CN101493445A - Method for measuring ferulaic acid content in propolis - Google Patents
Method for measuring ferulaic acid content in propolis Download PDFInfo
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- CN101493445A CN101493445A CNA2009101180566A CN200910118056A CN101493445A CN 101493445 A CN101493445 A CN 101493445A CN A2009101180566 A CNA2009101180566 A CN A2009101180566A CN 200910118056 A CN200910118056 A CN 200910118056A CN 101493445 A CN101493445 A CN 101493445A
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Abstract
The invention relates to a determination method for the content of ferulic acid in propolis, and the method smashes the pre-frozen propolis, extracts the ferulic acid from the powder by methanol, achieves effective separation of ferulic acid from the propolis sample on C18 chromatography column by the extract liquid through the liquid chromatography gradient elution method, and determines the content of ferulic acid under the detection wavelength of 316nm through the external standard method. The method comprises the following steps of: Step 1. preparing a ferulic acid standard solution; Step 2 preparing a to-be-detected propolis sample solution; Step 3. liquid chromatography analysis; and Step 4. calculating the content of ferulic acid in the sample through the external standard method. The pretreatment measures taken for the sample can improve the accuracy and stability of the detection results. In addition, the chromatography analysis adopts gradient elution to prevent strong preservation components in the propolis from interferring the continuous chromatography.
Description
Technical field
What the present invention relates to is the assay method of ferulaic acid content in a kind of propolis, belongs to the food security Measurement for Biotechnique.
Background technology
Propolis (propolis) is the resene material that honeybee is gathered from branch and the axillalry bud of collagen plant, the mandibular gland secretion and wax gland secretion and a small amount of pollen that add himself, by the biochemical reaction of complexity, chew the opaque colloid substance of a kind of aromaticity that processes through honeybee.Propolis contains many kinds healthy and helpful bioactie agent and some are possessed the material of pharmacologically active, and is of many uses at medical health field, because of its multiple efficacies, and is rare natural resources.
Forulic acid (ferulic acid) is topmost a kind of organic acid in the propolis, it also is a kind of phenolic acid that extensively exists in the plantage, being prevalent in the Chinese crude drugs such as rhizome of chuanxiong, Radix Angelicae Sinensis, asafoetide, scouring rush, rattletop, the white skin of camphor tree and spina date seed, is one of important composition of these Chinese medicines.Forulic acid is at medicine, food, and there is increasingly extensive purposes in fields such as cosmetics.Be used for treatment of diseases such as coronary heart disease, cerebrovascular disease, vasculitis, leucocyte and decrease of platelet clinically; In cosmetics, then use, have the effect that absorbs ultraviolet ray and anti-oxidation mainly as antioxidant.
The propolis component is very complicated, and the assay method of forulic acid in the propolis of bibliographical information mainly adopts efficient liquid-phase chromatography method, and idol has the human capillary electrophoresis method to measure.Great majority together carry out with other flavonoidss or phenolic acid usually to forulic acid check and analysis research, rare analysis and research to the single index of forulic acid in the propolis.
Usefulness liquid phase gradient elution method such as Polish scholar Jan Krzek are measured three organic acids such as forulic acids in the propolis simultaneously in conjunction with the method for RP18 solid-phase extraction column pre-treatment, and the forulic acid recovery reaches 99.42%, and relative standard deviation is controlled in 3%.Usefulness liquid chromatographies such as Ivona Jasprica have realized simultaneously 14 kinds of phenolic acid that comprise forulic acid and content of flavonoids are measured under 270nm detects wavelength, and the relative deviation of forulic acid measurement result is below 2%.
