CN109298125A - A kind of thin-layered chromatography detection method of tonifying speen and tonifying kidney liquid medicine - Google Patents
A kind of thin-layered chromatography detection method of tonifying speen and tonifying kidney liquid medicine Download PDFInfo
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- CN109298125A CN109298125A CN201811413527.1A CN201811413527A CN109298125A CN 109298125 A CN109298125 A CN 109298125A CN 201811413527 A CN201811413527 A CN 201811413527A CN 109298125 A CN109298125 A CN 109298125A
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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Abstract
The invention discloses a kind of thin-layered chromatography detection methods of tonifying speen and tonifying kidney liquid medicine, and tonifying speen and tonifying kidney liquid medicine includes following component: dried orange peel, radix aucklandiae, prepared fleece flower root, fructus lycii, fingered citron, Radix Astragali；To the thin-layered chromatography detection method of dried orange peel, comprising the following steps: 1) prepared by test solution；2) prepared by reference substance solution；3) prepared by control medicinal material solution；4) test solution, control medicinal material solution, reference substance solution difference point sample, using acetate-methanol-water as solvent, are taken out in same silica gel plate, it dries, then using toluene-ethyl acetate-formic acid-water upper solution as solvent, takes out, it dries, is inspected under ultraviolet light；5) sample chromatogram is compared with the spot on reference medicine chromatography, reference substance chromatography corresponding position.It is an advantage of the invention that using thin-layered chromatography detection method of the present invention, identifies in tonifying speen and tonifying kidney liquid medicine whether contain dried orange peel ingredient, improve the quality standard of tonifying speen and tonifying kidney liquid medicine.
Description
Technical field
The present invention relates to Chinese patent drug thin-layered chromatography detection method fields, more particularly to a kind of thin layer of tonifying speen and tonifying kidney liquid medicine
Chromatographic detection method.
Background technique
Tonifying speen and tonifying kidney liquid medicine, Yishen Jianpi, relaxing tendons and activating collaterals, strong waist are healthy and strong, benefiting qi and nourishing blood.For waist caused by speen-kidney dificiency
Ridge is ached, and two knees are powerless, the diseases such as spiritlessness and weakness.Tonifying speen and tonifying kidney liquid medicine by Radix Astragali, rhizoma polygonati, Radix Angelicae Sinensis, Radix Codonopsis, prepared fleece flower root, Cortex Eucommiae,
The Chinese medicinal compositions such as fructus lycii, Herba Cistanches, Semen Cuscutae, gentianae macrophyllae, cortex cinnamomi, dog kidney processed, radix aucklandiae, dried orange peel, fingered citron, Caulis Spatholobi, Radix Glycyrrhizae are
Traditional health care liquid medicine.The medicines liver-kidney tonifying such as Cortex Eucommiae, cortex cinnamomi, fructus lycii, Semen Cuscutae, prepared fleece flower root, strong muscles and bones in side；Meat desert
Rong, dog kidney tonifying kidney and strengthening yang processed, benefiting essence-blood, to control the diseases such as weak kidney yang, lumbago due to the kidney deficiency, muscles and bones inability, waist knee flaccidity；Rhizoma polygonati, party
The tonifying middle-Jiao and Qis such as ginseng, radix aucklandiae, dried orange peel, fingered citron, Radix Astragali, strengthening spleen and tonifying lung, promoting the circulation of qi invigorating the spleen, to control spleen and lung weakness, shortness of breath and palpitation.The Qin
The medicines wind-expelling pain-stopping such as Macrophylla, Caulis Spatholobi, Radix Angelicae Sinensis, replenishing and activating blood, to control rheumatic arthralgia, muscle arteries and veins contraction, skeletal pain；Radix Glycyrrhizae tonifying spleen benefit
Gas, relieving spasm to stop pain, coordinating the drug actions of a prescription.All the medicines compatibility, Yishen Jianpi, relaxing tendons and activating collaterals, strong waist are healthy and strong, benefiting qi and nourishing blood, for controlling
Ache of the spinal column caused by speen-kidney dificiency is treated, two knees are powerless, the diseases such as spiritlessness and weakness.
But in national standard, only has amount of alcohol detection to its quality standard, there is no the testing requirements of other compositions, Wu Fajian
The effective component in tonifying speen and tonifying kidney liquid medicine is surveyed, not can guarantee its quality of production.
Summary of the invention
Goal of the invention: in view of the above-mentioned problems, the object of the present invention is to provide a kind of inspections of the thin-layer chromatography of tonifying speen and tonifying kidney liquid medicine
Survey method, to solve the technical issues of can not detecting the effective component in tonifying speen and tonifying kidney liquid medicine.
Technical solution:
A kind of thin-layered chromatography detection method of tonifying speen and tonifying kidney liquid medicine, tonifying speen and tonifying kidney liquid medicine includes following component: dried orange peel, wood
Perfume, prepared fleece flower root, fructus lycii, fingered citron, Radix Astragali；
Wherein, to the thin-layered chromatography detection method of dried orange peel, comprising the following steps:
1) prepared by test solution: taking tonifying speen and tonifying kidney liquid medicine, water-bath is evaporated to no alcohol taste, adds saturated sodium chloride solution and second
Acetoacetic ester is ultrasonically treated 2~3 times, each 20~30min of ultrasonic time, and the ethyl acetate solution after merging ultrasound is evaporated, obtains
To powder add 1~2mL methanol dissolve, be made test solution；
2) prepared by control medicinal material solution: taking dried orange peel control medicinal material, is dissolved in water, adds saturated sodium chloride solution and acetic acid second
Ester is ultrasonically treated 2~3 times, each 20~30min of ultrasonic time, and the ethyl acetate solution after merging ultrasound is evaporated, obtains
Powder adds methanol to dissolve, and control medicinal material solution is made；
3) prepared by reference substance solution: taking aurantiamarin reference substance, adds methanol that the molten of the aurantiamarin containing 0.5~1.0mg/mL is made
Liquid is to get reference substance solution；
4) by test solution, control medicinal material solution, reference substance solution difference point sample in same silica gel plate, with acetic acid second
Ester-methanol-water is solvent, and 5~7cm is unfolded, and takes out, dries, then be with toluene-ethyl acetate-formic acid-water upper solution
Solvent is expanded to 10~12cm, takes out, dries, using 1~2% (w/v) alchlor ethanol solution as color developing agent, ultraviolet
Inspected under light, wherein ethyl acetate, methanol, water volume ratio be (100~110): (17~25): (13~20), toluene,
Ethyl acetate, formic acid, water volume ratio be (20~30): (10~20): (1~2): (1~2)；
5) sample chromatogram is compared with the spot on reference medicine chromatography, reference substance chromatography corresponding position, is shown
The spot of same color contains dried orange peel ingredient as in tonifying speen and tonifying kidney liquid medicine.It, can using thin-layered chromatography detection method of the invention
Whether to identify in tonifying speen and tonifying kidney liquid medicine containing dried orange peel ingredient, the effective component in tonifying speen and tonifying kidney liquid medicine can be effectively detected, is mentioned
The high quality standard of tonifying speen and tonifying kidney liquid medicine.
