CN108896695A - The discrimination method of corter pseudolaricis in a kind of Chinese medicine compound prescription - Google Patents
The discrimination method of corter pseudolaricis in a kind of Chinese medicine compound prescription Download PDFInfo
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- CN108896695A CN108896695A CN201810729005.6A CN201810729005A CN108896695A CN 108896695 A CN108896695 A CN 108896695A CN 201810729005 A CN201810729005 A CN 201810729005A CN 108896695 A CN108896695 A CN 108896695A
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- G—PHYSICS
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Abstract
The invention discloses a kind of discrimination methods of corter pseudolaricis in Chinese medicine compound prescription, include the following steps：(1) sample is added on polyamide column, is first eluted with mixed solution, then eluted with organic solvent A, collected eluent, be evaporated, residue is dissolved with organic solvent A, as test solution；(2) corter pseudolaricis control medicinal material is taken, organic solvent B is added to handle, filtrate is evaporated, and residue is dissolved with organic solvent B, as control medicinal material solution；(3) test solution and each 2~6 μ L of control medicinal material solution are taken, point sample using the mixed solution of cyclohexane-ethyl acetate as solvent, is unfolded on same silica gel thin-layer chromatography plate, takes out, dry, be placed under 365nm ultraviolet lamp and inspect respectively.Discrimination method of the present invention can effectively clear impurity in test sample, principal component loss simultaneously is smaller, it obtains test solution chromatogram clear spot easily to distinguish, and avoids the reagent being more toxic using benzene etc., have many advantages, such as specificity strong, favorable reproducibility, high sensitivity and environmentally protective.
Description
Technical field
The invention belongs to Chinese medicine detection technique fields, and in particular to the discrimination method of corter pseudolaricis in a kind of Chinese medicine compound prescription.
Background technique
Pseudolarice tincture compound is compound Chinese medicinal preparation, record in《Drug Standard of Ministry of Public Health of the Peoples Republic of China》Chinese medicine at
Square preparation the 17th, standard No. is：WS3-B-3269-98 has effects that sterilizing and itch-relieving, itch for toe, skin taste itch,
General psoriasis.Its prescription is made of corter pseudolaricis 42g, benzoic acid 125g, tri- taste of salicylic acid 62.5g, preparation method：Above three taste, takes soil
Rose of Sharon skin is added ethanol in proper amount, is heated to reflux 5 hours, filters；Benzoic acid, salicylic acid are dissolved with ethyl alcohol, closed with corter pseudolaricis filtrate
And add ethyl alcohol be made 1000ml to get.
The technical solution of thin layer identification is in pseudolarice tincture compound quality standard：Take this product 2ml as test solution.Separately
Corter pseudolaricis control medicinal material 2g is taken, ethyl alcohol 50ml is added, is heated to reflux 5 hours, flow liquid 2ml is fetched, as control medicinal material solution.According to thin
Layer chromatography (annex VI B) test, draws each 10 μ l of above two solution, puts respectively and be with sodium carboxymethylcellulose in same
On the silica gel g thin-layer plate of adhesive, forward position is first expanded to ether, takes out, dries, then with methanol-strong ammonia solution (4:It 1) is exhibition
Agent is opened, is unfolded, takes out, dries, sprays with 10% ethanol solution of sulfuric acid, is dried 15 minutes at 110 DEG C.In sample chromatogram, with
On the corresponding position of reference substance chromatography, the spot of same color is shown.(compound Golden Larch Bark matches quality standard research to Sun Hongying etc., existing
Generation apply pharmacy, 1995,8:18-20.) it is to the thin layer authentication technique scheme of chaste tree acetic acid native in corter pseudolaricis tincture：Take compound soil chaste tree
Skin tincture 20ml, volatilizes, and residue is dissolved in right amount with benzene.Benzene liquid is filtered to obtain, benzene is flung to, residue is dissolved in three times with ether 20ml,
Ether dissolution part is set in separatory funnel, is extracted in three times with 5% soda solution 30ml, after gained extract liquor merges, adds salt
Volume white precipitate is precipitated at acidity in acid acidification, and filtrate continues to be acidified to white precipitate to be precipitated completely, merges sediment, uses water
It washes, drains, ether liquid is dissolved to obtain with anhydrous ether, fling to ether, residue methanol 1ml dissolves, as test solution.Take native chaste tree
Skin acetic acid reference substance adds the methanol 1ml solution containing 1mg that makes into 1ml.Reference substance soil chaste tree acetic acid, each 20 μ l of test solution are taken, point
In being put on the same silica gel H lamellae using sodium carboxymethylcellulose as adhesive after point sample, chromatography cylinder is interior to be saturated 30 points to other point
It is unfolded after clock.After waving most solvent, spray with anisaldehyde-concentrated sulfuric acid solution.In 105 DEG C of baking about 10min.Observation colour developing spot, for examination
In product chromatography, at the position corresponding to the chromatogram of the reference substance, the spot of same color is shown.