Domestic in Chinese crude drug the research of forulic acid context of detection more, as Radix Angelicae Sinensis, rhizome of chuanxiong or the like, and the mensuration of forulic acid is not carried out in a deep going way as yet in the propolis.Cao Yuhua etc. have measured simultaneously with capillary electrophoresis method and have contained forulic acid in the propolis at six kinds of interior active substances, and this method linearity, repeatability and the recovery are all good, and detectability can reach 0.37～1.8 μ g/mL.Usefulness combined with liquid chromatography diode array detector such as Yu Shifeng have successfully been measured four kinds of organic acid contents such as forulic acid in the propolis, and the forulic acid recovery 93.5%, the range of linearity be at 0.05～0.36 μ g, related coefficient 0.9990.Yu Min etc. have set up content of ferulic acid assay method in the propolis total flavones sample with high performance liquid chromatography, and the average recovery rate of method is 97.9%, and the forulic acid range of linearity is in 0.054～0.420 μ g, related coefficient 0.9995.The Zhao Jing that Ministry of Agriculture's bee product detects test center once did some explorations with high performance liquid chromatography to the mensuration of ferulaic acid content in the propolis, for various reasons, experiment fails to obtain the result of study of system perfecting, recently Zhao waits the people quietly and has developed the method that a Ultra Performance Liquid Chromatography technology is measured 12 kinds of active substances such as forulic acid in the propolis simultaneously, this method is a separating column with Acquity BEH C18 post, 0.4% phosphate aqueous solution and methyl alcohol are moving phase, gradient elution, the employing diode array detector detects, whole detachment process is finished in 9.5min, the forulic acid recovery is 98.4～99.8%, and minimum detectable level can reach 0.154mg/L." the bee product detection practical technique " that the Ministry of Agriculture publishes also included the method for high-performance liquid chromatogram determination propolis forulic acid, this method is a moving phase with methanol (45: 55), measure at the 340nm place with the C18 post, but the method is through a plurality of laboratory proofings, the reappearance existing problems are difficult to promotion and implementation.
In a word, to the extremely complicated propolis sample of composition, the detection by quantitative of its forulic acid does not still have ripe and the good liquid chromatographic detection technology of applicability so far.
Summary of the invention
The objective of the invention is to overcome the deficiency of above-mentioned existence, and provide a kind of specificity strong, highly sensitive liquid phase chromatography, forulic acid in the propolis is carried out assay, and judge the assay method of forulic acid in the propolis of ferulaic acid content in the propolis according to mark method beyond the liquid chromatography collection of illustrative plates of standard items and sample.
The ferulaic acid content assay method may further comprise the steps in the propolis of the present invention:
The preparation of step 1. standard solution: take by weighing the standard substance of a certain amount of forulic acid, be dissolved in the solution of special ratios and make;
The preparation of step 2. need testing solution: make through freezing, pulverizing, weighing, forced ultrasonic dissolving, centrifugal and filtering with microporous membrane etc. for the propolis that detects usefulness;
The preparation of standard solution in the step 1, the concrete operations step is as follows:
Accurately take by weighing 10.0mg forulic acid standard substance in the brown volumetric flask of 50ml, add 70% methyl alcohol and make its dissolving and be settled to scale, mixing is as standard solution.
The preparation of need testing solution in the step 2, the concrete operations step is as follows:
Sample is put in the refrigerator-freezer in freezing below-10 ℃, 20g～the 30g that materialses smashes with Syrup-homogenizing instrument rapidly, takes by weighing the about 0.5g of sample (being accurate to 0.1mg), place the brown volumetric flask of 50mL, add 35mL methyl alcohol, ultrasonic 15min adds 10mL water, shake up, behind the cool to room temperature, water is settled to scale, mixing; With the centrifugal 20min of the rotating speed of 4500rpm, supernatant filters with 0.45 μ m polyvinylidene fluoride microporous filtering film, and filtrate is need testing solution.
Liquid-phase chromatographic analysis in the step 3, the concrete operations step is as follows:
(a) chromatographic condition:
Chromatographic column: C18 chromatographic column, 5 μ m, 4.6mm * 200mm
Moving phase: with 0.085% phosphoric acid solution is mobile phase A, is Mobile phase B with methyl alcohol, is moving phase C with the acetonitrile, carries out gradient elution by table 1;
Table 1 forulic acid liquid chromatography gradient elution method:
| Time (min) | Flow velocity (mL/min) | 0.085% phosphoric acid solution A (%) | Methyl alcohol B (%) | Acetonitrile C (%) |
| 0～20 | 1.0 | 83 | 0 | 17 |
| 20～21 | 1.0→1.5 | 83→0 | 0→100 | 17→0 |
| 21～36 | 1.5 | 0 | 100 | 0 |
| 36～37 | 1.5 | 0→83 | 100→0 | 0→17 |
| 37～52 | 1.5 | 83 | 0 | 17 |
Sample size: 20 μ L
Detect wavelength: 316nm
Column temperature: 30 ℃
(b) measure: draw standard solution and need testing solution successively, inject liquid chromatograph, the record chromatogram.Same sample is carried out parallel experiment to be measured.
Calculating content of ferulic acid in the propolis test sample in the step 4, is that by formula (1) calculates the percentage composition of forulic acid in the test sample with external standard method.