In one of the embodiments, to the thin-layered chromatography detection method of radix aucklandiae, comprising the following steps:
1) prepared by test solution: taking tonifying speen and tonifying kidney liquid medicine, water-bath is evaporated to no alcohol taste, moves in separatory funnel, with two
Chloromethanes extracts 2~3 times, collects dichloromethane solution, water-bath concentration, after with methylene chloride be settled to 1mL, it is molten to obtain test sample
Liquid；
2) prepared by control medicinal material solution: radix aucklandiae control medicinal material is added into methylene chloride, 30~60min of ultrasound, is filtered,
Filtrate is concentrated into 1mL, obtains control medicinal material solution；
It 3) is exhibition with dichloromethane-cyclohexane by test solution, control medicinal material solution difference point sample in same silica gel plate
Agent is opened, is unfolded, is taken out, is dried, using vanillin-sulfuric acid test solution as color developing agent, inspect, wherein the volume of methylene chloride, hexamethylene
Than for (5~10): (1~3)；
4) sample chromatogram is compared with the spot on reference medicine chromatography corresponding position, shows the spot of same color
Point contains radix aucklandiae ingredient as in tonifying speen and tonifying kidney liquid medicine.
In one of the embodiments, to the thin-layered chromatography detection method of prepared fleece flower root, comprising the following steps:
1) prepared by test solution: taking tonifying speen and tonifying kidney liquid medicine, water-bath is evaporated to no alcohol taste, moves in separatory funnel, uses chlorine
Imitative extraction 2~3 times, merges chloroformic solution, adds anhydrous sodium sulfate, shakes, and filtering, filtrate is concentrated into 1mL, it is molten to obtain test sample
Liquid；
2) prepared by reference substance solution: taking rheum emodin, 2,3,5,4 '-tetrahydroxystilbene -2-O- β-D-Glucose glycosides pair
According to product, respectively plus the solution of 1~2mg/mL, respectively reference substance solution one, reference substance solution two is made in dehydrated alcohol；
3) test solution, reference substance solution one, reference substance solution two are distinguished into point sample in same silica gel plate, with acetic acid second
Ester-acetone-water-toluene upper solution is solvent, is unfolded, and takes out, dries, inspect under ultraviolet light, wherein acetic acid second
Ester, acetone, water, toluene volume ratio be (6.5~7.5): (5.5~7.5): (1.2~2.0): (0.7~1.5)；
4) sample chromatogram is compared with the spot on reference substance chromatography corresponding position, shows the spot of same color
Point contains prepared fleece flower root ingredient as in tonifying speen and tonifying kidney liquid medicine.
In one of the embodiments, to the thin-layered chromatography detection method of fructus lycii, comprising the following steps:
1) prepared by test solution: taking tonifying speen and tonifying kidney liquid medicine, water-bath is evaporated to no alcohol taste, moves in separatory funnel, uses vinegar
Acetoacetic ester extracts 2~3 times, merges ethyl acetate solution, and water-bath concentration, afterwards plus ethyl acetate is settled to 1mL, and it is molten to obtain test sample
Liquid；
2) prepared by control medicinal material solution: taking fructus lycii control medicinal material, the alcohol reflux that volume fraction is 60% is added to extract 30
~60min, filtering, filtrate water bath is evaporated to no alcohol taste, moves in separatory funnel, with ethyl acetate extraction 2~3 times, merges
Ethyl acetate solution, water-bath concentration, afterwards plus ethyl acetate is settled to 1mL, obtains control medicinal material solution；
3) by test solution, control medicinal material solution difference point sample in same silica gel plate, with ethyl acetate-dichloromethane-
Formic acid is solvent, be unfolded, take out, dry, inspected under ultraviolet light, wherein ethyl acetate, methylene chloride, formic acid body
Product is than being (2~4): (6~8): (1~2)；
4) sample chromatogram is compared with the spot on reference medicine chromatography corresponding position, shows the spot of same color
Point contains fructus lycii ingredient as in tonifying speen and tonifying kidney liquid medicine.
In one of the embodiments, to the thin-layered chromatography detection method of fingered citron, comprising the following steps:
1) prepared by test solution: taking tonifying speen and tonifying kidney liquid medicine, is concentrated, dehydrated alcohol is added to dissolve, filter, filtrate concentration is used
Dehydrated alcohol is settled to 1~2mL, obtains test solution；
2) prepared by control medicinal material solution: taking fingered citron control medicinal material to add in dehydrated alcohol, is ultrasonically treated 20~60min, mistake
Filter, filtrate concentration, is settled to 0.5~1.0mL with dehydrated alcohol, obtains control medicinal material solution；
It 3) is exhibition with hexamethylene-ethyl acetate by test solution, control medicinal material solution difference point sample in same silica gel plate
Open agent, be unfolded, take out, dry, inspected under ultraviolet light, wherein hexamethylene, ethyl acetate volume ratio be (3~6): (1
~2)；
4) sample chromatogram is compared with the spot on reference medicine chromatography corresponding position, shows the spot of same color
Point contains fingered citron ingredient as in tonifying speen and tonifying kidney liquid medicine.