Thin-layer identification method in pseudolarice tincture compound quality standard tests to pseudolarice tincture compound, examination table
It is bright, in same batch sample chromatogram and reference medicine chromatography corresponding position, it is speckless or spot is unintelligible, influence result and sentence
Fixed or erroneous judgement product quality is unqualified.Tracing it to its cause is：1. complex chemical composition does not do purification processes in test solution, directly
Test solution point sample is taken, detection ingredient is interfered；2. solvent polarity is larger, thin layer spot and R f mistake after expansion is caused
Greatly, spot is easy overlapping to solvent front, fails to reach and efficiently separates, and influences result judgement；3. spot is inspected as universal visualization
Daylight is inspected after the colour developing of agent sulfuric acid ethyl alcohol, because ethanol solution of sulfuric acid is sprayed on lamellae, can all show same to institute's organic chemical composition
Different classes of organic chemical composition cannot be distinguished in a kind of color, and specificity is poor, influences the judgement of identification result.And Sun Hongying
Et al. discrimination method in test solution pre-treatment step it is cumbersome, and toxic reagent benzene need to be used, be highly detrimental to experimenter
Health and environmental protection.
Summary of the invention
Based on this, provided it is an object of the invention to overcome in place of above-mentioned the deficiencies in the prior art in a kind of Chinese medicine compound prescription
The discrimination method of corter pseudolaricis there is chromatogram clear spot easily to distinguish, is simple and convenient, the high and safe nothing of high sensitivity, identification efficiency
The advantages that pollution.
To achieve the above object, the technical solution adopted by the present invention is：The discrimination method of corter pseudolaricis in a kind of Chinese medicine compound prescription,
Include the following steps：
(1) preparation of test solution：Sample to be identified is added on polyamide column, first with ether-acetic acid butyl ester
Mixed solution elution, then eluted with organic solvent A, eluent is collected, is evaporated, residue is dissolved with organic solvent A, as test sample
Solution；
(2) preparation of control medicinal material solution：Corter pseudolaricis control medicinal material powder is taken, organic solvent B is added to be heated to reflux, filtrate is steamed
Dry, residue is dissolved with organic solvent B, as control medicinal material solution；
(3) indentification by TLC：Test solution and each 2~6 μ L of control medicinal material solution are taken, point sample is in same silica gel respectively
On chromatographic sheet, using the mixed solution of cyclohexane-ethyl acetate as solvent, it is unfolded, takes out, dry, is placed in 365nm purple
It is inspected under outer smooth lamp；In test solution chromatography, on position corresponding with control medicinal material solution chromatography, the glimmering of same color is shown
Hot spot point.
Preferably, in the mixed solution of ether-acetic acid butyl ester described in the step (1) ether and butyl acetate volume
Than for (10~12):1.Preferably, organic solvent A is selected from least one of methanol and ethyl alcohol in the step (1).