X: content of ferulic acid in the test sample, unit is every kilogram (mg/kg) of milligram,
A
Sample: the chromatographic peak area of test sample,
C
Mark: the concentration of forulic acid in the standard solution, unit is every milliliter of microgram (μ g/mL),
A
Mark: the chromatographic peak area of standard solution,
The quality of m---sample, unit is gram (g).
50---sample constant volume (mL).
According to the requirement of content detection, above need testing solution preparation method and chromatographic condition obtain through a large amount of experiment sievings, and concrete experiment sieving situation is as follows:
1 detects wavelength determination: get forulic acid standard substance solution, scan at 200～400nm, at the 316nm place absorption maximum is arranged, so select 316nm as detecting wavelength.
2 chromatographic conditions:
Chromatographic column: C18 chromatographic column, 5 μ m, 4.6mm * 250mm
Moving phase: see Table 1 forulic acid liquid chromatography gradient elution method;
Wavelength: 316nm;
3 forulic acid standard inventory formulations prepared from solutions: precision takes by weighing forulic acid standard substance 10mg (being accurate to 0.01mg), puts in the brown measuring bottle of 50ml, adds 70% methyl alcohol and makes dissolving and be diluted to scale, shakes up; Promptly get (every 1ml contains forulic acid 200 μ g).This solution can be lower than 4 ℃ of refrigerator and cooled in temperature and hide preservation two months.
4 forulic acid standard operation solution: draw an amount of forulic acid standard inventory solution respectively: to the 100mL volumetric flask, be settled to scale with 70% methanol solution, be made into 0.10 μ g/ml, 0.20 μ g/ml, 1.0 μ g/ml, 2.0 μ g/ml, 4.0 μ g/ml, 6.0 μ g/ml, 10 μ g/ml, standard operation solution.Fresh preparation on the same day.
5 linear relationships are investigated:
Table 2 assay linear relationship test findings (n:7)
The test of 6 precision: the accurate forulic acid standard substance solution of drawing, repeat sample introduction 5 times, each 20 μ l measure, RSD:1.8% (n=5)
Table 3 Precision test result
7 stability tests; The same need testing solution of accurate absorption was measured once every 2 hours, measured 6 hours altogether, and RSD is 2.0% (n=4)
Table 4 stability test result
The test of 8 reappearances: precision takes by weighing 6 parts in same sample, presses the method operation of need testing solution preparation, and sample introduction 20 μ l measure, and measure peak area, calculate content, and RSD is 4.75% (n=6)
Table 5 reproducible test results
9 application of sample recovery tests
9.1 average recovery test 1: it is 6 parts of 0.270% propolis that precision takes by weighing the known content of measuring with this method, the respectively accurate reference substance a certain amount of (actual sample detection limit 0.4 times, 0.5 times, 0.6 times) that adds, press need testing solution preparation method operation, its average recovery rate is that 99.4%RSD is 1.8% (n=6).
Table 6 assay recovery test result (n:6)
9.2 application of sample recovery test 2: it is 6 parts of 0.200% propolis that precision takes by weighing the known content of measuring with this method, the respectively accurate reference substance a certain amount of (actual sample detection limit 0.5 times, 2 times, 5 times) that adds, press need testing solution preparation method operation, its average recovery rate is that 99.7%RSD is 1.2% (n=6).
Table 7 assay recovery test result (n:6)
The test of 10 sample extraction: adopt following extracting method respectively, measure by aforementioned liquid phase chromatography analytical method,
(1) take by weighing the 0.5g sample and put in the apparatus,Soxhlet's, to colourless, evaporate to dryness is used dissolve with methanol with the 100ml alcohol reflux.The ferulaic acid content measurement result is 1010mg/kg.
(2) take by weighing the 0.5g sample and put in the apparatus,Soxhlet's, to colourless, evaporate to dryness is used dissolve with methanol with 100ml acetone refluxing extraction.The ferulaic acid content measurement result is 1000mg/kg.
(3) take by weighing the 0.5g sample and put in the apparatus,Soxhlet's, extract colourlessly with the 100ml ethyl acetate backflow, evaporate to dryness is used dissolve with methanol.The ferulaic acid content measurement result is 1300mg/kg.
(4) handle the propolis sample with the method for need testing solution preparation among the present invention.The ferulaic acid content measurement result is 1870mg/kg.
