CN106841414A - The detection method of Gardenoside and paeoniflorin content in a kind of chinaberry Cape jasmine oral liquid - Google Patents
The detection method of Gardenoside and paeoniflorin content in a kind of chinaberry Cape jasmine oral liquid Download PDFInfo
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- CN106841414A CN106841414A CN201611154596.6A CN201611154596A CN106841414A CN 106841414 A CN106841414 A CN 106841414A CN 201611154596 A CN201611154596 A CN 201611154596A CN 106841414 A CN106841414 A CN 106841414A
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- chinaberry
- cape jasmine
- mixed liquor
- gardenoside
- oral liquid
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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
Abstract
The present invention relates to the detection method of Gardenoside and paeoniflorin content in a kind of chinaberry Cape jasmine oral liquid, comprise the following steps：Chinaberry Cape jasmine oral liquid sample 2ml is measured by pipette；Chinaberry Cape jasmine oral liquid sample to measuring carries out water-bath concentration, and the chinaberry Cape jasmine oral liquid sample after being concentrated to water-bath adds methyl alcohol 20ml to be mixed, and weighed weight is carried out to gained mixed liquor；Carry out sending ultrasonic wave to mixed liquor, carry out 10~30min of ultrasonication, the mixed liquor after must processing；The weight of mixed liquor after treatment is supplied with methyl alcohol, the mixed liquor to supplying weight is filtered, and obtains final product need testing solution；Paeoniflorin, Gardenoside reference substance solution are prepared with methyl alcohol, need testing solution is measured by liquid chromatograph, sample introduction 10ul, the content of Gardenoside and Paeoniflorin in need testing solution is calculated with external standard two-point method logarithmic equation respectively respectively, obtains the content of Gardenoside and Paeoniflorin in need testing solution.Compared with the prior art, the present invention is simple to operate, accurate, reproducible, for the quality control of chinaberry Cape jasmine oral liquid provides the feasible foundation of science.
Description
Technical field
The present invention relates to drug measurement techniques field, Gardenoside and paeoniflorin content in more particularly to a kind of chinaberry Cape jasmine oral liquid
Detection method.
Background technology
Chinaberry Cape jasmine oral liquid is Chinese medicine preparation, is made up of the taste Chinese medicine of the coptis, the root of herbaceous peony, cape jasmine, corydalis tuber etc. 8, is clear brownish red
Prescribed liquid, bitter is sweet be long placed in after have a small amount of precipitation, jog is fugitive.There is regulating qi to disperse stagnation, clearing away heat to and alleviating pain, clinic is usually used in
Stomachache partial heat person, chronic gastritis, the acute attack of gastric and duodenal ulcer are evident in efficacy.Former standard preparation, checks project bag
Include proterties, discriminating, check, and differentiate that the thin layer that item only has Gardenoside differentiates, chinaberry Cape jasmine oral liquid assay is there are no at present
Research report.To improve standard preparation, quality is controlled, ensure the clinical efficacy and drug safety of chinaberry Cape jasmine oral liquid, it is necessary to right
Set up the detection method of Gardenoside and paeoniflorin content in a kind of chinaberry Cape jasmine oral liquid.
The content of the invention
The technical problems to be solved by the invention are to provide the inspection of Gardenoside and paeoniflorin content in a kind of chinaberry Cape jasmine oral liquid
Survey method.