Preferably, the volume fraction of the methanol or ethyl alcohol is 80%~100%.
Preferably, organic solvent B is selected from least one of methanol and ethyl alcohol in the step (2).
Preferably, the volume fraction of the methanol or ethyl alcohol is 80%~100%.Preferably, in the step (2) added with
The time that solvent B is heated to reflux is 5h.
Preferably, silica gel thin-layer chromatography plate is selected from silica gel H from making sheet or silica gel H prefabricated board in the step (3).
Preferably, the volume of the mixed solution cyclohexane of step (3) cyclohexane-ethyl acetate and ethyl acetate
Than for (2.3~4)：1.
Preferably, organic solvent A and the volume ratio of sample to be identified are (6~20) in the step (1):1；The step
(2) corter pseudolaricis control medicinal material and the w/v of organic solvent B are 1g in：(15~200) mL.
Compared with the existing technology, beneficial effects of the present invention are：(1) present invention is using column chromatography technology to test solution
Pre-treatment is carried out, purifies impurity elimination, and eluted using the ether-acetic acid butyl ester mixing eluent of special ratios, effectively clear
Except principal component loss is smaller while impurity in test sample, obtains test solution chromatogram clear spot and easily distinguish；(2) of the invention
In the thin-layer developing condition of discrimination method, agents useful for same is the lesser solvent of toxicity, is conducive to operator's health and environment
Protection；Grope through test, obtains selecting the mixed solution of cyclohexane-ethyl acetate as solvent, and hexamethylene and acetic acid second
The volume ratio of ester is (2.3~4)：When 1, it can make that target component spot efficiently separates and spot and R f value is moderate；Serviceability test card
The bright method of deploying good tolerance；(3) spot, which is inspected, uses the stronger ultraviolet lamp of specificity instead and inspects, and avoids using in primary standard
General sulfuric acid ethyl alcohol color developing agent can effectively reduce influence of the impurity spot to result.
Detailed description of the invention
Fig. 1 is discrimination method specificity experimental result of the present invention, wherein 1：Pseudolarice tincture compound E10026 batches；2：Compound
Corter pseudolaricis tincture E10027 batches；3：Pseudolarice tincture compound D12128 batches；4：Pseudolarice tincture compound E10029 batches；5：Pseudolarice tincture compound
E11030 batches；6：Pseudolarice tincture compound G01001 batches；7：Pseudolarice tincture compound G02003 batches；8：Pseudolarice tincture compound G03006
Batch；9：Pseudolarice tincture compound G03007 batches；10：Pseudolarice tincture compound G05008 batches；11：Corter pseudolaricis control medicinal material；12：It is negative right
According to product.
Fig. 2 is the effect of corter pseudolaricis discrimination method in corter pseudolaricis discrimination method and existing Chinese medicine compound in Chinese medicine compound prescription of the present invention
Fruit contrast and experiment, wherein 1：Pseudolarice tincture compound G02003 batches；2：Corter pseudolaricis control medicinal material.
Specific embodiment
To better illustrate the object, technical solutions and advantages of the present invention, below in conjunction with specific embodiment to the present invention
It is described further.
Following material may be selected in test material used in the present invention, but following material is not limited to when actual implementation：
Reagent：The production of silica gel H (lot number 150308) Haiyang Chemical Plant, Qingdao, makes 10 × 20mm of plate gauge lattice, thickness by oneself
0.5mm；Prefabricated board is Haiyang Chemical Plant, Qingdao's production, 10 × 20mm of specification, 0.2~0.25mm of thickness.Other agents useful for same are
It analyzes pure.
Control medicinal material：Corter pseudolaricis control medicinal material (lot number 121281-201002) is purchased from Chinese food drug assay research
Institute.