In one of the embodiments, to the thin-layered chromatography detection method of Radix Astragali, comprising the following steps:
1) prepared by test solution: tonifying speen and tonifying kidney liquid medicine is taken, water-bath is evaporated to no alcohol taste, adds water, and flow back 1~2h, filtering,
Filter residue volatilizes, and adds methanol, and flow back 1~2h, filtering, and filter residue is dissolved in water, and the n-butanol shaking being saturated with water is extracted 2~3 times, goes
Except aqueous, n-butanol liquid is evaporated, powder adds 5~10mL of methanol to dissolve, and sets on neutral alumina column, is 40% with volume fraction
Methanol elution, collects eluent, is evaporated, and powder adds 1~1.5mL of methanol to dissolve, and obtains test solution；
2) prepared by reference substance solution: taking Astragaloside IV reference substance, the solution of 0.5~1.0mg/mL is made of methanol, obtains
Reference substance solution；
It 3) is exhibition with chloroform-methanol-water by test solution, reference substance solution difference point sample in same silica gel plate
Agent is opened, is unfolded, takes out, dries, the ethanol solution of sulfuric acid for being 10~15% using volume fraction adds at 105~108 DEG C as color developing agent
Heat is clear to spot development, wherein chloroform, methanol, water volume ratio be (13~20): (7~10): (2~3)；
4) sample chromatogram is compared with the spot on reference substance chromatography corresponding position, shows the spot of same color
Point as contains astragalus root components in tonifying speen and tonifying kidney liquid medicine.
The utility model has the advantages that compared with prior art, it is an advantage of the invention that using thin-layered chromatography detection method of the invention, it can
Whether to identify in tonifying speen and tonifying kidney liquid medicine containing dried orange peel, radix aucklandiae, prepared fleece flower root, fructus lycii, fingered citron and Radix Astragali, can effectively detect strong
Effective component in spleen and tonifying kidney liquid medicine improves the quality standard of tonifying speen and tonifying kidney liquid medicine.
Detailed description of the invention
Fig. 1 is the indentification by TLC comparison diagram of dried orange peel in embodiment 1；
Fig. 2 is the indentification by TLC comparison diagram of dried orange peel in comparative example 1；
Fig. 3 is the indentification by TLC comparison diagram of dried orange peel in comparative example 2；
Fig. 4 is the indentification by TLC comparison diagram of radix aucklandiae in embodiment 2；
Fig. 5 is the indentification by TLC comparison diagram of prepared fleece flower root in embodiment 3；
Fig. 6 is the indentification by TLC comparison diagram of fructus lycii in embodiment 4；
Fig. 7 is the indentification by TLC comparison diagram of fingered citron in embodiment 5；
Fig. 8 is the indentification by TLC comparison diagram of Radix Astragali in embodiment 6.
Specific embodiment
Raw material, equipment used in the specific embodiment of the invention are known product, are obtained by purchase commercial product.
Drug and reagent
Dried orange peel control medicinal material (National Institute for Food and Drugs Control, 120969-201310), aurantiamarin reference substance (China
Food and medicine examine and determine research institute, 110721-201317), radix aucklandiae control medicinal material (National Institute for Food and Drugs Control, 120921-
201309), rheum emodin reference substance (National Institute for Food and Drugs Control, 110756-201212), 2,3,5,4 '-tetrahydroxys two
Styrene -2-O- β-D-Glucose glycosides reference substance (National Institute for Food and Drugs Control,
110844-201311), fructus lycii control medicinal material (National Institute for Food and Drugs Control, 121072-201310),
Fingered citron control medicinal material (National Institute for Food and Drugs Control, 120933-201305), Astragaloside IV reference substance (Chinese food medicine
Research institute, 110781-201316 are determined in product examine)
Tonifying speen and tonifying kidney liquid medicine is produced by Jiangsu Zhongxing Pharmaceutical Co., Ltd., lot number is respectively 140501,140502,
140503；Negative sample presses formulation and technology self-control.
(self-control, silica G produce (for thin-layer chromatography) by Haiyang Chemical Plant, Qingdao to silica gel g thin-layer plate, and thickness 0.6mm is sticked
Mixture is 0.05% sodium carboxymethylcellulose).Other reagents are that analysis is pure.
Wherein, the prescription of tonifying speen and tonifying kidney liquid medicine are as follows:
Preparation method: above 17 taste sets Herba Cistanches, Radix Codonopsis, fructus lycii, prepared fleece flower root, dog kidney in appropriate vessel, add 50 ° it is white
Wine 240mL sealing dipping 15 days, collect leachate；The tastes medicinal powder such as remaining Radix Astragali is broken into coarse powder, with 45 ° of white wine diacolations, collects and seeps
Filter liquid 220ml；Granulated sugar 100g, honey 100g plus suitable quantity of water dissolution are separately taken, filtering is boiled.By above-mentioned leachate, percolate and sugar
Sweet liquid merges, and mixes, and white wine is added to 1000mL, stands two weeks, filtering, dispense to get.
