CN110361496A - The detection method of scutelloside in a kind of Chinese materia medica preparation Jinsangsanjie ball - Google Patents

The detection method of scutelloside in a kind of Chinese materia medica preparation Jinsangsanjie ball Download PDF

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Publication number
CN110361496A
CN110361496A CN201910705387.3A CN201910705387A CN110361496A CN 110361496 A CN110361496 A CN 110361496A CN 201910705387 A CN201910705387 A CN 201910705387A CN 110361496 A CN110361496 A CN 110361496A
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China
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solution
scutelloside
reference substance
materia medica
jinsangsanjie
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石丽
耿小秀
田广科
田芝娟
王岗
李卉
李燕
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BEILIN PHARMACEUTICAL Co Ltd XI'AN
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BEILIN PHARMACEUTICAL Co Ltd XI'AN
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    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/90Plate chromatography, e.g. thin layer or paper chromatography

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Abstract

The detection method of scutelloside in Chinese materia medica preparation Jinsangsanjie ball provided in an embodiment of the present invention, in the preparation process of test solution, utilize 70% alcohol reflux, extract more detection ingredients, sour water solution is carried out to the solution containing scutelloside, separate sugared body and aglycon in scutelloside structure, as free state, improve the content of aglycon in the solution, and then improve the accuracy of detection, addition petroleum ether, which can preferably clean, eliminates map background, further improves the accuracy of detection.The silica G plate prepared using 4% sodium acetate solution to guarantee that active principle to be detected is fixed on lamellae, and then can guarantee the accuracy of testing result effectively by test solution and control solution sample-adding on lamellae.

Description

The detection method of scutelloside in a kind of Chinese materia medica preparation Jinsangsanjie ball
Technical field
The invention belongs to traditional Chinese medicine quality detection technique fields, and in particular to scutelloside in a kind of Chinese materia medica preparation Jinsangsanjie ball Detection method.
Background technique
Scutelloside is a kind of flavone compound, has significant bioactivity, has antibacterial, diuresis, anti-inflammatory, resistance state And spasmolysis, and there are the physiological potencies such as stronger antitumor response, it has been occupied an important position in clinical medicine.Scutelloside is made For the detection project in drug examination criteria, determine whether of crucial importance containing scutelloside in Jinsangsanjie ball.
Existing detection method is to take this product candidate drug 10g, finely ground, adds methanol 40ml, is ultrasonically treated 20 minutes, filter It crosses, filtrate is evaporated, and residue adds water 20ml to make to dissolve, and adjusts pH value to 2 with dilute hydrochloric acid, shakes extraction 2 times with ethyl acetate, every time 20ml, combined ethyl acetate extracting solution, is evaporated, and residue adds methanol 1ml to make to dissolve, as test solution.Separately take scutelloside pair According to product, add methanol that solution of every 1ml containing 1mg is made, as reference substance solution.According to thin-layered chromatography (Chinese Pharmacopoeia version in 2015 Four general rules 0502) test, each 10 μ l of above two solution is drawn, is put respectively on same silica gel g thin-layer plate, with acetic acid second Ester-butanone-formic acid-water (5:3:1:1) is solvent, is unfolded, and takes out, dries, and is sprayed with 1% ferric trichloride ethanol solution.For examination In product chromatography, at the position corresponding to the chromatogram of the reference substance, the spot of same color is shown.
But it is unobvious using the test sample spot that existing detection method detects, it influences quality inspection personnel and accurately judges, And then influence the quality of product.
