CN109298097A - A kind of detection method of the anti-ginseng itching-relieving granule of Chinese patent drug - Google Patents
A kind of detection method of the anti-ginseng itching-relieving granule of Chinese patent drug Download PDFInfo
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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Abstract
The present invention relates to a kind of detection methods of the anti-ginseng itching-relieving granule of Chinese patent drug, it the described method comprises the following steps: step 1, the preparation of reference substance solution: taking hederagenin, oleanolic acid, linamarin, matrine, Atisine chloride Atractydin, Ligustilide, rehmannioside, Panaxynol, arctiin, D-menthone, ammonium glycyrrhetate, timosaponin, ferulic acid that methanol is added to be configured to reference substance stock solution；Each reference substance stock solution is mixed to get reference substance mixed solution；Step 2, the preparation of test solution: taking anti-ginseng itching-relieving granule, extracted with methanol, the test solution after being extracted；Step 3, it detects: reference substance mixed solution and test solution being injected separately into high performance liquid chromatograph, obtain chromatogram, according to the absorption peak position in chromatogram and peak area is absorbed, by the content that each component absorption peak and each component is calculated.
Description
Technical field:
It is the present invention relates to a kind of detection method of Chinese materia medica preparation, in particular to a variety of in a kind of anti-ginseng itching-relieving granule of Chinese patent drug
The measuring method of ingredient.
Background technique:
The Chinese patent drug that anti-ginseng itching-relieving granule one kind has listed, is produced by Liaoning Kangchen Pharmaceutical Co., Ltd., in formula
Including schizonepeta, radix saposhnikoviae, kuh-seng, rhizoma atractylodis, cicada slough, great burdock achene, caulis akebiae, Radix Angelicae Sinensis, rhizoma anemarrhenae, radix rehmanniae recen, Radix Glycyrrhizae, linseed, gypsum etc.
Chinese medicine is clinically used for acute urticaria with the antipruritic effect of expelling wind and clearing away heat, eliminating dampness.Anti- ginseng itching-relieving granule quality standard is recorded
In " new drug become a full member standard " the 86th, only the ferulic acid in other side, matrine have carried out assay in standard.However Chinese medicine medicine
The generation of effect is that a variety of chemical components act synergistically as a result, therefore the quality control of Chinese medicine should also select multiple chemical components to make
For Testing index.Therefore, carrying out multicomponent assay to herbal mixture is particularly important.
Our systems have carried out the quality controling research of anti-ginseng itching-relieving granule, determine dextrorotation peppermint in anti-ginseng itching-relieving granule
Ketone, Panaxynol, matrine, Atisine chloride Atractydin, arctiin, oleanolic acid, hederagenin, Ligustilide, ferulic acid, rhizoma anemarrhenae soap
The content of 13 kinds of chemical components such as glycosides, matrine, ammonium glycyrrhetate, linamarin.
Summary of the invention
The present invention provides a kind of detection method of anti-ginseng itching-relieving granule of Chinese patent drug, the described method comprises the following steps:
Step 1, the preparation of reference substance solution
Take hederagenin, oleanolic acid, linamarin, matrine, Atisine chloride Atractydin, Ligustilide, rehmannioside, ginseng alkynes
Alcohol, arctiin, D-menthone, ammonium glycyrrhetate, timosaponin, ferulic acid add methanol to be configured to reference substance stock solution；
Each reference substance stock solution is mixed to get reference substance mixed solution.
