chromatography column in swelling and pain relieving patch medical fluid,
Acquisition time 50min.
(2) linear and range
Precision weighs protocatechuic acid reference substance 15.08mg and sets in 100ml measuring bottle, and scale is dissolved and be diluted to ethanol water,
Accurate absorption 0.5ml, 0.8ml, 1ml, 1.2ml, 1.5ml are set in 5 10ml measuring bottles again plus ethanol water is diluted to scale, point
The inaccurate above-mentioned 20 μ l of solution and 20 μ l of quantitative limit strength solution that measures injects liquid chromatograph, chromatogram is recorded, with concentration pair
Peak area carries out linear regression, and the regression equation of protocatechuic acid is y=69604x+4736.5.
2 protocatechuic acid linear relationship data of table
Shown in Fig. 2, the linear relationship chart of protocatechuic acid concentration and peak area.
(3) detection limit and quantitative limit
Precision weighs protocatechuic acid reference substance 15.08mg and sets in 100ml measuring bottle, and scale is dissolved and be diluted to ethanol water,
Accurate absorption 1ml is set in 10ml measuring bottle again plus ethanol water is diluted to scale, is gradually diluted to signal-to-noise ratio with ethanol water
It is calculated when about 10/1, chromatogram is recorded, as quantitative limit.It is gradually diluted to calculating when signal-to-noise ratio is about 3/1 with mobile phase, remembers
Chromatogram is recorded, as detection line.
3 quantitative limit test result of table
4 detection line test result of table
As a result: quantitative limit and detection line reach test requirements document
(4) sample introduction precision
Precision weighs that protocatechuic acid reference substance is appropriate, adds ethanol water that the solution containing about 15 μ g/ml of protocatechuic acid is made, as
Sample solution, precision measure 20 μ l, inject liquid chromatograph, continuous sample introduction 6 times, record chromatogram.
5 impurity sample introduction precision (peak area) of table
6 impurity sample introduction precision (retention time) of table
Conclusion: each impurity continuous sample introduction 6 times, for peak area RSD less than 2%, retention time RSD illustrates that impurity sample introduction is accurate less than 2%
Degree is good.
(5) stability of solution
Precision measures bastard speedwell extracting solution sample 2ml, sets in 10ml measuring bottle, adds stream ethanol water to be diluted to scale, shakes up, makees
For sample solution, sets and place 24 hours under conditions of room temperature, measured in 0,2,5,6,8,10 hour sample introduction, record chromatogram.
7 sample stability test result table of table
Conclusion: swelling and pain relieving patch assay test solution placed 10 hours at room temperature, at room temperature
Quality is stablized, and content RSD% is less than 1%.
(6) sample recovery rate
Precision weighs protocatechuic acid reference substance 14.93mg and sets in 100ml measuring bottle, and scale is dissolved and be diluted to ethanol water,
It is accurate again to draw each three parts of 0.3ml, 0.5ml, 0.7ml, 9 10ml measuring bottles are set respectively, and the water that 2ml is added in each measuring bottle is climing
Cyanines extracting solution, adds ethanol water to be diluted to scale, shakes up, as test solution；It is suitable that precision weighs protocatechuic acid reference substance
Amount, is dissolved with ethanol water and is diluted to the solution containing about 15 μ g/ml of protocatechuic acid, as reference substance solution；It takes respectively pair
Inject liquid chromatograph according to product solution and 20 μ l of test solution, record chromatogram, by external standard method with calculated by peak area to get.
8 sample recovery rate experimental result of table
As a result: the average recovery rate under each concentration should all be between 98%-101%, and the method accuracy drafted meets the requirements, and shows
This method rate of recovery is good.
By above method verifying it is found that the method that bastard speedwell of the invention extracts liquid hold-up control is stablized, reliably.
This method uses the absorption of octadecylsilane chemically bonded silica column (5 μm, 250mm × 4.6mm) to different compounds
Ability difference separates effective component in bastard speedwell with reaching, and controls so as to measure the content of its each middle ingredient
Its quality.As shown in Figure 1, each effective component is kept completely separate.
Claims (4)
1. a kind of method using effective component protocatechuic acid in HPLC method detection bastard speedwell extracting solution, it is characterised in that: with ten
Eight alkyl silane bonded silica gels are the filler of chromatographic column, using acetonitrile or methanol as mobile phase A, with mass concentration 0.5 2.0%
Acetum or 0.1 1.0% phosphoric acid solution of mass concentration are Mobile phase B, carry out gradient elution to chromatographic column, Detection wavelength is
255-265nm draws reference substance solution and test solution respectively, injects liquid chromatograph, measurement to get.
2. a kind of side using effective component protocatechuic acid in HPLC method detection bastard speedwell extracting solution according to claim 1
Method, it is characterised in that: elution requirement: the volume of mobile phase A and Mobile phase B are as follows: when 0≤t≤20 minute, 0 → 5 10:
100→95〜90；When 20 t≤30 minute <, 5-10:95-90；When 30 t≤35 minute <, 5 10 → 90 95:
90〜95→5〜10；When 50 minutes, 90-95:5-10.
3. a kind of side using effective component protocatechuic acid in HPLC method detection bastard speedwell extracting solution according to claim 1
Method, it is characterised in that: the preparation of reference substance solution: taking protocatechuic acid reference substance appropriate, adds 30% 80% ethyl alcohol of volumetric concentration molten
Liquid be made every 1ml containing 15 μ g solution to get.
4. a kind of side using effective component protocatechuic acid in HPLC method detection bastard speedwell extracting solution according to claim 1
Method, it is characterised in that: the preparation of test solution: water intaking turnip extract is appropriate, adds 30% 80% ethanol solution of volumetric concentration
To scale, shake up to get.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810867160.4A CN108982727A (en) | 2018-08-01 | 2018-08-01 | A method of using effective component protocatechuic acid in HPLC method detection bastard speedwell extracting solution |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810867160.4A CN108982727A (en) | 2018-08-01 | 2018-08-01 | A method of using effective component protocatechuic acid in HPLC method detection bastard speedwell extracting solution |
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| Publication Number | Publication Date |
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| CN108982727A true CN108982727A (en) | 2018-12-11 |
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| CN201810867160.4A Withdrawn CN108982727A (en) | 2018-08-01 | 2018-08-01 | A method of using effective component protocatechuic acid in HPLC method detection bastard speedwell extracting solution |
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| CN (1) | CN108982727A (en) |
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Application publication date: 20181211 |
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