Summary of the invention
In order to become apparent from the detection spot of test sample, to improve the inspection to scutelloside in Chinese materia medica preparation Jinsangsanjie ball Accuracy rate is surveyed, the present invention provides a kind of detection methods of scutelloside in Chinese materia medica preparation Jinsangsanjie ball.The invention solves Technical problem is achieved through the following technical solutions:
The embodiment of the invention provides a kind of detection methods of scutelloside in Chinese materia medica preparation Jinsangsanjie ball, including following step It is rapid:
Chinese materia medica preparation 10g to be detected and finely ground is taken, Chinese materia medica preparation powder to be detected is obtained;
70% ethyl alcohol 40ml is added in the Chinese materia medica preparation powder to be detected, is heated to reflux 1 hour, will be heated to reflux Liquid filtration afterwards, the filtrate after filtration is evaporated, extraction of substance to be processed is obtained;
Add water 20ml in the extraction of substance to be processed, obtains solution to be processed;
20ml petroleum ether is added in the solution to be processed, after impurity is extracted in shaking, removes petroleum ether liquid, repeats to shake Extraction step 1 time, solution after being extracted, wherein the petroleum ether boiling range is 60~90 DEG C;
To repeatedly shaking is extracted, merging mentions every time after solution progress pH value adjustment after the extraction plus ethyl acetate solution After ethyl acetate solution, purification dissolution after taking, test solution is made;
Using scutelloside powder as reference substance, and reference substance solution is made in the reference substance;
The test solution of isodose and the reference substance solution are put respectively on same silica gel g thin-layer plate;
Using ethyl acetate-butanone-formic acid-water as solvent, the silica gel g thin-layer plate is unfolded, is taken out, dries place Reason, obtains silica gel g thin-layer plate to be inspected;
It is sprayed on silica gel g thin-layer plate with ferric trichloride ethanol solution, so that the silica G to be inspected is thin described wait inspect The spot of the test sample and the spot of the reference substance are shown on laminate;
The spot of the test sample and the spot of the reference substance are compared, determines the Chinese materia medica preparation Jinsangsanjie to be detected Whether contain scutelloside in ball.
In a specific embodiment, the silica gel g thin-layer plate is thin with the silica G of 4% sodium acetate solution preparation Laminate.
In a specific embodiment, described that pH value adjustment plus ethyl acetate solution are carried out to solution after the extraction Repeatedly shaking extracts, merges the ethyl acetate solution after extracting every time, after purification dissolution, test solution, including step is made afterwards It is rapid:
The pH value of solution after the extraction is adjusted to 2, solution after being adjusted;
20ml ethyl acetate solution is added in solution after adjustment section, shaking is extracted, and is collected after extracting for the first time Ethyl acetate solution repeats shaking extraction step 2 times, collects acetic acid ethyl fluid and third time after extracting respectively second and mentions Acetic acid ethyl fluid after taking;
The acetic acid ethyl fluid after acetic acid ethyl fluid, second of extraction after the first time is extracted, the third Acetic acid ethyl fluid after secondary extraction merges, and obtains extracting solution;
After the extraction solution is evaporated, purifying substances are obtained, the dissolution of 1ml methanol is added in the purifying substances, obtains To test solution.
In a specific embodiment, the pH value by solution after the extraction is adjusted to 2, comprising steps of
Detect the pH value of solution after the extraction;
Hydrochloric acid is added in solution after the extraction, until the pH value of solution is 2 after the extraction, stops that hydrochloric acid is added.
In a specific embodiment, described using scutelloside as reference substance, and reference substance is made in the reference substance Solution, comprising steps of
Take scutelloside powder as reference substance;
Methanol is added in the reference substance, the reference substance solution that the reference substance content is 1mg/ml is made.
In a specific embodiment, described to distinguish the test solution of isodose and the reference substance solution Point is on same silica gel g thin-layer plate, comprising:
The reference substance solution of the test solution of 10 μ l and 10 μ l are put respectively on same silica gel g thin-layer plate In.
In a specific embodiment, in the solvent, ethyl acetate-butanone-formic acid-water volume ratio is 5 ﹕, 3 ﹕ 1 ﹕ 1.
In a specific embodiment, the concentration of ferric trichloride is 5% in the ferric trichloride ethanol solution.
In a specific embodiment, the spot of the spot for comparing the test sample and the reference substance, determines In the Chinese materia medica preparation Jinsangsanjie ball to be detected whether containing scutelloside include:
Judge at the same position of the spot of the reference substance, the test sample whether there is and the reference substance spot The spot of same color, and if it exists, then determine to contain scutelloside in the Chinese materia medica preparation Jinsangsanjie ball to be detected;
If it does not exist, then determine not contain scutelloside in the Chinese materia medica preparation Jinsangsanjie ball to be detected.