Test sample：Pseudolarice tincture compound 10 batches (lot number E10026, E10027, D12128, E10029, E11030,
G01001, G02003, G03006, G03007, G05008), it is produced for Community in Baiyunshan, Guangzhou Jing Xiutang medicine company limited liability company.
Embodiment 1
A kind of embodiment of the discrimination method of corter pseudolaricis in Chinese medicine compound prescription of the present invention, to corter pseudolaricis in pseudolarice tincture compound into
Row identifies, and includes the following steps：
(1) preparation of test solution：
Take pseudolarice tincture compound (lot number E10026, E10027, D12128) 5ml to be added on polyamide column, first with ether and
Butyl acetate volume ratio is 12:1 ether-acetic acid butyl ester mixed solution elution, discards eluent, then be with 30ml volume fraction
80% ethanol solution elution, collects eluent, is evaporated, and the residue ethanol solution that 1ml volume fraction is 80% dissolves, as
Test solution；
(2) preparation of control medicinal material solution：
Corter pseudolaricis control medicinal material powder 1g is taken, adding 30ml volume fraction is that 80% ethanol solution is heated to reflux 5 hours, is filtered
Liquid is evaporated, and the residue ethanol solution that 1ml volume fraction is 80% dissolves, as control medicinal material solution；
(3) test sample is identified using tlc identification method：
Test solution and each 2 μ L of control medicinal material solution are taken, distinguishes point sample in same silica gel H from making sheet, with hexamethylene
It is 4 with ethyl acetate volume ratio:The mixed solution of 1 cyclohexane-ethyl acetate will be unfolded as solvent, ascending development
Complete lamellae takes out, and dries, is placed under 365nm ultraviolet lamp and inspects；In test solution chromatography, with control medicinal material solution
On the corresponding position of chromatography, the fluorescence spot of same color is shown, illustrates that test sample is qualified product.
Embodiment 2
A kind of embodiment of the discrimination method of corter pseudolaricis in Chinese medicine compound prescription of the present invention, to corter pseudolaricis in pseudolarice tincture compound into
Row identifies, and includes the following steps：
(1) preparation of test solution：
Take pseudolarice tincture compound (lot number E10029, E11030, G01001) 5ml to be added on polyamide column, first with ether and
Butyl acetate volume ratio is 11:1 ether-acetic acid butyl ester mixed solution elution, discards eluent, then be with 50ml volume fraction
90% ethanol solution elution, collects eluent, is evaporated, and the residue ethanol solution that 1ml volume fraction is 90% dissolves, as
Test solution；
(2) preparation of control medicinal material solution：
Control medicinal material powder 1g is taken, adding 50ml volume fraction is that 90% ethanol solution is heated to reflux 5 hours, and filtrate is steamed
Dry, the residue ethanol solution that 1ml volume fraction is 90% dissolves, as control medicinal material solution；
(3) test sample is identified using tlc identification method：
Take test solution and each 3 μ L of control medicinal material solution, point sample is on same silica gel H prefabricated board respectively, with hexamethylene
It is 7 with ethyl acetate volume ratio:The mixed solution of 2 cyclohexane-ethyl acetate will be unfolded as solvent, ascending development
Complete lamellae takes out, and dries, is placed under 365nm ultraviolet lamp and inspects；In test solution chromatography, with control medicinal material solution
On the corresponding position of chromatography, the fluorescence spot of same color is shown, illustrates that test sample is qualified product.