The result who measures ferulaic acid content in the propolis with the method for need testing solution preparation among the present invention is 1870mg/kg.This method is the peak area maximum in four kinds of sample-pretreating methods, and the recovery also reaches more than 99% simultaneously, so extracting method is decided to be method of the present invention: the frozen propolis of learning from else's experience sample, smash with the electronic Syrup-homogenizing instrument of YJA-, take by weighing the about 0.5g of sample, place the brown volumetric flask of 50ml, add 35ml methyl alcohol, ultrasonic 15min, add 10ml water, shake up, behind the cool to room temperature, the water constant volume shakes up.Sample is put into hydro-extractor, with the centrifugal 20min of the rotating speed of 4500 commentaries on classics/min.With 0.45 μ m membrane filtration, filtrate is stand-by, promptly with supernatant.
The present invention is to be the forulic acid liquid chromatography detecting method of specimen exploitation with the propolis, has following characteristics:
(1) composition of propolis is very complicated, and its ferulaic acid content is not only low, and is difficult to separate.The forulic acid that the conventional chemical analytical approach detects in the propolis is difficult to obtain good specificity and sensitivity, and the present invention uses liquid-phase chromatography method to solve this problem.
(2) propolis is the stronger material of viscosity under a kind of normal temperature, the homogeneity of endoplasm own is not ideal enough, for making test sample more representative, the present invention adopts the method for cryogenic freezing to handle propolis raw material, it is good to make it fragility, get 20g～30g on this basis and carry out low-temperature grinding to obtain more uniform sample, make to be subjected to the representativeness of sample product better, it is more accurate and stable to detect data.
(3) composition complexity in the propolis, some component reserve capability on chromatographic column is very strong, and the isocratic elution chromatogram is these strong retained fractions of wash-out effectively, and follow-up chromatogram is had powerful interference, therefore can not carry out chromatogram continuously.The present invention adopts gradient elution method, guarantees that each chromatogram can both the strong retained fraction of wash-out after finishing, and continuous chromatography can be carried out.
(4) the present invention sets up the liquid chromatography detecting method of propolis forulic acid on the hardware foundation of C18 analytical column and UV-detector, current liquid chromatograph is widely-used at home, C18 analytical column and UV-detector all are the equipment that the most generally uses, therefore method provided by the invention has good application and popularization value, and is practical.
Show by experimental study, adopt analytical approach of the present invention, can measure content of ferulic acid in the propolis well, indexs such as its precision, accuracy, stability, reappearance and the range of linearity all meet the requirement of related standards regulation, prove absolutely that analytical approach of the present invention has scientific meaning and using value.
Description of drawings
Fig. 1 is a forulic acid standard substance uv scan collection of illustrative plates of the present invention;
Fig. 2 is a forulic acid standard substance chromatogram of the present invention;
Fig. 3 is the propolis sample chromatogram figure that contains forulic acid of the present invention;
Embodiment
The present invention will be described in detail below in conjunction with specific embodiment:
Embodiment:
Choose 10 parts of the propolis raw material in the different places of production, measure content of ferulic acid in the propolis by method provided by the invention.Concrete enforcement is as follows:
1, reagent and material
Except as otherwise herein provided, it is pure that agents useful for same is analysis; Water is: the one-level water of GB/T 6682 regulations (water is distilled water or equal purity water); When not indicating, all refer to aqueous solution with the preparation of which kind of solvent.
1.1 methyl alcohol; Chromatographically pure.
0.085% 1.2 (v/v) phosphoric acid solution: measure 0.85ml phosphoric acid, add water 1000ml dissolving, filter through 0.45 μ m.
1.3 acetonitrile: chromatographically pure.
1.4 forulic acid standard substance: available from Nat'l Pharmaceutical ﹠ Biological Products Control Institute, lot number is 110773-200611, purity 〉=99%.
1.5 forulic acid standard solution preparation: accurately take by weighing 10.0mg forulic acid standard substance in the brown volumetric flask of 50ml, adding 70% methyl alcohol makes its dissolving and is settled to scale, mixing, as standard solution, this solution can be lower than 4 ℃ of refrigerator and cooled in temperature and hide preservation two months.
2, instrument and equipment
2.1 liquid chromatograph: Agilent 100Series (the Agilent liquid chromatograph is furnished with UV-detector)
2.2 analytical balance: scale division value 0.1mg/0.01mg.
2.3 filtering membrane: 0.45 μ m polyvinylidene fluoride microporous filtering film.
2.4 Ultrasound Instrument (frequency is 25KHZ, and power is 50W).
2.5 hydro-extractor.
2.6YJA-electronic Syrup-homogenizing instrument.