The technical scheme that the present invention solves above-mentioned technical problem is as follows：Gardenoside and Paeoniflorin contain in a kind of chinaberry Cape jasmine oral liquid
The detection method of amount, comprises the following steps：
Step 1. measures chinaberry Cape jasmine oral liquid sample 2ml by pipette；
The chinaberry Cape jasmine oral liquid sample that step 2. pair is measured carries out water-bath concentration, the chinaberry Cape jasmine oral liquid sample after being concentrated to water-bath
Add methyl alcohol 20ml to be mixed, weighed weight is carried out to gained mixed liquor；
Step 3. carries out sending ultrasonic wave to mixed liquor, carries out 10~30min of ultrasonication, the mixing after must processing
Liquid；
Step 4., to methyl alcohol is added in the mixed liquor after treatment, supplies mixed liquor after treatment according to the weighed weight of mixed liquor
Weight, the mixed liquor to supplying weight filters, and obtains final product need testing solution；
Step 5. is measured by the chromatographic condition of setting by liquid chromatograph to need testing solution, and Cape jasmine is prepared with methyl alcohol
Sub- glycosides and Paeoniflorin reference substance solution, sample introduction 10ul respectively, in calculating need testing solution respectively with external standard two-point method logarithmic equation
The content of Gardenoside and Paeoniflorin, obtains the content of Gardenoside and Paeoniflorin in need testing solution.
Further, in step 2, claim the mixed liquor to obtained by weighed weight as electronic balance.
Further, in step 3, mixed liquor is carried out by ultrasonic cleaner send ultrasonic wave, carries out ultrasonication
20min。
The beneficial effects of the invention are as follows：The method of foundation is simple to operate, accurate, reproducible, is the matter of chinaberry Cape jasmine oral liquid
Amount control is there is provided the feasible foundation of science.
Specific embodiment
It is described below in conjunction with to principle of the invention and feature, example is served only for explaining the present invention, not uses
In restriction the scope of the present invention.
The detection method of Gardenoside and paeoniflorin content, comprises the following steps in a kind of chinaberry Cape jasmine oral liquid：
Step 1. measures chinaberry Cape jasmine oral liquid sample 2ml by pipette；
The chinaberry Cape jasmine oral liquid sample that step 2. pair is measured carries out water-bath concentration, the chinaberry Cape jasmine oral liquid sample after being concentrated to water-bath
Add methyl alcohol 20ml to be mixed, weighed weight is carried out to gained mixed liquor；
Step 3. carries out sending ultrasonic wave to mixed liquor, carries out 10~30min of ultrasonication, the mixing after must processing
Liquid；
Step 4., to methyl alcohol is added in the mixed liquor after treatment, supplies mixed liquor after treatment according to the weighed weight of mixed liquor
Weight, the mixed liquor to supplying weight filters, and obtains final product need testing solution；
Step 5. is measured by the chromatographic condition of setting by liquid chromatograph to need testing solution, and Cape jasmine is prepared with methyl alcohol
Sub- glycosides and Paeoniflorin reference substance solution, sample introduction 10ul respectively, in calculating need testing solution respectively with external standard two-point method logarithmic equation
The content of Gardenoside and Paeoniflorin, obtains the content of Gardenoside and Paeoniflorin in need testing solution.
In above-described embodiment, in step 2, claim the mixed liquor to obtained by weighed weight as electronic balance.
In above-described embodiment, in step 3, mixed liquor is carried out by ultrasonic cleaner send ultrasonic wave, carry out ultrasound
Ripple processes 20min.
Optionally, as one embodiment of the present of invention：The inspection of Gardenoside and paeoniflorin content in a kind of chinaberry Cape jasmine oral liquid
Survey method, step following steps：
1st, instrument and reagent
Instrument：Tlc silica gel plate Si60 (Merck), the high performance liquid chromatographs of Waters 2685；UV-detector；
METTLER AE240 electronic balances；AS7240BT type ultrasonic cleaners；
Reagent：Coptis control medicinal material (lot number 913-9404), Berberine hydrochloride (lot number 110713-201212) corydalis tuber pair
According to medicinal material (lot number 120928-201208) tetrahydropalmatine (lot number 110726-201414), Paeoniflorin (lot number 110736-
201539, content 96.4%), Gardenoside (lot number 110749-201115, content 99.7%), be purchased from Chinese food medicine inspection
Determine research institute.Methyl alcohol, methyl alcohol are chromatographically pure, other reagents to analyze pure, distilled water and distilled water for this laboratory is made by oneself.