Embodiment 3
A kind of embodiment of the discrimination method of corter pseudolaricis in Chinese medicine compound prescription of the present invention, to corter pseudolaricis in pseudolarice tincture compound into
Row identifies, and includes the following steps：
(1) preparation of test solution：
Take pseudolarice tincture compound (lot number G02003, G03006, G03007) 5ml to be added on polyamide column, first with ether and
Butyl acetate volume ratio is 10:1 ether-acetic acid butyl ester mixed solution elution, discards eluent, then with 100ml dehydrated alcohol
Elution is collected eluent, is evaporated, and residue 1ml dehydrated alcohol dissolves, as test solution；
(2) preparation of control medicinal material solution：
Control medicinal material powder 1g is taken, adds 100ml dehydrated alcohol to be heated to reflux 5 hours, filtrate is evaporated, and residue is anhydrous with 1ml
Ethyl alcohol dissolution, as control medicinal material solution；
(3) test sample is identified using tlc identification method：
Take test solution and each 5 μ L of control medicinal material solution, point sample is on same silica gel H prefabricated board respectively, with hexamethylene
It is 8 with ethyl acetate volume ratio:The mixed solution of 3 cyclohexane-ethyl acetate will be unfolded as solvent, ascending development
Complete lamellae takes out, and dries, is placed under 365nm ultraviolet lamp and inspects；In test solution chromatography, with control medicinal material solution
On the corresponding position of chromatography, the fluorescence spot of same color is shown, illustrates that test sample is qualified product.
Embodiment 4
A kind of embodiment of the discrimination method of corter pseudolaricis in Chinese medicine compound prescription of the present invention, to corter pseudolaricis in pseudolarice tincture compound into
Row identifies, and includes the following steps：
(1) preparation of test solution：
Take pseudolarice tincture compound (lot number G02003, G03006, G03007) 5ml to be added on polyamide column, first with ether and
Butyl acetate volume ratio is 10:1 ether-acetic acid butyl ester mixed solution elution, discards eluent, then washed with 30ml anhydrous methanol
It is de-, eluent is collected, is evaporated, residue 1ml anhydrous methanol dissolves, as test solution；
(2) preparation of control medicinal material solution：
Control medicinal material powder 1g is taken, 30ml anhydrous methanol is added to be heated to reflux 5 hours, filtrate is evaporated, and residue is with 1ml without water beetle
Alcohol dissolution, as control medicinal material solution；
(3) test sample is identified using tlc identification method：
Take test solution and each 6 μ L of control medicinal material solution, point sample is on same silica gel H prefabricated board respectively, with hexamethylene
It is 7 with ethyl acetate volume ratio:The mixed solution of 3 cyclohexane-ethyl acetate will be unfolded as solvent, ascending development
Complete lamellae takes out, and dries, is placed under 365nm ultraviolet lamp and inspects；In test solution chromatography, with control medicinal material solution
On the corresponding position of chromatography, the fluorescence spot of same color is shown, illustrates that test sample is qualified product.
Embodiment 5
A kind of embodiment of the discrimination method of corter pseudolaricis in Chinese medicine compound prescription of the present invention, to corter pseudolaricis in pseudolarice tincture compound into
Row identifies, and includes the following steps：
(1) preparation of test solution：
Take pseudolarice tincture compound (lot number G03006, G03007, G05008) 5ml to be added on polyamide column, first with ether and
Butyl acetate volume ratio is 12:1 ether-acetic acid butyl ester mixed solution elution, discards eluent, then with 100ml volume fraction
It is eluted for 90% methanol solution, collects eluent, be evaporated, the residue methanol solution that 1ml volume fraction is 90% dissolves, and makees
For test solution；
(2) preparation of control medicinal material solution：
Control medicinal material powder 1g is taken, adding 100ml volume fraction is that 90% methanol solution is heated to reflux 5 hours, and filtrate is steamed
Dry, the residue methanol solution that 1ml volume fraction is 90% dissolves, as control medicinal material solution；
(3) test sample is identified using tlc identification method：
Test solution and each 5 μ L of control medicinal material solution are taken, distinguishes point sample in same silica gel H from making sheet, with hexamethylene
It is 7 with ethyl acetate volume ratio:The mixed solution of 3 cyclohexane-ethyl acetate will be unfolded as solvent, ascending development
Complete lamellae takes out, and dries, is placed under 365nm ultraviolet lamp and inspects；In test solution chromatography, with control medicinal material solution
On the corresponding position of chromatography, the fluorescence spot of same color is shown, illustrates that test sample is qualified product.