The detection method of scutelloside in Chinese materia medica preparation Jinsangsanjie ball provided in an embodiment of the present invention, with prior art phase Than having the following advantages that and effect:
1, in the preparation process of test solution of the present invention, using 70% alcohol reflux, more detection ingredients are extracted, it is right Solution containing scutelloside carries out sour water solution, separates sugared body and aglycon in scutelloside structure, becomes free state, mention The high content of aglycon in the solution, and then improve the accuracy of detection is added petroleum ether and can preferably clean and eliminates map Background further improves the accuracy of detection.
2, the silica G plate that lamellae uses 4% sodium acetate solution to prepare in the present invention, can be effectively by test solution With reference substance solution sample-adding on lamellae, to guarantee that active principle to be detected is fixed on lamellae, and then guarantee detection As a result accuracy.
Detailed description of the invention
Fig. 1 is the result figure detected using the prior art to scutelloside in Chinese materia medica preparation Jinsangsanjie ball;
Fig. 2 is using scutelloside detection method in Chinese materia medica preparation Jinsangsanjie ball provided by the invention to Chinese materia medica preparation gold throat The testing result figure that scutelloside is detected in Sanjie Pill;
Fig. 3 is for another kind using scutelloside detection method in Chinese materia medica preparation Jinsangsanjie ball provided by the invention to Chinese medicine system The testing result figure that scutelloside is detected in agent Jinsangsanjie ball.
Specific embodiment
Further detailed description is done to the present invention combined with specific embodiments below, but embodiments of the present invention are not limited to This.
Embodiment 1
In order to become apparent from the detection spot of test sample, to improve the inspection to scutelloside in Chinese materia medica preparation Jinsangsanjie ball Accuracy rate is surveyed, the present invention provides a kind of detection methods of scutelloside in Chinese materia medica preparation Jinsangsanjie ball, specifically include following step It is rapid:
S1, Chinese materia medica preparation 10g to be detected and finely ground is taken, obtains Chinese materia medica preparation powder to be detected.
Chinese materia medica preparation to be detected is Jinsangsanjie ball.Accurately weighed Chinese materia medica preparation 10g to be detected is simultaneously finely ground, obtains to be detected Powder to be detected is placed in conical flask by Chinese materia medica preparation powder, can be realized in the following way: meeting drug examination criteria Under the premise of, using conventional mortar, Chinese materia medica preparation 10g to be detected is ground, is finely ground, powder is made.
S2, the ethyl alcohol 40ml that 70% is added in the Chinese materia medica preparation powder to be detected, are heated to reflux 1 hour, will heat Liquid filtration after reflux, the filtrate after filtration is evaporated, extraction of substance to be processed is obtained.
S3, add water 20ml in the extraction of substance to be processed, obtain solution to be processed.
S4,20ml petroleum ether is added in the solution to be processed, after impurity is extracted in shaking, removes petroleum ether liquid, repeats Shaking extraction step 1 time, solution after being extracted, wherein the petroleum ether boiling range is 60~90 DEG C.
Specifically, it is as follows to repeat to shake extraction step 1 time implementation: 20ml stone being added in the solution to be processed After solution impurity is extracted in shaking, after removing petroleum ether, 20ml is added in removing the solution to be processed after petroleum ether again in oily ether Petroleum ether after solution impurity is extracted in shaking, removes petroleum ether, the solution after being extracted.
S5, solution after the extraction is carried out after pH value adjustment plus ethyl acetate solution repeatedly shaking extract, merge it is each After ethyl acetate solution, purification dissolution after extraction, test solution is made.
S6, using scutelloside powder as reference substance, and reference substance solution is made in the reference substance.
In step s 6, above-mentioned scutelloside can be scutelloside powder, can be by above-mentioned scutelloside powder system in the step At solution as reference substance solution, which can be directly obtained.
S7, the test solution of isodose and the reference substance solution are put respectively on same silica gel g thin-layer plate.
Above-mentioned steps S7, it is possible to reduce using error brought by multiple silica gel g thin-layer plates, improve and scutelloside is detected Accuracy.
S8, with ethyl acetate-butanone-formic acid-water (5:3:1:1) be solvent, the silica gel g thin-layer plate is opened up It opens, take out, drying processing, obtaining silica gel g thin-layer plate to be inspected.