2 methods and result
The discriminating of 2.1 coptiss
3 crowdes of each 10ml of sample are taken, water bath method, plus methyl alcohol 2ml dissolvings is put, as need testing solution.The same method of negative sample
Prepare.Another to take coptis control medicinal material 0.25g, plus methyl alcohol 25ml, water bath method, plus 2ml are put in ultrasonication 30 minutes, filtration
Methyl alcohol dissolves, and obtains control medicinal material solution, then takes Berberine hydrochloride reference substance, plus methyl alcohol is made solution of every 1ml containing 0.5mg, makees
It is reference substance solution；According to thin-layered chromatography [1] experiment, above-mentioned reference substance solution and each 1ul of control medicinal material solution, test sample are drawn
Solution 5ul, puts on same high-efficient silica gel G lamellaes, with cyclohexane-ethyl acetate-isopropanol-methanol-water-triethylamine respectively
(3：3.5：1：1.5：0.5：1) it is solvent, puts in the expansion cylinder with strong ammonia solution presaturation 20 minutes, launch, take out, dries in the air
It is dry, put and inspect under ultraviolet lamp (365nm).In test sample chromatogram, with the relevant position of control medicinal material chromatogram on, show identical face
The fluorescence spot of color.
The discriminating of 2.2 corydalis tubers
3 crowdes of each 10ml of sample are taken, enriching ammonia solution is adjusted to alkalescence, shaken with ether and extracted 2 times, each 20ml merges second
Ether liquid, is evaporated, and residue adds the methyl alcohol 1ml to make dissolving, used as need testing solution.Negative sample is prepared with method.It is another to take corydalis tuber control
Medicinal material 1g, plus methyl alcohol 50ml, ultrasonically treated 30 minutes, filtration, filtrate was evaporated, and the residue 10ml that adds water makes dissolving, is shaken with ether
Extraction is shaken to rise for 2 times with method operation, as control medicinal material solution.Tetrahydropalmatine reference substance is taken again, plus methyl alcohol is made every 1ml and contains
The solution of 0.5mg, as reference substance solution.According to thin-layered chromatography experiment, each 10ul of above-mentioned three kinds of solution is drawn, put in same respectively
On one silica gel g thin-layer plate with the preparation of 1% sodium hydroxide solution, with toluene-acetone (9:2) it is solvent, launches, take out, dries in the air
It is dry, put and taken out after about 3 minutes in iodine cylinder, after waving the iodine adsorbed on most plate, put and inspect under ultraviolet lamp (365nm).Test sample color
In spectrum, with the relevant position of control medicinal material chromatogram on, show same color fluorescence spot.
2.3 assays
2.3.1 chromatographic condition and system suitability
Waters SunFire C18 posts；With the phosphoric acid solution of acetonitrile -0.2% (15:85) it is mobile phase；Flow velocity is 1.0ml/
min；PDAD, Detection wavelength 238nm；The μ l of sample size 10；Separating degree is 12.0.
2.3.2 the preparation of need testing solution
Precision measures sample 2ml, and water-bath concentration is near dry, plus methyl alcohol 20ml, weighed weight, ultrasonic 20min, supplies weight,
Filtering, obtains final product.
2.3.2 the preparation of reference substance solution
Precision weighs Paeoniflorin reference substance, each 10mg of Gardenoside reference substance respectively, is respectively placed in 25ml volumetric flasks, plus first
Alcohol dissolved dilution to scale, as reference substance solution.