Embodiment 6
A kind of embodiment of the discrimination method of corter pseudolaricis in Chinese medicine compound prescription of the present invention, to corter pseudolaricis in pseudolarice tincture compound into
Row identifies, and includes the following steps：
(1) preparation of test solution：
Take pseudolarice tincture compound (lot number G02003, G03006, G03007) 5ml to be added on polyamide column, first with ether and
Butyl acetate volume ratio is 10:1 ether-acetic acid butyl ester mixed solution elution, discards eluent, then be with 50ml volume fraction
80% methanol solution elution, collects eluent, is evaporated, and the residue methanol solution that 1ml volume fraction is 80% dissolves, as
Test solution；
(2) preparation of control medicinal material solution：
Control medicinal material powder 1g is taken, adding 50ml volume fraction is that 80% methanol solution is heated to reflux 5 hours, and filtrate is steamed
Dry, the residue methanol solution that 1ml volume fraction is 80% dissolves, as control medicinal material solution；
(3) test sample is identified using tlc identification method：
Take test solution and each 5 μ L of control medicinal material solution, point sample is on same silica gel H prefabricated board respectively, with hexamethylene
It is 8 with ethyl acetate volume ratio:The mixed solution of 3 cyclohexane-ethyl acetate will be unfolded as solvent, ascending development
Complete lamellae takes out, and dries, is placed under 365nm ultraviolet lamp and inspects；In test solution chromatography, with control medicinal material solution
On the corresponding position of chromatography, the fluorescence spot of same color is shown, illustrates that test sample is qualified product.
The specificity of the discrimination method of the present invention of embodiment 7
The present embodiment verifies the specificity of discrimination method of the present invention.
(1) preparation of test solution：
Take pseudolarice tincture compound 10 batches (lot number E10026, E10027, D12128, E10029, E11030, G01001,
G02003, G03006, G03007, G05008) 5ml is added on polyamide column, and it is first 12 with ether and butyl acetate volume ratio:1
The elution of ether-acetic acid butyl ester mixed solution, discard eluent, then use 50ml anhydrous ethanol elution, collection eluent is evaporated,
Residue 1ml dehydrated alcohol dissolves, as test solution；
(2) preparation of control medicinal material solution：
Control medicinal material powder 1g is taken, 50ml dehydrated alcohol is added to be heated to reflux 5 hours, filtrate is evaporated, the residue anhydrous second of 1ml
Alcohol dissolution, as control medicinal material solution；
(3) preparation of negative test solution：
Benzoic acid 125g and salicylic acid 62.5g are taken, according to the preparation method of pseudolarice tincture compound, it is right that the feminine gender without corter pseudolaricis is made
According to product, then according to the preparation method of test solution, the negative test solution without corter pseudolaricis is made；
(4) test sample is identified using tlc identification method：
Test solution, control medicinal material solution and each 5 μ L of negative test solution are taken, point sample is pre- in same silica gel H respectively
In making sheet, with hexamethylene and ethyl acetate volume ratio for 7:The mixed solution of 3 cyclohexane-ethyl acetate as solvent, on
Row expansion, the lamellae that expansion is finished take out, dry, be placed under 365nm ultraviolet lamp and inspect.
Chromatography recognition result is as shown in Figure 1, the results showed that, in sample chromatogram, with control medicinal material corter pseudolaricis chromatography phase
On the position answered, the fluorescence spot of same color is shown, illustrates that test sample is qualified product；In negative sample chromatogram, with compare
Sphragidite rose of Sharon color of the leather is composed on corresponding position, and the fluorescence spot of not aobvious same color illustrates that negative controls are noiseless.Above-mentioned knot
Fruit shows that thin-layer identification method specificity of the present invention is stronger.