Embodiment 1
A kind of thin-layered chromatography detection method of tonifying speen and tonifying kidney liquid medicine, including the thin-layered chromatography detection method to dried orange peel, including
Following steps:
1) prepared by test solution: taking tonifying speen and tonifying kidney liquid medicine 50mL, water-bath is evaporated to no alcohol taste, adds saturated sodium chloride solution
50mL, ethyl acetate 20mL are ultrasonically treated 2 times, each ultrasonic time 20min, and the ethyl acetate solution after merging ultrasound steams
Dry, obtained powder adds 1mL methanol to dissolve, and test solution is made；
2) prepared by control medicinal material solution: taking dried orange peel control medicinal material 2g, adds water 30mL to dissolve, add saturated sodium chloride solution
30mL, ethyl acetate 20mL are ultrasonically treated 2 times, each ultrasonic time 20min, and the ethyl acetate solution after merging ultrasound steams
Dry, obtained powder adds methanol to dissolve, and control medicinal material solution is made；
3) prepared by reference substance solution: taking aurantiamarin reference substance 2g, adds methanol that the reference substance of aurantiamarin containing 0.5mg/mL is made
Solution is to get reference substance solution；
4) prepared by negative control solution: taking the negative sample of scarce dried orange peel appropriate, feminine gender is made in the identical method with step 1)
Reference substance solution；
5) test solution, control medicinal material solution, negative controls solution are respectively taken into 5 μ L, 2 μ L of reference substance solution, respectively
Point sample in it is same with 0.5% sodium hydroxide solution prepare silica gel g thin-layer plate on, using acetate-methanol-water as solvent,
5cm is unfolded, takes out, dries, then using toluene-ethyl acetate-formic acid-water upper solution as solvent, be expanded to 10cm, take
Out, it dries, using 1% (w/v) alchlor ethanol solution as color developing agent, is inspected under ultraviolet light, wherein ethyl acetate, first
Alcohol, water volume ratio be 100:17:13, toluene, ethyl acetate, formic acid, water volume ratio be 20:10:1:1；
6) sample chromatogram is compared with the spot on reference medicine chromatography, reference substance chromatography corresponding position, is shown
The spot of same color contains dried orange peel ingredient as in tonifying speen and tonifying kidney liquid medicine.
Testing result is as shown in Figure 1, be wherein from left to right followed successively by aurantiamarin reference substance, dried orange peel control medicinal material, yin in Fig. 1
Property 140501,140502,140,503 3 parts of sample, lot number samples.As shown in Figure 1, negative sample is noiseless, and passes through this inspection
Survey method is capable of detecting when in tonifying speen and tonifying kidney liquid medicine that, containing dried orange peel ingredient, detection method is accurate.
Embodiment 2
A kind of thin-layered chromatography detection method of tonifying speen and tonifying kidney liquid medicine, including the thin-layered chromatography detection method to radix aucklandiae, including
Following steps:
1) prepared by test solution: taking tonifying speen and tonifying kidney liquid medicine 50mL, sets in evaporating dish, water-bath is evaporated to no alcohol taste, moves to
In separatory funnel, with 10mL water washing evaporating dish, repeatedly, washing lotion is incorporated in separatory funnel for washing, is extracted with dichloromethane 2 times,
The each dosage 25mL of methylene chloride, collects dichloromethane solution, water-bath concentration, after with methylene chloride be settled to 1mL, obtain for examination
Product solution；
2) prepared by control medicinal material solution: radix aucklandiae control medicinal material 1g being added into 25mL methylene chloride, ultrasonic 30min, mistake
Filter, filtrate are concentrated into 1mL, obtain control medicinal material solution；
3) negative control solution: taking the negative sample 50mL of scarce radix aucklandiae, and negative control solution is made using step 1) method；
4) each 10 μ L of test solution, control medicinal material solution, negative control solution is taken, point sample is in same with carboxymethyl respectively
Sodium cellulosate is using dichloromethane-cyclohexane as solvent, to be unfolded on the silica gel g thin-layer plate of binder, take out, dry, with perfume (or spice)
Oxalaldehyde sulfuric acid test solution be color developing agent, toast 5min at 105 DEG C, inspect, wherein methylene chloride, hexamethylene volume ratio be 5:
1；
5) sample chromatogram is compared with the spot on reference medicine chromatography corresponding position, shows the spot of same color
Point contains radix aucklandiae ingredient as in tonifying speen and tonifying kidney liquid medicine.
Thin-layer chromatography testing result as shown in figure 4, in Fig. 4, be from left to right followed successively by negative sample, lot number 140501,
140502,140503 samples, radix aucklandiae control medicinal material.As shown in Figure 4, negative sample is noiseless, and can by this detection method
Detect that, containing radix aucklandiae ingredient in tonifying speen and tonifying kidney liquid medicine, detection method is accurate.
Embodiment 3
A kind of thin-layered chromatography detection method of tonifying speen and tonifying kidney liquid medicine, including the thin-layered chromatography detection method to prepared fleece flower root,
The following steps are included:
1) prepared by test solution: taking tonifying speen and tonifying kidney liquid medicine 30mL, is placed in evaporating dish, water-bath is evaporated to no alcohol taste, moves
It into separatory funnel, with 20mL water washing evaporating dish, repeatedly washs, washing lotion is incorporated in separatory funnel, extracts 2 times with chloroform, often
Secondary chloroform dosage 5mL merges chloroformic solution, adds 1g anhydrous sodium sulfate, shakes, and filtering, filtrate is concentrated into 1mL, obtains test sample
Solution；
2) prepared by reference substance solution: taking rheum emodin, 2,3,5,4 '-tetrahydroxystilbene -2-O- β-D-Glucose glycosides pair
According to product, respectively plus the solution of 1mg/mL, respectively reference substance solution one, reference substance solution two is made in dehydrated alcohol；
3) negative control solution: taking the negative sample of scarce prepared fleece flower root, obtains negative control solution according to step 1) method；
4) take each 5 μ L of test solution, reference substance solution one, reference substance solution two, negative control solution, respectively point sample in
It is same using sodium carboxymethylcellulose as on the silica gel g thin-layer plate of binder, with ethyl acetate-acetone-water-toluene upper solution
For solvent, it is unfolded, takes out, dry, inspected at ultraviolet light (365nm), wherein ethyl acetate, acetone, water, toluene
Volume ratio is 6.5:5.5:1.2:0.7；
5) sample chromatogram is compared with the spot on reference substance chromatography corresponding position, shows the spot of same color
Point contains prepared fleece flower root ingredient as in tonifying speen and tonifying kidney liquid medicine.
Testing result is as shown in figure 5, in Fig. 5, from left to right successively are as follows: 140501,140502,140503 sample of lot number
Product, rheum emodin reference substance, Stibene-glucoside reference substance, negative sample.