S9, it is sprayed on silica gel g thin-layer plate with ferric trichloride ethanol solution, so that the silica gel to be inspected described wait inspect The spot of the test sample and the spot of the reference substance are shown on G lamellae.
Specifically, the concentration of ferric trichloride is 5% in above-mentioned ferric trichloride ethanol solution.
The spot of S10, the spot for comparing the test sample and the reference substance, determine the Chinese materia medica preparation gold throat to be detected Whether contain scutelloside in Sanjie Pill.
The detection method of scutelloside in Chinese materia medica preparation provided in an embodiment of the present invention, in the preparation process of test solution In, using 70% alcohol reflux, more detection ingredients are extracted, sour water solution is carried out to the solution containing scutelloside, makes scutelloside Sugared body and aglycon in structure separate, and become free state, improve the content of aglycon in the solution, and then improve detection Accuracy, petroleum ether, which is added, can preferably clean and eliminates map background, further improve the accuracy of detection.Institute It states and sprays wait inspect on silica gel g thin-layer plate with 5% ferric trichloride ethanol solution, spot development is clear, greatly increases the inspection of thin layer spot Effect out identifies convenient for observation, has ensured the accuracy of identification result;Above-mentioned detection method is simple, easy to operate, eliminates original The uncertainty that scutelloside identifies is that one kind can more comprehensively, accurately identify scutelloside in Chinese materia medica preparation Jinsangsanjie ball Discrimination method, above-mentioned revised discrimination method meet drug examination criteria, improve the quality control of drug;Above-mentioned detection side Method, using thin-layered chromatography, condition is reasonable, and method is feasible, and specificity is strong, and reproducibility, durability are preferable.
Optionally, the silica gel g thin-layer plate can be the silica gel g thin-layer plate prepared with 4% sodium acetate solution.
The silica gel g thin-layer plate prepared using 4% sodium acetate solution, can be effectively by test solution and control solution Sample-adding, using 4% sodium acetate solution as adhesive, can make active principle to be detected and reference substance solution on lamellae In active principle be loaded on silica gel g thin-layer plate, thin layer spot rounding is clear, eliminate map background interference, detect at sorting Effect is obvious out, and separating degree and repdocutbility are preferable, the final accuracy for guaranteeing testing result.
Optionally, above-mentioned steps S5 can be realized with S501-S504 according to the following steps:
S501, the pH value of solution after the extraction is adjusted to 2, solution after being adjusted.
S502,20ml ethyl acetate solution is added in solution after the adjustment, shaking is extracted, and is collected after extracting for the first time Ethyl acetate solution, repeat shaking extraction step 2 times, collect respectively second extract after acetic acid ethyl fluid and third time Acetic acid ethyl fluid after extraction.
Specifically, 20ml ethyl acetate solution can be added in solution after the adjustment, shaking is extracted, and is collected and is extracted for the first time After ethyl acetate solution afterwards, 20ml ethyl acetate solution is added in surplus solution, shaking is extracted, and is collected second after extracting Ethyl acetate solution;After having collected the ethyl acetate solution after extracting second, 20ml acetic acid is added in surplus solution Ethyl ester solution, shaking are extracted, and are collected the ethyl acetate solution after third time is extracted, are extracted three times by above-mentioned, more fully Scutelloside in solution is extracted into ethyl acetate solution, the accuracy of detection is improved.
S503, the first time is extracted after acetic acid ethyl fluid, described second extract after acetic acid ethyl fluid, described Acetic acid ethyl fluid after third time is extracted merges, and obtains extracting solution.
S504, after being evaporated the extraction solution, purifying substances are obtained, it is molten that 1ml methanol is added in the purifying substances Solution, obtains test solution.
Due to including sugared body and aglycon in the composed structure of scutelloside, the pH value of solution after the extraction is adjusted to 2, it can So that scutelloside carries out sour water solution, sugared body and aglycon in scutelloside structure are separated, becomes free state, improves glycosides The content of member in the solution.It, more fully will be in Chinese materia medica preparation Jinsangsanjie ball using the preparation method of above-mentioned test solution Scutelloside adequately extracts, in case the progress of subsequent detection work, improves detection accuracy.
Optionally, in step S501, the pH value of solution after the extraction can be adjusted to 2 in the following manner:
Detect the pH value of solution after the extraction;
Hydrochloric acid is added in solution after the extraction, until the pH value of solution is 2 after the extraction, stops that hydrochloric acid is added.