3, determination step
3.1 sample is handled
Sample in smashing with Syrup-homogenizing instrument below 10 ℃, is taken by weighing the about 0.5g of sample (being accurate to 0.1mg), place the brown volumetric flask of 50ml, add 35ml methyl alcohol, ultrasonic 15min (frequency is 25KHZ, and power is 50W) adds 10ml water, shakes up, behind the cool to room temperature, water is settled to scale, mixing.Sample is put into hydro-extractor, with the centrifugal 20min of the rotating speed of 4500rpm.With 0.45 μ m membrane filtration, filtrate is used for liquid chromatogram measuring with clarified solution.
3.2 the chromatogram side is fixed
3.2.1 liquid phase chromatogram condition
A) chromatographic column: Hypersil ODS2 5 μ m 4.6mm * 200mm,
B) moving phase: acetonitrile-0.085% phosphoric acid solution (V/V=17: 83);
C) sample size: 20 μ l;
D) detect wavelength 316nm;
E) column temperature: 30 ℃;
3.2.2 liquid chromatogram measuring
Accurate respectively the absorption forulic acid standard operation solution and each 20 μ l of need testing solution injected liquid chromatograph, adopts gradient elution method assay determination shown in the table 8.
Table 8 detects the liquid chromatography gradient elution method of forulic acid in the propolis:
| Time (min) | Flow velocity (mL/min) | 0.085% phosphoric acid solution A (%) | Methyl alcohol B (%) | Acetonitrile C (%) |
| 0～20 | 1.0 | 83 | 0 | 17 |
| 20～21 | 1.0→1.5 | 83→0 | 0→100 | 17→0 |
| 21～36 | 1.5 | 0 | 100 | 0 |
| 36～37 | 1.5 | 0→83 | 100→0 | 0→17 |
| 37～52 | 1.5 | 83 | 0 | 17 |
3.3 parallel experiment
By above-mentioned steps, same sample is carried out parallel experiment measure.
4, the result calculates
By formula (1) calculates ferulaic acid content in the propolis sample.
X: content of ferulic acid in the test sample, unit is every kilogram (mg/kg) of milligram,
A
Sample: the chromatographic peak area of test sample,
C
Mark: the concentration of forulic acid in the standard solution, unit is every milliliter of microgram (μ g/mL),
A
Mark: the chromatographic peak area of standard solution,
The quality of m---sample, unit is gram (g).
50---sample constant volume (mL).
The data that record ferulaic acid content in the propolis in 10 batches of different places of production as stated above see Table 9:
The propolis ferulaic acid content table in 10 batches of different places of production of table 9
| Sequence number | The propolis collection point | Content of ferulic acid (mg/kg) |
| 1 | Changbai mountain, Jilin | 1870 |
| 2 | Dashiqiao, Liaoning | 560 |
| 3 | The Hebei mahjong | 1180 |
| 4 | Yongqing, Hebei | 140 |
| 5 | Nanyang, Henan | 1070 |
| 6 | The Jiangsu Jianhu | 340 |
| 7 | Mengcheng, Anhui | 2710 |
| 8 | Shou County, Anhui | 860 |
| 9 | Xianju, Zhejiang | 890 |
| 10 | The Guizhou waterside town | 1280 |
The invention provides a kind of liquid chromatography detecting method of measuring forulic acid in the propolis, this method is by the resulting practicable method of a large amount of tests, has good reappearance, and advantages such as specificity is strong, highly sensitive, popularization facility are arranged.
To those skilled in the art, according to technology contents disclosed by the invention, those skilled in the art will very clear other embodiments of the present invention.Under the situation of purport of the present invention and scope, those skilled in the art can carry out various changes or improvement to the present invention.For example, use the different gradient elution programs or the C18 chromatographic column of different length, may obtain the similar detection result.
Among Fig. 1:
Peak value detects
Among Fig. 2: horizontal ordinate is time (min), and ordinate is voltage (mv), and the numeral that indicates on each chromatographic peak is the retention time of this chromatographic peak.The indicated chromatographic peak of retention time 13.998min is the forulic acid chromatographic peak in this collection of illustrative plates.
Among Fig. 3: horizontal ordinate is time (min), and ordinate is voltage (mv), and the numeral that indicates on each chromatographic peak is the retention time of this chromatographic peak.The indicated chromatographic peak of retention time 13.657min is the forulic acid chromatographic peak in this collection of illustrative plates.