As shown in Figure 5, negative sample is noiseless, and is capable of detecting when to contain in tonifying speen and tonifying kidney liquid medicine by this detection method
Prepared fleece flower root ingredient, detection method are accurate.
In addition, using toluene-ethyl acetate-methyl alcohol-formic acid (4:3:0.8:0.2) (3:3:0.2:0.2), thiacyclohexane-vinegar
Acetoacetic ester-formic acid (5:5:1), toluene-ethyl acetate-formic acid (15:2:1), ethyl acetate-acetone-water-toluene-glacial acetic acid
(6.5:4.5:1.2:0.7:0.5), ethyl acetate-acetone-water-toluene (6.5:5.5:1.2:0.7) upper solution are expansion
Agent, find using ethyl acetate-acetone-water-toluene (6.5:5.5:1.2:0.7) upper solution as solvent when, rheum emodin and
2,3,5,4 '-tetrahydroxystilbene -2-O- β-D-Glucose glycosides can be separated with other spots, and effect is good, therefore be exhibition with it
Open agent.
Embodiment 4
A kind of thin-layered chromatography detection method of tonifying speen and tonifying kidney liquid medicine, including the thin-layered chromatography detection method to fructus lycii, including
Following steps:
1) prepared by test solution: taking tonifying speen and tonifying kidney liquid medicine 50mL, is placed in evaporating dish, water-bath is evaporated to no alcohol taste, moves
Into separatory funnel, with 10mL water washing evaporating dish, repeatedly wash, washing lotion is incorporated in separatory funnel, with ethyl acetate extraction 2
Secondary, each ethyl acetate dosage 20mL merges ethyl acetate solution, and water-bath concentration, afterwards plus ethyl acetate is settled to 1mL, obtains
Test solution；
2) prepared by control medicinal material solution: taking fructus lycii control medicinal material 2g, the ethyl alcohol 30mL that volume fraction is 60% is added to flow back
30min is extracted, filtering, filtrate water bath is evaporated to no alcohol taste, moves in separatory funnel, with ethyl acetate extraction 2 times, merges vinegar
Acetate solution, water-bath concentration, afterwards plus ethyl acetate is settled to 1mL, obtains control medicinal material solution；
3) negative control solution: taking the negative sample 50mL of scarce fructus lycii, and negative control solution is made according to step 1) method；
3) each 10 μ L of test solution, control medicinal material solution, negative control solution is taken, point sample is in same with carboxymethyl respectively
Sodium cellulosate is using ethyl acetate-dichloromethane-formic acid as solvent, to be unfolded on the silica gel g thin-layer plate of binder, take out, dry in the air
It is dry, inspected under ultraviolet light, wherein ethyl acetate, methylene chloride, formic acid volume ratio be 2:6:1；
4) sample chromatogram is compared with the spot on reference medicine chromatography corresponding position, shows the spot of same color
Point contains fructus lycii ingredient as in tonifying speen and tonifying kidney liquid medicine.
Testing result is as shown in fig. 6, in Fig. 6, from left to right successively are as follows: 140501,140502,140503 sample of lot number
Product, negative sample, fructus lycii control medicinal material.
It will be appreciated from fig. 6 that negative sample is noiseless, and it is capable of detecting when to contain in tonifying speen and tonifying kidney liquid medicine by this detection method
Fructus lycii ingredient, detection method are accurate.
Embodiment 5
A kind of thin-layered chromatography detection method of tonifying speen and tonifying kidney liquid medicine, including the thin-layered chromatography detection method to fingered citron, including
Following steps:
1) prepared by test solution: tonifying speen and tonifying kidney liquid medicine 50mL is taken, is concentrated, 20mL dehydrated alcohol is added to dissolve, filtering, and filtrate
Concentration, is settled to 1mL with dehydrated alcohol, obtains test solution；
2) prepared by control medicinal material solution: it takes fingered citron control medicinal material 1g to add in 10mL dehydrated alcohol, is ultrasonically treated 20min,
Filtering, filtrate concentration, is settled to 0.5mL with dehydrated alcohol, obtains control medicinal material solution；
3) negative control solution: taking the negative sample 50mL of scarce fingered citron, and negative control solution is made according to step 1) method；
4) each 10 μ L of test solution, control medicinal material solution, negative control solution is taken, point sample is in same with carboxymethyl respectively
Sodium cellulosate is using hexamethylene-ethyl acetate as solvent, to be unfolded on the silica gel g thin-layer plate of binder, take out, dry, in purple
Inspected under outer light, wherein hexamethylene, ethyl acetate volume ratio be 3:1；
5) sample chromatogram is compared with the spot on reference medicine chromatography corresponding position, shows the spot of same color
Point contains fingered citron ingredient as in tonifying speen and tonifying kidney liquid medicine.
Testing result is as shown in fig. 7, in Fig. 7, from left to right successively are as follows: negative sample, fingered citron control medicinal material, lot number are
140501,140502,140,503 3 samples.
As shown in Figure 7, negative sample is noiseless, and is capable of detecting when to contain in tonifying speen and tonifying kidney liquid medicine by this detection method
Fingered citron ingredient, detection method are accurate.