2.3.3 linear relationship is investigated
Precision draws above-mentioned reference substance solution each 0.1ml, 0.2ml, 0.5ml, 1ml, 2.5ml, 5ml, splits 10ml capacity
In bottle, with methanol dilution to scale, reference substance solution is added, totally 7 points, determined by above-mentioned chromatographic condition.With reference substance sample introduction
Amount X is abscissa, and peak area Y is ordinate, draws standard curve, and carries out linear regression, obtains Gardenoside linear equation：y
=15,632,589.2435 x+4,152.9233 R2=0.9998 and Paeoniflorin linear equation：Y=11,304,405.0167
X-16,659.0977 R2=1.0000 results show that Gardenoside sample size is in 0.0041~0.4000 μ g ranges, Paeoniflorin
Sample size is in good linear relationship with respective integrating peak areas value in 0.0041~0.4064 μ g ranges；
2.3.4 precision test
Gardenoside reference substance solution 5ml, Paeoniflorin reference substance solution 1ml are taken, in putting same 10ml volumetric flasks, plus methyl alcohol is dilute
Release to scale.Used as mixed reference substance solution, continuous sample introduction 6 times determines peak area respectively, and as a result Gardenoside peak area is average
It is that 3066023, RSD is 0.31% to be worth, and the average value of Paeoniflorin peak area is 0.43% for 437561, RSD, shows instrument essence
Density is good.
2.3.5 stability
Precision draws same need testing solution, in 0 after preparation, 2,4,8,12h when determine peak area, Gardenoside peak area
Average value is that 4692318, RSD is 0.61%, and the average value of Paeoniflorin peak area is 1.42% for 397366, RSD, is illustrated for examination
Product solution stabilization in 12h.
2.3.6 replica test
6 parts of chinaberry Cape jasmine oral liquid sample is taken, need testing solution is prepared by " preparation of 2.3.2 reference substance solutions " method, sample introduction,
The content of Gardenoside, Paeoniflorin in determination sample, Gardenoside, paeoniflorin content RSD are respectively 1.0% and 1.2%.Show method
It is repeated good.
2.3.7 average recovery experiment
Precision measures the chinaberry Cape jasmine oral liquid 2ml of known content, and totally 6 parts, difference is accurate to add 1ml mixed reference substance solutions
(Gardenoside 0.1998mg/ml, Paeoniflorin 0.04064mg/ml), is operated by " preparation of 2.3.2 reference substance solutions " method, must be added
Sample reclaims need testing solution.Reference substance solution, sample-adding being drawn respectively and reclaiming need testing solution 10ul, sample introduction, root shines this paper chromatograms
Condition is determined, and the content of Gardenoside, Paeoniflorin is calculated according to external standard two-point method logarithmic equation, and calculates the rate of recovery, the results are shown in Table 1,
Table 2.
The Determination of Gardenoside measurement result of table 1 and the rate of recovery
The paeoniflorin content measurement result of table 2 and the rate of recovery
2.4 sample sizes are determined
Above-mentioned 6 batches of chinaberrys Cape jasmine oral liquid sample is taken, need testing solution is prepared by " preparation of 2.3.2 reference substance solutions " method,
Chromatographic condition by drafting is measured, and sample introduction 10ul, Gardenoside, Paeoniflorin are counted with external standard two-point method logarithmic equation respectively respectively
Content, the results are shown in Table 3.
The sample size measurement result (n=4) of table 3
3. conclusion
The selection of 3.1 mobile phases
The systems such as mobile phase acetonitrile-water (15: 85), the second eyeball -1% acetic acid (13: 87) different to high performance liquid chromatography are entered
Go and compared, as a result shown：With the phosphoric acid solution of acetonitrile -0.2% (15:85) when for mobile phase, in chinaberry Cape jasmine oral liquid Gardenoside and
Completely, peak shape stabilization, other compositions are not disturbed for the separation of Paeoniflorin.
3.2 selections for determining wavelength and detector
Gardenoside, Paeoniflorin reference substance UV scanning maximum absorption wavelength are respectively 238,230nm, and selection 238nm is survey
Standing wave is long, compares the measurement result of UV-detector, PDAD, and selection PDAD is surveyed simultaneously
Determine the content of Gardenoside, Paeoniflorin, obtain result relatively satisfactory.