In embodiments of the present invention, the pH value of solution after the extraction can be measured in real time, specific inspection in real time When surveying pH value, the detection of PH test paper or instrument detection can be used.
Optionally, step S6 can be realized according to the following steps:
Take scutelloside powder as reference substance;
Methanol is added in the reference substance, the reference substance solution that the reference substance content is 1mg/ml is made.
Scutelloside powder is directly prepared into reference substance solution, it is comparative strong, and accuracy is high.
Optionally, step S7 can be realized according to the following steps: by the described right of the test solution of 10 μ l and 10 μ l It is put on same silica gel g thin-layer plate respectively according to product solution.
Optionally, step S10 can be realized according to the following steps:
Judge at the same position of the spot of the reference substance, the test sample whether there is and the reference substance spot The spot of same color, and if it exists, then determine to contain scutelloside in the Chinese materia medica preparation Jinsangsanjie ball to be detected;
If it does not exist, then determine not contain scutelloside in the Chinese materia medica preparation Jinsangsanjie ball to be detected.
Further, spray described wait inspect on silica gel g thin-layer plate with ferric trichloride ethanol solution, it is provided by the invention in The detection method of scutelloside does not limit temperature and humidity in medicine preparation, in the temperature of Laboratory Request and the item of humidity Under part, scutelloside can be detected using the detection method of scutelloside in Chinese materia medica preparation provided by the invention, be referred to Fig. 2, Fig. 2 detect scutelloside in Chinese materia medica preparation using scutelloside detection method in Chinese materia medica preparation provided by the invention Testing result figure, wherein label 4 is the spot of reference substance, and label 1-3 is the spot of 3 kinds of test samples, is 24 DEG C in temperature, wet Under conditions of degree is 30%, the testing result figure in left side in above-mentioned Fig. 2 is obtained, is 5 DEG C in temperature, the condition that humidity is 64% Under, obtain the testing result figure on right side in above-mentioned Fig. 2;Fig. 3 is referred to, Fig. 3 is another using Chinese medicine system provided by the invention The testing result figure that scutelloside detection method detects scutelloside in Chinese materia medica preparation in agent, wherein label 1 is reference substance Spot, label 2-5 are the spot of test sample, are 24 DEG C in temperature, under conditions of humidity is 20%, obtain left side in above-mentioned Fig. 3 Testing result figure, be 5 DEG C in temperature, under conditions of humidity is 64%, obtain in above-mentioned Fig. 3 the testing result figure on right side, figure 2, in the testing result figure that Fig. 3 is showed, the spot of test solution and the spot of reference substance solution are shown clearly, so that quality inspection Personnel can be whether there is scutelloside, to guarantee the quality of Chinese materia medica preparation Jinsangsanjie ball in accurate judgement Chinese materia medica preparation.
Embodiment 2
Existing detection means are as follows: Chinese materia medica preparation Jinsangsanjie ball 10g is taken, it is finely ground, add methanol 40ml, is ultrasonically treated 20 points Clock, filtration, filtrate are evaporated, and residue adds water 20ml to make to dissolve, and adjust pH value to 2 with dilute hydrochloric acid, extract 2 with ethyl acetate shaking Secondary, each 20ml, combined ethyl acetate extracting solution is evaporated, and residue adds methanol 1ml to make to dissolve, as test solution.Separately take Huang A kind of reed mentioned in ancient books glycosides reference substance adds methanol that solution of every 1ml containing 1mg is made, as reference substance solution.According to thin-layered chromatography (Chinese Pharmacopoeia Four general rules 0502 of version in 2015) test, each 10 μ l of above two solution is drawn, is put respectively on same silica gel g thin-layer plate, with Ethyl acetate-butanone-formic acid-water (5:3:1:1) is solvent, is unfolded, and takes out, dries, and is sprayed molten with 1% ferric trichloride ethyl alcohol Liquid.In sample chromatogram, at the position corresponding to the chromatogram of the reference substance, the spot of same color is shown.