Embodiment 6
A kind of thin-layered chromatography detection method of tonifying speen and tonifying kidney liquid medicine, including the thin-layered chromatography detection method to Radix Astragali, including
Following steps:
1) prepared by test solution: taking tonifying speen and tonifying kidney liquid medicine 50mL, is placed in evaporating dish, water-bath is evaporated to no alcohol taste, adds
Water 50mL, flow back 1h, filtering, and filter residue volatilizes, and adds 50mL methanol, and flow back 1h, filtering, and filter residue adds 30mL water to dissolve, is saturated with water
N-butanol shaking extract 2 times, each water saturated n-butanol dosage is 20mL, aqueous is removed, by the n-butanol liquid after merging
It is evaporated, powder adds methanol 5mL to dissolve, and sets on neutral alumina column (100~200 mesh, 5g, 10~15mm), is with volume fraction
40% methanol 80mL elution, collects eluent, is evaporated, and powder adds methanol 1mL to dissolve, and obtains test solution；
2) prepared by reference substance solution: taking Astragaloside IV reference substance, the reference substance of Astragaloside IV containing 0.5mg/mL is made with methanol
Solution, obtain reference substance solution；
3) negative control solution: taking the negative sample 50mL of scarce Radix Astragali, and negative control solution is made according to step 1) method；
4) each 10 μ L of test solution, negative controls solution, 5 μ L of reference substance solution are taken, point sample is in same with carboxylic respectively
Sodium carboxymethylcellulose pyce is using chloroform-methanol-water as solvent, to be unfolded on the silica gel g thin-layer plate of binder, take out, dry in the air
Dry, it is clear that the ethanol solution of sulfuric acid for being 10% using volume fraction as color developing agent, at 105 DEG C is heated to spot development, wherein trichlorine
Methane, methanol, water volume ratio be 13:7:2；
5) sample chromatogram is compared with the spot on reference substance chromatography corresponding position, shows the spot of same color
Point as contains astragalus root components in tonifying speen and tonifying kidney liquid medicine.
Testing result is as shown in figure 8, in Fig. 8, from left to right successively are as follows: negative sample, Astragaloside IV reference substance, lot number are
140501,140502,140,503 3 samples.
As shown in Figure 8, negative sample is noiseless, and is capable of detecting when to contain in tonifying speen and tonifying kidney liquid medicine by this detection method
Astragalus root components, detection method are accurate.
In addition, once using the lower layer of chloroform-methanol-water (13: 5: 1) 10 DEG C of layerings arranged below for solvent
Solution is solvent, ammonia steam presaturation 20min；Chloroform -10 DEG C of acetate-methanol-water (3:8:4.4:2) is to transfer
Set lower layer's solution of layering；Chloroform-acetate-methanol-water (40 ︰, 5 ︰, 10 ︰ 0.2)；1,2- dichloroethanes-n-butanol-
Lower layer's solution of methanol-water (6: 8: 3: 5)；N-butanol-glacial acetic acid-water (4: 1: 1)；N-butanol-ethyl acetate-water (4: 1: 5)
Upper solution (expansion of ammonia saturated with vapor), finally obtained using chloroform-methanol-water (13:7:2) subnatant as solvent
Spot is the most clear.
Embodiment 7
A kind of thin-layered chromatography detection method of tonifying speen and tonifying kidney liquid medicine, including the thin-layered chromatography detection method to dried orange peel, including
Following steps:
1) prepared by test solution: taking tonifying speen and tonifying kidney liquid medicine 50mL, water-bath is evaporated to no alcohol taste, adds saturated sodium chloride solution
50mL, ethyl acetate 20mL are ultrasonically treated 3 times, each ultrasonic time 30min, and the ethyl acetate solution after merging ultrasound steams
Dry, obtained powder adds 2mL methanol to dissolve, and test solution is made；
2) prepared by control medicinal material solution: taking dried orange peel control medicinal material 2g, adds water 30mL to dissolve, add saturated sodium chloride solution
30mL, ethyl acetate 20mL are ultrasonically treated 3 times, each ultrasonic time 30min, and the ethyl acetate solution after merging ultrasound steams
Dry, obtained powder adds methanol to dissolve, and control medicinal material solution is made；
3) prepared by reference substance solution: taking aurantiamarin reference substance 2g, adds methanol that the reference substance of aurantiamarin containing 1.0mg/mL is made
Solution is to get reference substance solution；
4) prepared by negative control solution: taking the negative sample of scarce dried orange peel appropriate, feminine gender is made in the identical method with step 1)
Reference substance solution；
5) test solution, control medicinal material solution, negative controls solution are respectively taken into 5 μ L, 2 μ L of reference substance solution, respectively
Point sample in it is same with 0.5% sodium hydroxide solution prepare silica gel g thin-layer plate on, using acetate-methanol-water as solvent,
7cm is unfolded, takes out, dries, then using toluene-ethyl acetate-formic acid-water upper solution as solvent, be expanded to 11cm, take
Out, it dries, using 2% (w/v) alchlor ethanol solution as color developing agent, is inspected under ultraviolet light, wherein ethyl acetate, first
Alcohol, water volume ratio be 110:25:20, toluene, ethyl acetate, formic acid, water volume ratio be 30:20:1:2；
6) sample chromatogram is compared with the spot on reference medicine chromatography, reference substance chromatography corresponding position, is shown
The spot of same color contains dried orange peel ingredient as in tonifying speen and tonifying kidney liquid medicine.
Testing result shows that negative sample is noiseless, and is capable of detecting when in tonifying speen and tonifying kidney liquid medicine by this detection method
Containing dried orange peel ingredient, detection method is accurate.
Embodiment 8
A kind of thin-layered chromatography detection method of tonifying speen and tonifying kidney liquid medicine, including the thin-layered chromatography detection method to radix aucklandiae, including
Following steps:
1) prepared by test solution: taking tonifying speen and tonifying kidney liquid medicine 50mL, sets in evaporating dish, water-bath is evaporated to no alcohol taste, moves to
In separatory funnel, with 10mL water washing evaporating dish, repeatedly, washing lotion is incorporated in separatory funnel for washing, is extracted with dichloromethane 3 times,
The each dosage 25mL of methylene chloride, collects dichloromethane solution, water-bath concentration, after with methylene chloride be settled to 1mL, obtain for examination
Product solution；
2) prepared by control medicinal material solution: radix aucklandiae control medicinal material 1g being added into 25mL methylene chloride, ultrasonic 60min, mistake
Filter, filtrate are concentrated into 1mL, obtain control medicinal material solution；
3) negative control solution: taking the negative sample 50mL of scarce radix aucklandiae, and negative control solution is made using step 1) method；
4) each 10 μ L of test solution, control medicinal material solution, negative control solution is taken, point sample is in same with carboxymethyl respectively
Sodium cellulosate is using dichloromethane-cyclohexane as solvent, to be unfolded on the silica gel g thin-layer plate of binder, take out, dry, with perfume (or spice)
Oxalaldehyde sulfuric acid test solution be color developing agent, toast 5min at 105 DEG C, inspect, wherein methylene chloride, hexamethylene volume ratio be 10:
3；
5) sample chromatogram is compared with the spot on reference medicine chromatography corresponding position, shows the spot of same color
Point contains radix aucklandiae ingredient as in tonifying speen and tonifying kidney liquid medicine.