Step 2, the preparation of test solution
Anti- ginseng itching-relieving granule is taken, is extracted with methanol, the test solution after being extracted；
Step 3, it detects
Reference substance mixed solution and test solution are injected separately into high performance liquid chromatograph, chromatogram is obtained, according to color
Absorption peak position and absorption peak area in spectrogram, by the content that each component absorption peak and each component is calculated；
Wherein the chromatographic condition of high performance liquid chromatography is as follows:
Chromatographic column Agilent-ZORBAX Eclipse Plus C18；
Mobile phase: 0.01% formic acid water (A)-acetonitrile (B),
Using gradient elution, elution program is as follows:
2 μ L of sample volume；
Flow velocity 0.3mL/min；
Detection wavelength 0~30min, 220nm；30~35.5min, 254nm；35.5~45.0min, 330nm；
35 DEG C of column temperature.
Preferred detection method of the invention, steps are as follows:
Step 1, the preparation of reference substance solution
Take hederagenin, oleanolic acid, linamarin, matrine, Atisine chloride Atractydin, Ligustilide, rehmannioside, ginseng alkynes
Alcohol, arctiin, D-menthone, ammonium glycyrrhetate, timosaponin, ferulic acid each 8-12mg, it is accurately weighed, it is placed in 8-12mL capacity
In bottle, methanol is added to be configured to reference substance stock solution；Take each reference substance stock solution that 45-55mL volumetric flask constant volume is added in right amount to quarter
Line mixes, obtains concentration and be respectively as follows: hederagenin 36-37 μ g/mL, oleanolic acid 23-24 μ g/mL, linamarin 38-39 μ
G/mL, matrine 62-63 μ g/mL, rehmannioside 55-56 μ g/mL, Panaxynol 43-44 μ g/mL, arctiin 30-31 μ g/mL, the right side
Revolve menthones 20-21 μ g/mL, ammonium glycyrrhetate 85-86 μ g/mL, timosaponin 58-59 μ g/mL, ferulic acid 71-72 μ g/mL, grey
The mixed reference substance solution of art element 42-43 μ g/mL, Ligustilide 53-54 μ g/mL；
Step 2, the preparation of test solution
Anti- ginseng itching-relieving granule is taken, is crushed, is taken 0.4-0.6g, set in 20-30mL volumetric flask, methanol is added, is ultrasonically treated 5-
15min is settled to groove, takes out 1-2mL, adds the methanol solution dilution such as 40-60%, is centrifuged 5-15min, and supernatant is to supply
Test sample solution；
Step 3, it detects
Reference substance solution and test solution 1-3 μ L are injected separately into high performance liquid chromatograph, chromatogram is obtained, according to color
Absorption peak position and absorption peak area in spectrogram, are calculated the content of each component absorption peak and each component.
Wherein chromatographic condition is same as above.
Most preferably, measuring method of the invention, steps are as follows:
Step 1, the preparation of reference substance solution
Take hederagenin, oleanolic acid, linamarin, matrine, Atisine chloride Atractydin, Ligustilide, rehmannioside, ginseng alkynes
Alcohol, arctiin, D-menthone, ammonium glycyrrhetate, timosaponin, ferulic acid each 10mg, it is accurately weighed, it is placed in 10mL volumetric flask
In, add methanol to be configured to reference substance stock solution；It takes each reference substance stock solution that 50mL volumetric flask constant volume is added in right amount to groove, mixes
It is even, obtain concentration be respectively as follows: 36.28 μ g/mL of hederagenin, 23.60 μ g/mL of oleanolic acid, 38.51 μ g/mL of linamarin,
62.45 μ g/mL of matrine, 55.26 μ g/mL of rehmannioside, 43.10 μ g/mL of Panaxynol, 30.25 μ g/mL of arctiin, dextrorotation are thin
20.73 μ g/mL of lotus ketone, 85.33 μ g/mL of ammonium glycyrrhetate, 58.39 μ g/mL of timosaponin, 71.42 μ g/mL of ferulic acid, Atisine chloride Atractydin
The mixed reference substance solution of 42.55 μ g/mL, 53.74 μ g/mL of Ligustilide；
Step 2, the preparation of test solution
Anti- ginseng itching-relieving granule is taken, crushes, takes 0.5g, it is accurately weighed, it sets in 25mL volumetric flask, addition proper amount of methanol, close plug,
It is ultrasonically treated (power 300W, frequency 40kHz) 10min, lets cool, is settled to groove, shake up, take 1mL, add 50% methanol of 1ml molten
Liquid dilution, mixes, and 14000rpm is centrifuged 10min, supernatant, that is, test solution；
Step 3, it detects
Reference substance solution and 2 μ L of test solution are injected separately into high performance liquid chromatograph, chromatogram is obtained, according to chromatography
Absorption peak position and absorption peak area in figure, obtain the content of each component absorption peak and each component.