The durability of the discrimination method of the present invention of embodiment 8
The present embodiment verifies the durability of discrimination method of the present invention.
1, the comparison of different lamellaes：Hand paving H-CMC.Na and prefabricated silica gel H plate are chosen, respectively by the test method drafted
Test.It is required the result shows that can reach identification from making sheet and prefabricated board.
2, the comparison of different relative humidity：Lamellae after taking point sample, adjusting humidity with sulfuric acid respectively is 32% and 72%
Chromatography cylinder in be unfolded, inspect.The result shows that the environment of relative humidity 32% and 72% has no significant effect chromatography.
3, the comparison of different temperatures：The chromatography cylinder of existing solvent is placed in refrigerator (4 DEG C), after placing a period of time,
Lamellae after point sample is put into chromatography cylinder, is unfolded, inspects.The result shows that the thin layer clear spot under cryogenic conditions, separation
Degree is preferably, similar to the thin-layer developing situation of room temperature, shows that low temperature has no significant effect the thin-layer identification method.
It is above-mentioned experiments have shown that, the thin-layer identification method of pseudolarice tincture compound of the invention in terms of lamellae, hand bed board and
Prefabricated board can reach separating effect；Temperature, humidity variation are little to expansion influential effect.Therefore this method good tolerance,
Meet《<Chinese Pharmacopoeia>Quality standards in Chinese drugs studies and defines technical requirements》In the regulation in relation to durability.
Comparative example 1
This comparative example studies the difference on effect of corter pseudolaricis discrimination method and existing discrimination method in Chinese medicine compound prescription of the present invention.
(1) experimental method
1, corter pseudolaricis discrimination method in Chinese medicine compound prescription of the present invention
(1) preparation of test solution：
It takes pseudolarice tincture compound (lot number G02003) 5ml to be added on polyamide column, first uses ether and butyl acetate volume ratio
It is 10:1 ether-acetic acid butyl ester mixed solution elution, discards eluent, then use 50ml anhydrous ethanol elution, collection eluent,
It is evaporated, residue 1ml dehydrated alcohol dissolves, as test solution；
(2) preparation of control medicinal material solution：
Control medicinal material powder 1g is taken, 50ml dehydrated alcohol is added to be heated to reflux 5 hours, filtrate is evaporated, the residue anhydrous second of 1ml
Alcohol dissolution, as control medicinal material solution；
(3) test sample is identified using tlc identification method：
Take test solution and each 5 μ L of control medicinal material solution, point sample is on same silica gel H prefabricated board respectively, with hexamethylene
It is 8 with ethyl acetate volume ratio:The mixed solution of 3 cyclohexane-ethyl acetate will be unfolded as solvent, ascending development
Complete lamellae takes out, and dries, is placed under 365nm ultraviolet lamp and inspects.
Chromatography identification：In sample chromatogram, on position corresponding with control medicinal material corter pseudolaricis chromatography, same color is shown
Fluorescence spot illustrates that test sample is qualified product.
2, the existing discrimination method of corter pseudolaricis in Chinese medicine compound prescription
(1) preparation of test solution：
Take pseudolarice tincture compound (lot number G02003) 2ml as test solution；
(2) preparation of control medicinal material solution：
Corter pseudolaricis control medicinal material 2g is taken, 50ml dehydrated alcohol is added, is heated to reflux 5 hours, flow liquid 2ml is fetched, as control
Medicinal material solution；
(3) test sample is identified using tlc identification method：
Test solution and each 10 μ L of control medicinal material solution are taken, point sample first uses ether on same silica G prefabricated board respectively
Ascending development takes out, dries, again with methanol and dense ammonia volume ratio are 4 to forward position：1 methanol-strong ammonia solution ascending development, exhibition
It opens, takes out, dry；Spray is dried 15 minutes at 110 DEG C with 10% ethanol solution of sulfuric acid.