Thin-layer chromatography testing result shows that negative sample is noiseless, and is capable of detecting when invigorating the spleen benefit by this detection method
Contain radix aucklandiae ingredient in renal drug wine, detection method is accurate.
Embodiment 9
A kind of thin-layered chromatography detection method of tonifying speen and tonifying kidney liquid medicine, including the thin-layered chromatography detection method to prepared fleece flower root,
The following steps are included:
1) prepared by test solution: taking tonifying speen and tonifying kidney liquid medicine 30mL, is placed in evaporating dish, water-bath is evaporated to no alcohol taste, moves
It into separatory funnel, with 20mL water washing evaporating dish, repeatedly washs, washing lotion is incorporated in separatory funnel, extracts 3 times with chloroform, often
Secondary chloroform dosage 5mL merges chloroformic solution, adds 1g anhydrous sodium sulfate, shakes, and filtering, filtrate is concentrated into 1mL, obtains test sample
Solution；
2) prepared by reference substance solution: taking rheum emodin, 2,3,5,4 '-tetrahydroxystilbene -2-O- β-D-Glucose glycosides pair
According to product, respectively plus the solution of 2mg/mL, respectively reference substance solution one, reference substance solution two is made in dehydrated alcohol；
3) negative control solution: taking the negative sample of scarce prepared fleece flower root, obtains negative control solution according to step 1) method；
4) take each 5 μ L of test solution, reference substance solution one, reference substance solution two, negative control solution, respectively point sample in
It is same using sodium carboxymethylcellulose as on the silica gel g thin-layer plate of binder, with ethyl acetate-acetone-water-toluene upper solution
For solvent, it is unfolded, takes out, dry, inspected at ultraviolet light (365nm), wherein ethyl acetate, acetone, water, toluene
Volume ratio is 7.5:7.5:2.0:1.5；
5) sample chromatogram is compared with the spot on reference substance chromatography corresponding position, shows the spot of same color
Point contains prepared fleece flower root ingredient as in tonifying speen and tonifying kidney liquid medicine.
Testing result shows that negative sample is noiseless, and is capable of detecting when in tonifying speen and tonifying kidney liquid medicine by this detection method
Containing prepared fleece flower root ingredient, detection method is accurate.
Embodiment 10
A kind of thin-layered chromatography detection method of tonifying speen and tonifying kidney liquid medicine, including the thin-layered chromatography detection method to fructus lycii, including
Following steps:
1) prepared by test solution: taking tonifying speen and tonifying kidney liquid medicine 50mL, is placed in evaporating dish, water-bath is evaporated to no alcohol taste, moves
Into separatory funnel, with 10mL water washing evaporating dish, repeatedly wash, washing lotion is incorporated in separatory funnel, with ethyl acetate extraction 3
Secondary, each ethyl acetate dosage 20mL merges ethyl acetate solution, and water-bath concentration, afterwards plus ethyl acetate is settled to 1mL, obtains
Test solution；
2) prepared by control medicinal material solution: taking fructus lycii control medicinal material 2g, the ethyl alcohol 30mL that volume fraction is 60% is added to flow back
60min is extracted, filtering, filtrate water bath is evaporated to no alcohol taste, moves in separatory funnel, with ethyl acetate extraction 3 times, merges vinegar
Acetate solution, water-bath concentration, afterwards plus ethyl acetate is settled to 1mL, obtains control medicinal material solution；
3) negative control solution: taking the negative sample 50mL of scarce fructus lycii, and negative control solution is made according to step 1) method；
3) each 10 μ L of test solution, control medicinal material solution, negative control solution is taken, point sample is in same with carboxymethyl respectively
Sodium cellulosate is using ethyl acetate-dichloromethane-formic acid as solvent, to be unfolded on the silica gel g thin-layer plate of binder, take out, dry in the air
It is dry, inspected under ultraviolet light, wherein ethyl acetate, methylene chloride, formic acid volume ratio be 2:4:1；
4) sample chromatogram is compared with the spot on reference medicine chromatography corresponding position, shows the spot of same color
Point contains fructus lycii ingredient as in tonifying speen and tonifying kidney liquid medicine.
Testing result shows that negative sample is noiseless, and is capable of detecting when in tonifying speen and tonifying kidney liquid medicine by this detection method
Containing fructus lycii ingredient, detection method is accurate.
Embodiment 11
A kind of thin-layered chromatography detection method of tonifying speen and tonifying kidney liquid medicine, including the thin-layered chromatography detection method to fingered citron, including
Following steps:
1) prepared by test solution: tonifying speen and tonifying kidney liquid medicine 50mL is taken, is concentrated, 20mL dehydrated alcohol is added to dissolve, filtering, and filtrate
Concentration, is settled to 2mL with dehydrated alcohol, obtains test solution；
2) prepared by control medicinal material solution: it takes fingered citron control medicinal material 1g to add in 10mL dehydrated alcohol, is ultrasonically treated 60min,
Filtering, filtrate concentration, is settled to 1.0mL with dehydrated alcohol, obtains control medicinal material solution；
3) negative control solution: taking the negative sample 50mL of scarce fingered citron, and negative control solution is made according to step 1) method；
4) each 10 μ L of test solution, control medicinal material solution, negative control solution is taken, point sample is in same with carboxymethyl respectively
Sodium cellulosate is using hexamethylene-ethyl acetate as solvent, to be unfolded on the silica gel g thin-layer plate of binder, take out, dry, in purple
Inspected under outer light, wherein hexamethylene, ethyl acetate volume ratio be 5:1；
5) sample chromatogram is compared with the spot on reference medicine chromatography corresponding position, shows the spot of same color
Point contains fingered citron ingredient as in tonifying speen and tonifying kidney liquid medicine.