Wherein chromatographic condition is same as above.
Detection method of the invention is obtained by screening, and screening process is as follows:
1 materials and methods
1.1 material
1.2 reagent
Reference substance: D-menthone, Panaxynol, matrine, Atisine chloride Atractydin, arctiin, oleanolic acid, Hederagenin
Member, Ligustilide, ferulic acid, timosaponin, matrine, ammonium glycyrrhetate, linamarin standard items, are purchased from Chinese food drug
Examine and determine research institute.Each standard items purity is all larger than 98.0%.Sample: anti-ginseng itching-relieving granule lot number is respectively 20180201,
20180202、20180203、20180301、20180302、20180303、20180304、20180503、20180504、
20180505, it is provided by Liaoning Kangchen Pharmaceutical Co., Ltd..
1.3 reagent
1.4 method
1.4.1 chromatographic condition
Chromatographic column Agilent-ZORBAX Eclipse Plus C18；Mobile phase: 0.01% formic acid water (A)-acetonitrile (B),
Gradient elution program see the table below 2-1；2 μ L of sample volume；Flow velocity 0.3mL/min；Detection wavelength 0~30min, 220nm；30~
35.5min 254nm；35.5~45.0min, 330nm；35 DEG C of column temperature.
Table 2-1 eluent gradient elution requirement
1.4.2 the preparation of reference substance solution
Take hederagenin, oleanolic acid, linamarin, matrine, Atisine chloride Atractydin, Ligustilide, rehmannioside, ginseng alkynes
Alcohol, arctiin, D-menthone, ammonium glycyrrhetate, timosaponin, ferulic acid each 10mg, it is accurately weighed, it is placed in 10mL volumetric flask
In, add methanol to be configured to reference substance stock solution.
It takes each reference substance stock solution that 50mL volumetric flask constant volume is added in right amount to groove, mixes, obtaining concentration is respectively (ivy
36.28 μ g/mL of sapogenin, 23.60 μ g/mL of oleanolic acid, 38.51 μ g/mL of linamarin, 62.45 μ g/mL of matrine, glutinous rehmannia
55.26 μ g/mL of glucoside, 43.10 μ g/mL of Panaxynol, 30.25 μ g/mL of arctiin, 20.73 μ g/mL of D-menthone, glycyrrhizic acid
85.33 μ g/mL of ammonium, 58.39 μ g/mL of timosaponin, 71.42 μ g/mL of ferulic acid, 42.55 μ g/mL of Atisine chloride Atractydin, Ligustilide
53.74 μ g/mL) mixed reference substance solution.
1.4.3 the preparation of test solution
Anti- ginseng itching-relieving granule is taken, crushes, takes about 0.5g, it is accurately weighed, it sets in 25mL volumetric flask, proper amount of methanol is added, it is close
Plug is ultrasonically treated (power 300W, frequency 40kHz) 10min, lets cool, be settled to groove, shake up, 1mL is taken to add 50% methanol 1:1
Dilution, mix, 14000rpm be centrifuged 10min, take supernatant to get.
2 test results
2.1 extraction conditions are investigated
This experiment has investigated hederagenin, olive in terms of extraction time, extraction solid-liquid ratio, Extraction solvent three
Acid, linamarin, matrine, rehmannioside, sennoside, arctiin, D-menthone, ammonium glycyrrhetate, timosaponin, ferulic acid,
The influence factor of the extraction efficiencies such as Atisine chloride Atractydin, Ligustilide.It the results are shown in Table 2-2.