The scutelloside in Chinese materia medica preparation Jinsangsanjie ball is detected using prior art, testing result refers to In Fig. 1, Fig. 1, what it is marked as 4 is the spot of reference substance, marked as 1-3 be three kinds of test samples spot, temperature be 16 DEG C, Humidity detects under conditions of being 48%, obtains above-mentioned testing result figure shown in FIG. 1, testing result are as follows: in sample chromatogram, With scutelloside reference substance chromatography corresponding position, test sample shows the spot of essentially identical color in chromatography, but spot is shown It is unobvious, influence the judgement of product quality;Using detection method provided by the invention to the Huang in Chinese materia medica preparation Jinsangsanjie ball A kind of reed mentioned in ancient books glycosides is detected, testing result referring to fig. 2, testing result are as follows: in sample chromatogram, corresponding to scutelloside reference substance chromatography Position show the spot of same color, spot shows obviously.The testing result of more above two scheme finds that the present invention provides Chinese materia medica preparation in the detection method detection spot detection spot compared with the existing technology of scutelloside become apparent, passing through color After the analysis verifying of spectrometer device, the detection method detection spot of scutelloside is become apparent from Chinese materia medica preparation provided by the invention, detection knot Fruit is more acurrate.
The above content is a further detailed description of the present invention in conjunction with specific preferred embodiments, and it cannot be said that Specific implementation of the invention is only limited to these instructions.For those of ordinary skill in the art to which the present invention belongs, exist Under the premise of not departing from present inventive concept, a number of simple deductions or replacements can also be made, all shall be regarded as belonging to of the invention Protection scope.

Claims (7)

1. the detection method of scutelloside in a kind of Chinese materia medica preparation Jinsangsanjie ball, which comprises the following steps:
1) test solution of Chinese materia medica preparation Jinsangsanjie ball is prepared
Obtain Chinese materia medica preparation powder to be detected;
70% ethyl alcohol 40ml is added in the Chinese materia medica preparation powder to be detected, is heated to reflux 1 hour, after being heated to reflux Liquid filtration, the filtrate after filtration is evaporated, extraction of substance to be processed is obtained;
Add water 20ml in the extraction of substance to be processed, obtains solution to be processed;
20ml petroleum ether is added in the solution to be processed, after impurity is extracted in shaking, removes petroleum ether liquid, repeats shaking and extracts Step 1 time, solution after being extracted, wherein the petroleum ether boiling range is 60~90 DEG C;
PH value adjustment is carried out to solution after the extraction, after adding after ethyl acetate solution repeatedly shaking to extract, merging and extract every time Ethyl acetate solution, purification dissolution after, test solution is made, comprising steps of
The pH value of solution after the extraction is adjusted to 2, detects the pH value of solution after the extraction;
Hydrochloric acid is added in solution after the extraction, until the pH value of solution is 2 after the extraction, stops that hydrochloric acid is added, obtains Solution after adjusting;
20ml ethyl acetate solution is added in solution after the adjusting, shaking is extracted, and the acetic acid second after extracting for the first time is collected Ester solution repeats shaking extraction step 2 times, after the acetic acid ethyl fluid and third time after collecting second of extraction respectively extract Acetic acid ethyl fluid;
The acetic acid ethyl fluid after acetic acid ethyl fluid, second of extraction after the first time is extracted, the third time mention Acetic acid ethyl fluid after taking merges, and obtains extracting solution;
After the extraction solution is evaporated, purifying substances are obtained, the dissolution of 1ml methanol is added in the purifying substances, is supplied Test sample solution.
2) reference substance solution is prepared;
Using scutelloside powder as reference substance, and reference substance solution is made in the reference substance;
3) it is tested according to thin-layered chromatography (four general rules 0502 of Chinese Pharmacopoeia version in 2015), draws test solution and reference substance is molten Liquid is put respectively on same silica gel g thin-layer plate;
Using ethyl acetate-butanone-formic acid-water as solvent, the silica gel g thin-layer plate is unfolded, is taken out, dries processing, Obtain silica gel g thin-layer plate to be inspected;
It is sprayed on silica gel g thin-layer plate with ferric trichloride ethanol solution, so that the silica gel g thin-layer plate to be inspected described wait inspect The spot of the upper display test sample and the spot of the reference substance;
The spot of the test sample and the spot of the reference substance are compared, is determined in the Chinese materia medica preparation Jinsangsanjie ball to be detected Whether scutelloside is contained.