The selection of 3.3 solvents and extracting method
Investigated ultrasonic extraction and heating and refluxing extraction method respectively, and investigated various concentrations Extraction solvent (methyl alcohol,
20% methyl alcohol, 50% methyl alcohol) and different extraction times (15,30,40,60min) result.Through comparing, optimal extracting method is：
Precision measures sample 2ml, and water-bath concentration is near dry, plus methyl alcohol 20ml, weighed weight, ultrasonic 20min, supplies weight.
3.4 compared with existing standard, and ingredient hydrochloric acid is small during the chinaberry Cape jasmine oral liquid main ingredient coptis, corydalis tuber are increased herein
The Qualitive test of bark of a cork tree alkali, tetrahydropalmatine, while increased ingredient Gardenoside in the main ingredient root of herbaceous peony, cape jasmine, Paeoniflorin containing
Quantity measuring method.The present invention is simple to operate, accurate, reproducible, and for the quality control of chinaberry Cape jasmine oral liquid, to provide science feasible
Foundation.
The foregoing is only presently preferred embodiments of the present invention, be not intended to limit the invention, it is all it is of the invention spirit and
Within principle, any modification, equivalent substitution and improvements made etc. should be included within the scope of the present invention.
Claims (3)
1. in a kind of chinaberry Cape jasmine oral liquid Gardenoside and paeoniflorin content detection method, it is characterised in that comprise the following steps：
Step 1. measures chinaberry Cape jasmine oral liquid sample 2ml by pipette；
The chinaberry Cape jasmine oral liquid sample that step 2. pair is measured carries out water-bath concentration, and the chinaberry Cape jasmine oral liquid sample after being concentrated to water-bath is added
Methyl alcohol 20ml is mixed, and weighed weight is carried out to gained mixed liquor；
Step 3. carries out sending ultrasonic wave to mixed liquor, carries out 10~30min of ultrasonication, the mixed liquor after must processing；
Step 4., to methyl alcohol is added in the mixed liquor after treatment, supplies the weight of mixed liquor after treatment according to the weighed weight of mixed liquor
Amount, the mixed liquor to supplying weight is filtered, and obtains final product need testing solution；
Step 5. is measured by the chromatographic condition of setting by liquid chromatograph to need testing solution, and Gardenoside is prepared with methyl alcohol
With Paeoniflorin reference substance solution, sample introduction 10ul, cape jasmine in need testing solution is calculated with external standard two-point method logarithmic equation respectively respectively
The content of glycosides and Paeoniflorin, obtains the content of Gardenoside and Paeoniflorin in need testing solution.
2. according to claim 1 in a kind of chinaberry Cape jasmine oral liquid Gardenoside and paeoniflorin content detection method, its feature exists
In：In step 2, claim the mixed liquor to obtained by weighed weight as electronic balance.
3. according to claim 1 in a kind of chinaberry Cape jasmine oral liquid Gardenoside and paeoniflorin content detection method, its feature exists
In：In step 3, mixed liquor is carried out by ultrasonic cleaner send ultrasonic wave, carry out ultrasonication 20min.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101987121A (en) * | 2009-08-05 | 2011-03-23 | 漳州片仔癀药业股份有限公司 | Detection method of medicine composition for treating hepatitis |
| CN106053702A (en) * | 2016-07-29 | 2016-10-26 | 吉林化工学院 | Multi-ingredient content measuring method of Jiaweixiaoyao pills |
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2016
- 2016-12-14 CN CN201611154596.6A patent/CN106841414A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101987121A (en) * | 2009-08-05 | 2011-03-23 | 漳州片仔癀药业股份有限公司 | Detection method of medicine composition for treating hepatitis |
| CN106053702A (en) * | 2016-07-29 | 2016-10-26 | 吉林化工学院 | Multi-ingredient content measuring method of Jiaweixiaoyao pills |
Non-Patent Citations (2)
| Title |
|---|
| 杨庆胜 等: "HPLC同时测定加味逍遥丸中栀子苷和芍药苷的含量", 《中国现代中药》 * |
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Application publication date: 20170613 |