Table 2-2 extraction conditions are investigated
Note: " * " represents solid-liquid ratio
Each constituent concentration is suitable when the result shows that solid-liquid ratio being 1:50, separating degree is good, and saves solvent；Extraction time is
30min, each constituents extraction rate is with respect to highest when with methanol as solvent.Therefore, selective extraction condition are as follows: take anti-ginseng itching-relieving granule powder
Last 0.5g is in 25mL volumetric flask, addition proper amount of methanol, close plug, ultrasonic 30min, and taking-up lets cool, with methanol constant volume to groove, shakes
It is even, 1mL is taken, is diluted with 50% methanol 1:1, whirlpool is even, 14000rpm, is centrifuged 10min.
2.2 linear relationships are investigated
By mixed reference substance solution under " 1.4.2 ", takes 2 μ L to inject liquid chromatograph, calculate separately same retention time
Under peak area, using concentration x as abscissa, using peak area y as ordinate draw standard curve.Calculate the recurrence of standard curve
Equation and related coefficient.The result shows that: each reference substance linear relationship in respective concentration range is good, and linear relationship is shown in Table 2-
3。
The equation of linear regression and the range of linearity of each index components of table 2-3
2.5 precision test
2.5.1 withinday precision is tested
Precision draws same test solution, and 2 μ L of sample introduction is repeated sample introduction 6 times, measures content, calculates its RSD.As a result table
Bright: withinday precision RSD value range illustrates that the method precision is good, the results are shown in Table 2-4 0.28~0.96%.
Table 2-4 withinday precision test result (n=6)
2.5.2 day to day precision is tested
Precision draws same test solution, and 2 μ L of sample introduction is repeated sample introduction 6 times, and METHOD FOR CONTINUOUS DETERMINATION three days, preparation was a daily
Test solution measures the content of each ingredient, calculates its RSD.The result shows that: day to day precision RSD value is 0.13~0.59%,
Illustrate that the method precision is good, the results are shown in Table 2-5.
Table 2-5 day to day precision test result (n=3) (mg/g)
2.6 repetitive test
Parallel precision weighs 6 parts of anti-ginseng itching-relieving granule powder, prepares anti-antipruritic of ginseng according to " 1.4.3 " lower section methods respectively
6 parts of test solution of grain, the test solution handled well is analyzed, and is measured the content of each quantitative ingredient, is calculated its RSD
Value, investigates the reproducibility of this method.The result shows that each component content RSD value range shows this method 0.72~2.55%
Reproducibility is good, the results are shown in Table 2-6.
The repetitive test result (mg/g) of the anti-ginseng itching-relieving granule index components content measurement of table 2-6
2.7 stability test
Precision draws same test solution, saves at room temperature, respectively at the time interval of 0,2,4,6,8,12h, essence
2 μ L of close absorption inject liquid chromatograph, measure peak area, calculate RSD, investigate anti-ginseng itching-relieving granule under room temperature experiment condition
Whether stability is good.The result shows that: RSD value range shows that anti-ginseng itching-relieving granule tests item in room temperature 0.19~1.07%
Part stability inferior is good, the results are shown in Table 2-7.
Table 2-7 stability test result (mg/g)
Methodological study by system show this method in a few days, day to day precision, repeatability and have good stability, accord with
The requirement for closing related methodology, can be used for the assay of sample.Separately sampled product solution and standard solution are measured into HPLC,
Chromatogram is as shown in Figure 1 and Figure 2.