2. the detection method of scutelloside in Chinese materia medica preparation Jinsangsanjie ball according to claim 1, which is characterized in that described Silica gel g thin-layer plate is the silica gel g thin-layer plate prepared with 4% sodium acetate solution.
3. the detection method of scutelloside in Chinese materia medica preparation Jinsangsanjie ball according to claim 1, which is characterized in that described Using scutelloside as reference substance, and reference substance solution is made in the reference substance, comprising steps of
Take scutelloside powder as reference substance;
Methanol is added in the reference substance, the reference substance solution that the reference substance content is 1mg/ml is made.
4. the detection method of scutelloside in Chinese materia medica preparation Jinsangsanjie ball according to claim 1, which is characterized in that described The test solution of isodose and the reference substance solution are put respectively on same silica gel g thin-layer plate, comprising:
The reference substance solution of the test solution of 10 μ l and 10 μ l are put respectively on same silica gel g thin-layer plate.
5. the detection method of scutelloside in Chinese materia medica preparation Jinsangsanjie ball according to claim 1, which is characterized in that described In solvent, ethyl acetate-butanone-formic acid-water volume ratio is 5 ﹕, 3 ﹕, 1 ﹕ 1.
6. the detection method of scutelloside in Chinese materia medica preparation Jinsangsanjie ball according to claim 1, which is characterized in that described The concentration of ferric trichloride is 5% in ferric trichloride ethanol solution.
7. the detection method of scutelloside in Chinese materia medica preparation Jinsangsanjie ball according to claim 1, which is characterized in that described Compare the spot of the test sample and the spot of the reference substance, determine in the Chinese materia medica preparation Jinsangsanjie ball to be detected whether Contain scutelloside, comprising:
Judge at the same position of the spot of the reference substance, the test sample is with the presence or absence of identical as the reference substance spot The spot of color, and if it exists, then determine to contain scutelloside in the Chinese materia medica preparation Jinsangsanjie ball to be detected;
If it does not exist, then determine not contain scutelloside in the Chinese materia medica preparation Jinsangsanjie ball to be detected.
CN201910705387.3A 2019-08-01 2019-08-01 The detection method of scutelloside in a kind of Chinese materia medica preparation Jinsangsanjie ball Pending CN110361496A (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1785294A (en) * 2005-11-16 2006-06-14 贵阳德昌祥药业有限公司 Quality control method of eucommia bark blood pressure lowering preparation for treating high blood pressure
CN101024060A (en) * 2006-02-19 2007-08-29 刘洁 Jinsangsanjie preparation and preparing method
CN101301383A (en) * 2008-07-08 2008-11-12 邯郸制药有限公司 Quality control method of formulation for clearing wind-heat of children
CN103308644A (en) * 2013-07-03 2013-09-18 广西邦琪药业集团有限公司 Quality detection method for miscarriage-preventing leonurus preparation
WO2017176708A1 (en) * 2016-04-05 2017-10-12 Arvinas, Inc. Protein-protein interaction inducing technology

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1785294A (en) * 2005-11-16 2006-06-14 贵阳德昌祥药业有限公司 Quality control method of eucommia bark blood pressure lowering preparation for treating high blood pressure
CN101024060A (en) * 2006-02-19 2007-08-29 刘洁 Jinsangsanjie preparation and preparing method
CN101301383A (en) * 2008-07-08 2008-11-12 邯郸制药有限公司 Quality control method of formulation for clearing wind-heat of children
CN103308644A (en) * 2013-07-03 2013-09-18 广西邦琪药业集团有限公司 Quality detection method for miscarriage-preventing leonurus preparation
WO2017176708A1 (en) * 2016-04-05 2017-10-12 Arvinas, Inc. Protein-protein interaction inducing technology

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
T AKAO 等: "Baicalin, the predominant flavone glucuronide of scutellariae radix, is absorbed from the rat gastrointestinal tract as the aglycone and restored to its original form", 《J PHARM PHARMACOL》 *
张冬梅: "清热润肺合剂质量标准的研究", 《辽宁中医杂志》 *
隆颖等: "八宝惊风散质量标准研究", 《中国当代医药》 *

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