Claims (4)
1, the assay method of ferulaic acid content in a kind of propolis, it adopts the uv detection method in the high performance liquid chromatography that the forulic acid in the propolis raw material is carried out the qualitative and quantitative detection analysis, it is characterized in that this assay method may further comprise the steps:
The preparation of step 1. forulic acid standard solution: take by weighing the standard substance of a certain amount of forulic acid, be dissolved in the solution of special ratios and make;
The preparation of step 2. propolis test sample solution: make through freezing, pulverizing, weighing, forced ultrasonic dissolving, centrifugal and filtering with microporous membrane etc. for the propolis that detects usefulness;
Step 3. liquid-phase chromatographic analysis: sample introduction, carry out gradient elution on the C18 chromatographic column;
Step 4. is calculated for detecting content of ferulic acid in the propolis sample.
2, the assay method of ferulaic acid content in the propolis according to claim 1 is characterized in that, the preparation of standard solution in the step 1, and the concrete operations step is as follows:
Accurately take by weighing 10.0mg forulic acid standard substance in the 50ml volumetric flask, add 70% methyl alcohol and make its dissolving and be settled to scale, mixing is as standard solution;
The preparation of propolis test sample solution in the step 2, the concrete operations step is as follows:
The propolis sample is put in the refrigerator-freezer in freezing below-10 ℃, and the 20g～30g that materialses smashes with Syrup-homogenizing instrument rapidly, take by weighing the about 0.5g of sample, and be accurate to 0.1mg, and place the brown volumetric flask of 50mL, add 35mL methyl alcohol, ultrasonic 15min, add 10mL water, shake up, behind the cool to room temperature, water is settled to scale, mixing; With the centrifugal 20min of the rotating speed of 4500rpm, supernatant filters with 0.45 μ m polyvinylidene fluoride microporous filtering film, and filtrate is need testing solution;
Carry out step 3 liquid-phase chromatographic analysis after step 1 and the step 2.
3, the assay method of ferulaic acid content in the propolis according to claim 1 and 2 is characterized in that the liquid-phase chromatographic analysis in the described step 3, and the concrete operations step is as follows:
(a) chromatographic condition:
Chromatographic column: C18 chromatographic column, 5 μ m, 4.6mm * 200mm;
Moving phase: with 0.085% phosphoric acid solution is mobile phase A, is Mobile phase B with methyl alcohol, is moving phase C with the acetonitrile, carries out gradient by method as shown in the table and washes:
Sample size: 20 μ L; Detect wavelength: 316nm; Column temperature: 30 ℃;
(b) measure: draw standard solution and propolis test sample solution successively, inject liquid chromatograph, measure, the record chromatogram.
4, the assay method of ferulaic acid content in the propolis according to claim 1 is characterized in that content of ferulic acid is calculated in the described solution, is to calculate content of ferulic acid in the test sample with external standard method by following (1) formula, promptly carry out step 4;
In the formula:
X: content of ferulic acid in the test sample, unit is every kilogram (mg/kg) of milligram,
A
Sample: the forulic acid chromatographic peak area of test sample,
C
Mark: the concentration of forulic acid in the standard solution, unit is every milliliter of microgram (μ g/mL),
A
Mark: the forulic acid chromatographic peak area of standard solution,
The quality of m---sample, unit is gram (g).
50---sample constant volume (mL).
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103105447A (en) * | 2011-11-09 | 2013-05-15 | 贵州益佰制药股份有限公司 | Detection method for Cinnamomum migao heart-comforting preparation |
| CN104237404A (en) * | 2014-09-04 | 2014-12-24 | 贵州信邦制药股份有限公司 | Method for measuring content of ferulic acid in Yixinshu preparations |
| CN104407030A (en) * | 2014-12-12 | 2015-03-11 | 广西科技大学 | Preparation method for ferulic acid/methacrylic acid molecularly imprinted polymer modified glassy carbon electrodes |
-
2009
- 2009-02-17 CN CNA2009101180566A patent/CN101493445A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103105447A (en) * | 2011-11-09 | 2013-05-15 | 贵州益佰制药股份有限公司 | Detection method for Cinnamomum migao heart-comforting preparation |
| CN103105447B (en) * | 2011-11-09 | 2014-09-24 | 贵州益佰制药股份有限公司 | Detection method for Cinnamomum migao heart-comforting preparation |
| CN104237404A (en) * | 2014-09-04 | 2014-12-24 | 贵州信邦制药股份有限公司 | Method for measuring content of ferulic acid in Yixinshu preparations |
| CN104407030A (en) * | 2014-12-12 | 2015-03-11 | 广西科技大学 | Preparation method for ferulic acid/methacrylic acid molecularly imprinted polymer modified glassy carbon electrodes |
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