The anti-ginseng itching-relieving granule sample size measurement result of table 2-8 (mg/ piece)
Detailed description of the invention:
The anti-ginseng itching-relieving granule sample solution chromatogram of Fig. 1
Fig. 2 mixed reference substance solution chromatogram
In attached drawing, (1, hederagenin；2, oleanolic acid；3, linamarin；4, matrine；5, rehmannioside；6, ginseng
Alkynol；7, arctiin；8, D-menthone；9, ammonium glycyrrhetate；10, timosaponin；11, ferulic acid；12, Atisine chloride Atractydin；13, rhizoma ligustici
Lactone)
Specific embodiment:
Embodiment 1
1, the preparation of reference substance solution
Take hederagenin, oleanolic acid, linamarin, matrine, Atisine chloride Atractydin, Ligustilide, rehmannioside, ginseng alkynes
Alcohol, arctiin, D-menthone, ammonium glycyrrhetate, timosaponin, ferulic acid each 10mg, it is accurately weighed, it is placed in 10mL volumetric flask
In, add methanol to be configured to reference substance stock solution；It takes each reference substance stock solution that 50mL volumetric flask constant volume is added in right amount to groove, mixes
It is even, obtain concentration be respectively as follows: 36.28 μ g/mL of hederagenin, 23.60 μ g/mL of oleanolic acid, 38.51 μ g/mL of linamarin,
62.45 μ g/mL of matrine, 55.26 μ g/mL of rehmannioside, 43.10 μ g/mL of Panaxynol, 30.25 μ g/mL of arctiin, dextrorotation are thin
20.73 μ g/mL of lotus ketone, 85.33 μ g/mL of ammonium glycyrrhetate, 58.39 μ g/mL of timosaponin, 71.42 μ g/mL of ferulic acid, Atisine chloride Atractydin
The mixed reference substance solution of 42.55 μ g/mL, 53.74 μ g/mL of Ligustilide；
2, the preparation of test solution
Anti- ginseng itching-relieving granule is taken, crushes, takes 0.5g, it is accurately weighed, it sets in 25mL volumetric flask, addition proper amount of methanol, close plug,
It is ultrasonically treated (power 300W, frequency 40kHz) 10min, lets cool, is settled to groove, shake up, take 1mL, add 50% methanol of 1ml molten
Liquid dilution, mixes, and 14000rpm is centrifuged 10min, supernatant, that is, test solution；
3, it detects
Reference substance solution and 2 μ L of test solution are injected separately into high performance liquid chromatograph, chromatogram is obtained, according to chromatography
Absorption peak position and absorption peak area in figure, obtain the content of each component absorption peak and each component.
Embodiment 2
1, the preparation of reference substance solution
Take hederagenin, oleanolic acid, linamarin, matrine, Atisine chloride Atractydin, Ligustilide, rehmannioside, ginseng alkynes
Alcohol, arctiin, D-menthone, ammonium glycyrrhetate, timosaponin, ferulic acid each 8mg, it is accurately weighed, it is placed in 10mL volumetric flask,
Methanol is added to be configured to reference substance stock solution；It takes each reference substance stock solution that 50mL volumetric flask constant volume is added in right amount to groove, mixes, obtain
Concentration be respectively as follows: 36 μ g/mL of hederagenin, 23 μ g/mL of oleanolic acid, 38 μ g/mL of linamarin, 62 μ g/mL of matrine,
55 μ g/mL of rehmannioside, 43 μ g/mL of Panaxynol, 30 μ g/mL of arctiin, 20 μ g/mL of D-menthone, 85 μ g/ of ammonium glycyrrhetate
ML, 58 μ g/mL of timosaponin, 71 μ g/mL of ferulic acid, 42 μ g/mL of Atisine chloride Atractydin, the mixing reference substance of 53 μ g/mL of Ligustilide are molten
Liquid；
2, the preparation of test solution
Anti- ginseng itching-relieving granule is taken, crushes, takes 0.4g, it is accurately weighed, it sets in 20mL volumetric flask, addition proper amount of methanol, close plug,
It is ultrasonically treated (power 300W, frequency 40kHz) 5min, lets cool, is settled to groove, shake up, take 2mL, add 40% methanol of 1ml molten
Liquid dilution, mixes, and 14000rpm is centrifuged 5min, supernatant, that is, test solution；
3, it detects
Reference substance solution and 3 μ L of test solution are injected separately into high performance liquid chromatograph, chromatogram is obtained, according to chromatography
Absorption peak position and absorption peak area in figure, obtain the content of each component absorption peak and each component.