Chromatography identification：In sample chromatogram, on position corresponding with control medicinal material corter pseudolaricis chromatography, same color is shown
Spot illustrates that test sample is qualified product.
(2) experimental result
Experimental result is as shown in Figure 2, the results showed that, pseudolarice tincture compound discrimination method authentication technique specificity of the present invention,
The indexs such as sensitivity and separating effect are superior to the prior art.
Finally, it should be noted that the above embodiments are merely illustrative of the technical solutions of the present invention rather than protects to the present invention
The limitation of range is protected, although the invention is described in detail with reference to the preferred embodiments, those skilled in the art should
Understand, it can be with modification or equivalent replacement of the technical solution of the present invention are made, without departing from the essence of technical solution of the present invention
And range.
Claims (10)
1. the discrimination method of corter pseudolaricis in a kind of Chinese medicine compound prescription, which is characterized in that include the following steps：
(1) preparation of test solution：Sample to be identified is added on polyamide column, the mixing of ether-acetic acid butyl ester is first used
Solution elution, then eluted with organic solvent A, eluent is collected, is evaporated, residue is dissolved with organic solvent A, molten as test sample
Liquid；
(2) preparation of control medicinal material solution：Corter pseudolaricis control medicinal material powder is taken, organic solvent B is added to be heated to reflux, filtrate is evaporated,
Residue is dissolved with organic solvent B, as control medicinal material solution；
(3) indentification by TLC：Test solution and each 2~6 μ L of control medicinal material solution are taken, point sample is in same silica gel thin-layer respectively
On chromatosheet, using the mixed solution of cyclohexane-ethyl acetate as solvent, it is unfolded, takes out, dry, be placed in 365nm ultraviolet light
It is inspected under lamp；In test solution chromatography, on position corresponding with control medicinal material solution chromatography, the fluorescent spot of same color is shown
Point.
2. the discrimination method of corter pseudolaricis in Chinese medicine compound prescription according to claim 1, which is characterized in that in the step (1)
The volume ratio of ether and butyl acetate is (10~12) in the mixed solution of the ether-acetic acid butyl ester:1.
3. the discrimination method of corter pseudolaricis in Chinese medicine compound prescription according to claim 1, which is characterized in that in the step (1)
Organic solvent A is selected from least one of methanol and ethyl alcohol.
4. the discrimination method of corter pseudolaricis in Chinese medicine compound prescription according to claim 3, which is characterized in that the methanol or ethyl alcohol
Volume fraction be 80%~100%.
5. the discrimination method of corter pseudolaricis in Chinese medicine compound prescription according to claim 1, which is characterized in that in the step (2)
Organic solvent B is selected from least one of methanol and ethyl alcohol.
6. the discrimination method of corter pseudolaricis in Chinese medicine compound prescription according to claim 5, which is characterized in that the methanol or ethyl alcohol
Volume fraction be 80%~100%.
7. the discrimination method of corter pseudolaricis in Chinese medicine compound prescription according to claim 1, which is characterized in that in the step (2)
The time for adding organic solvent B to be heated to reflux is 5h.
8. the discrimination method of corter pseudolaricis in Chinese medicine compound prescription according to claim 1, which is characterized in that in the step (3)
Silica gel thin-layer chromatography plate is selected from silica gel H from making sheet or silica gel H prefabricated board.
9. the discrimination method of corter pseudolaricis in Chinese medicine compound prescription according to claim 1, which is characterized in that in the step (3)
The mixed solution cyclohexane of cyclohexane-ethyl acetate and the volume ratio of ethyl acetate are (2.3~4)：1.
10. the discrimination method of corter pseudolaricis in Chinese medicine compound prescription according to claim 1, which is characterized in that in the step (1)
Organic solvent A and the volume ratio of sample to be identified are (6~20):1；In the step (2) corter pseudolaricis control medicinal material with it is organic molten
The w/v of agent B is 1g：(15~200) mL.
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