Embodiment 3
1, the preparation of reference substance solution
Take hederagenin, oleanolic acid, linamarin, matrine, Atisine chloride Atractydin, Ligustilide, rehmannioside, ginseng alkynes
Alcohol, arctiin, D-menthone, ammonium glycyrrhetate, timosaponin, ferulic acid each 12mg, it is accurately weighed, it is placed in 10mL volumetric flask
In, add methanol to be configured to reference substance stock solution；It takes each reference substance stock solution that 50mL volumetric flask constant volume is added in right amount to groove, mixes
It is even, it obtains concentration and is respectively as follows: 37 μ g/mL of hederagenin, 24 μ g/mL of oleanolic acid, 39 μ g/mL of linamarin, 63 μ of matrine
G/mL, 56 μ g/mL of rehmannioside, 44 μ g/mL of Panaxynol, 31 μ g/mL of arctiin, 21 μ g/mL of D-menthone, ammonium glycyrrhetate 86
The mixing reference substance of μ g/mL, 59 μ g/mL of timosaponin, 72 μ g/mL of ferulic acid, 43 μ g/mL of Atisine chloride Atractydin, 54 μ g/mL of Ligustilide
Solution；
2, the preparation of test solution
Anti- ginseng itching-relieving granule is taken, crushes, takes 0.6g, it is accurately weighed, it sets in 30mL volumetric flask, addition proper amount of methanol, close plug,
It is ultrasonically treated (power 300W, frequency 40kHz) 15min, lets cool, is settled to groove, shake up, take 1mL, add 60% methanol of 1ml molten
Liquid dilution, mixes, and 14000rpm is centrifuged 15min, supernatant, that is, test solution；
3, it detects
Reference substance solution and 1 μ L of test solution are injected separately into high performance liquid chromatograph, chromatogram is obtained, according to chromatography
Absorption peak position and absorption peak area in figure, obtain the content of each component absorption peak and each component.
Claims (3)
1. a kind of detection method of the anti-ginseng itching-relieving granule of Chinese patent drug, which is characterized in that the described method comprises the following steps:
Step 1, the preparation of reference substance solution
Take hederagenin, oleanolic acid, linamarin, matrine, Atisine chloride Atractydin, Ligustilide, rehmannioside, Panaxynol,
Arctiin, D-menthone, ammonium glycyrrhetate, timosaponin, ferulic acid add methanol to be configured to reference substance stock solution；By each reference substance
Stock solution is mixed to get reference substance mixed solution；
Step 2, the preparation of test solution
Anti- ginseng itching-relieving granule is taken, is extracted with methanol, the test solution after being extracted；
Step 3, it detects
Reference substance mixed solution and test solution are injected separately into high performance liquid chromatograph, chromatogram is obtained, according to chromatogram
In absorption peak position and absorb peak area, by the content that each component absorption peak and each component is calculated；
Wherein the chromatographic condition of high performance liquid chromatography is as follows:
C18 chromatographic column；
Mobile phase: 0.01% formic acid water (A)-acetonitrile (B),
Using gradient elution, elution program is as follows:
2 μ L of sample volume；
Flow velocity 0.3mL/min；
Detection wavelength 0~30min, 220nm；30~35.5min, 254nm；35.5~45.0min, 330nm；
35 DEG C of column temperature.
2. detection method according to claim 1, which is characterized in that the described method comprises the following steps:
Step 1, the preparation of reference substance solution
Take hederagenin, oleanolic acid, linamarin, matrine, Atisine chloride Atractydin, Ligustilide, rehmannioside, Panaxynol,
Arctiin, D-menthone, ammonium glycyrrhetate, timosaponin, ferulic acid each 8-12mg, it is accurately weighed, it is placed in 8-12mL volumetric flask
In, add methanol to be configured to reference substance stock solution；Each reference substance stock solution is taken 45-55mL volumetric flask constant volume to be added in right amount to groove,
It mixes, obtains concentration and be respectively as follows: hederagenin 36-37 μ g/mL, oleanolic acid 23-24 μ g/mL, linamarin 38-39 μ g/
ML, matrine 62-63 μ g/mL, rehmannioside 55-56 μ g/mL, Panaxynol 43-44 μ g/mL, arctiin 30-31 μ g/mL, dextrorotation
Menthones 20-21 μ g/mL, ammonium glycyrrhetate 85-86 μ g/mL, timosaponin 58-59 μ g/mL, ferulic acid 71-72 μ g/mL, rhizoma atractylodis
The mixed reference substance solution of plain 42-43 μ g/mL, Ligustilide 53-54 μ g/mL；
Step 2, the preparation of test solution
Anti- ginseng itching-relieving granule is taken, is crushed, is taken 0.4-0.6g, set in 20-30mL volumetric flask, methanol is added, is ultrasonically treated 5-
15min is settled to groove, takes out 1-2mL, adds the methanol solution dilution such as 40-60%, is centrifuged 5-15min, and supernatant is to supply
Test sample solution；
Step 3, it detects
Reference substance solution and test solution 1-3 μ L are injected separately into high performance liquid chromatograph, chromatogram is obtained, according to chromatogram
In absorption peak position and absorb peak area, the content of each component absorption peak and each component is calculated.
3. detection method according to claim 1, which is characterized in that the described method comprises the following steps:
Step 1, the preparation of reference substance solution
Take hederagenin, oleanolic acid, linamarin, matrine, Atisine chloride Atractydin, Ligustilide, rehmannioside, Panaxynol,
Arctiin, D-menthone, ammonium glycyrrhetate, timosaponin, ferulic acid each 10mg, it is accurately weighed, it is placed in 10mL volumetric flask, adds
Methanol is configured to reference substance stock solution；It takes each reference substance stock solution that 50mL volumetric flask constant volume is added in right amount to groove, mixes, obtain dense
Degree is respectively as follows: 36.28 μ g/mL of hederagenin, 23.60 μ g/mL of oleanolic acid, 38.51 μ g/mL of linamarin, matrine
62.45 μ g/mL, 55.26 μ g/mL of rehmannioside, 43.10 μ g/mL of Panaxynol, 30.25 μ g/mL of arctiin, D-menthone
20.73 μ g/mL, 85.33 μ g/mL of ammonium glycyrrhetate, 58.39 μ g/mL of timosaponin, 71.42 μ g/mL of ferulic acid, Atisine chloride Atractydin 42.55
The mixed reference substance solution of μ g/mL, 53.74 μ g/mL of Ligustilide；
Step 2, the preparation of test solution
Anti- ginseng itching-relieving granule is taken, crushes, takes 0.5g, it is accurately weighed, it sets in 25mL volumetric flask, proper amount of methanol, close plug, ultrasound is added
(power 300W, frequency 40kHz) 10min is handled, lets cool, is settled to groove, shake up, take 1mL, add 50% methanol solution of 1ml dilute
It releases, mixes, 14000rpm is centrifuged 10min, supernatant, that is, test solution；
Step 3, it detects
Reference substance solution and 2 μ L of test solution are injected separately into high performance liquid chromatograph, chromatogram is obtained, according in chromatogram
Absorption peak position and absorb peak area, obtain the content of each component absorption peak and each component.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811380501.1A CN109298097B (en) | 2018-11-20 | 2018-11-20 | Detection method of Chinese patent medicine ginseng-prevention and itching-relieving granules |
Applications Claiming Priority (1)
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| CN111103385A (en) * | 2019-12-27 | 2020-05-05 | 辽宁康辰药业有限公司 | Fingerprint spectrum determination method of ginseng-prevention and itching-relieving granules |
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