Testing result shows that negative sample is noiseless, and is capable of detecting when in tonifying speen and tonifying kidney liquid medicine by this detection method
Containing fingered citron ingredient, detection method is accurate.
Embodiment 12
A kind of thin-layered chromatography detection method of tonifying speen and tonifying kidney liquid medicine, including the thin-layered chromatography detection method to Radix Astragali, including
Following steps:
1) prepared by test solution: taking tonifying speen and tonifying kidney liquid medicine 50mL, is placed in evaporating dish, water-bath is evaporated to no alcohol taste, adds
Water 50mL, flow back 2h, filtering, and filter residue volatilizes, and adds 50mL methanol, and flow back 2h, filtering, and filter residue adds 30mL water to dissolve, is saturated with water
N-butanol shaking extract 3 times, each water saturated n-butanol dosage is 20mL, aqueous is removed, by the n-butanol liquid after merging
It is evaporated, powder adds methanol 5mL to dissolve, and sets on neutral alumina column (100~200 mesh, 5g, 10~15mm), is with volume fraction
40% methanol 80mL elution, collects eluent, is evaporated, and powder adds methanol 1.5mL to dissolve, and obtains test solution；
2) prepared by reference substance solution: taking Astragaloside IV reference substance, the reference substance of Astragaloside IV containing 1.0mg/mL is made with methanol
Solution, obtain reference substance solution；
3) negative control solution: taking the negative sample 50mL of scarce Radix Astragali, and negative control solution is made according to step 1) method；
4) each 10 μ L of test solution, negative controls solution, 5 μ L of reference substance solution are taken, point sample is in same with carboxylic respectively
Sodium carboxymethylcellulose pyce is using chloroform-methanol-water as solvent, to be unfolded on the silica gel g thin-layer plate of binder, take out, dry in the air
Dry, it is clear that the ethanol solution of sulfuric acid for being 15% using volume fraction as color developing agent, at 108 DEG C is heated to spot development, wherein trichlorine
Methane, methanol, water volume ratio be 20:110:3；
5) sample chromatogram is compared with the spot on reference substance chromatography corresponding position, shows the spot of same color
Point as contains astragalus root components in tonifying speen and tonifying kidney liquid medicine.
Testing result shows that negative sample is noiseless, and is capable of detecting when in tonifying speen and tonifying kidney liquid medicine by this detection method
Containing astragalus root components, detection method is accurate.
Comparative example 1
This comparative example 1 and the distinctive points of embodiment 1 are: in this comparative example, in step 1), test solution water-bath is flung to
After ethyl alcohol, add salt acid for adjusting pH to 1~2, and do not carry out second outspread when thin-layer chromatography, is only with acetate-methanol-water
Solvent.
As shown in Fig. 2, in Fig. 2, be followed successively by negative sample, aurantiamarin reference substance, lot number from left to right is testing result
140501,140502,140,503 3 parts of samples, the spot of test solution is in speckle displacement corresponding with reference substance solution
On cannot be kept completely separate with other spots, it is ineffective.Illustrate One step development method in this comparative example 1 cannot well by for
Test sample solution expansion, cannot complete the detection to dried orange peel.
Comparative example 2
This comparative example 2 and the distinctive points of embodiment 1 are: in this comparative example, after ethyl alcohol is flung in test solution water-bath, adding
Salt acid for adjusting pH is to 1~2, and when thin-layer chromatography, the solvent of One step development is acetate-methanol-water (100:17:13), and two
The solvent of secondary expansion is chloroform-ethyl acetate-glacial acetic acid-water (20:10:10:1).
Testing result is as shown in figure 3, in Fig. 3, and the spot of test solution is in spot corresponding with reference substance solution
It cannot be kept completely separate with other spots on position, it is ineffective.Illustrate the solvent selected in the expansion twice in this comparative example 1
Test solution cannot be unfolded well, the detection to dried orange peel cannot be completed.
Claims (6)
1. a kind of thin-layered chromatography detection method of tonifying speen and tonifying kidney liquid medicine, which is characterized in that tonifying speen and tonifying kidney liquid medicine includes following component:
Dried orange peel, radix aucklandiae, prepared fleece flower root, fructus lycii, fingered citron, Radix Astragali；
Wherein, to the thin-layered chromatography detection method of dried orange peel, comprising the following steps:
1) prepared by test solution: taking tonifying speen and tonifying kidney liquid medicine, water-bath is evaporated to no alcohol taste, adds saturated sodium chloride solution and acetic acid second
Ester is ultrasonically treated 2~3 times, each 20~30min of ultrasonic time, and the ethyl acetate solution after merging ultrasound is evaporated, obtains
Powder adds 1~2mL methanol to dissolve, and test solution is made；
2) prepared by control medicinal material solution: taking dried orange peel control medicinal material, is dissolved in water, add saturated sodium chloride solution and ethyl acetate, surpasses
Sonication 2~3 times, each 20~30min of ultrasonic time, the ethyl acetate solution after merging ultrasound is evaporated, obtained powder adds
Methanol dissolution, is made control medicinal material solution；
3) prepared by reference substance solution: taking aurantiamarin reference substance, adds methanol that the solution of the aurantiamarin containing 0.5~1.0mg/mL is made, i.e.,
Obtain reference substance solution；
4) by test solution, control medicinal material solution, reference substance solution difference point sample in same silica gel plate, with ethyl acetate-first
Alcohol-water be solvent, be unfolded 5~7cm, take out, dry, then with toluene-ethyl acetate-formic acid-water upper solution be expansion
Agent is expanded to 10~12cm, takes out, dries, using 1~2% (w/v) alchlor ethanol solution as color developing agent, in ultraviolet light
Under inspect, wherein ethyl acetate, methanol, water volume ratio be (100~110): (17~25): (13~20), toluene, acetic acid
Ethyl ester, formic acid, water volume ratio be (20~30): (10~20): (1~2): (1~2)；
5) sample chromatogram is compared with the spot on reference medicine chromatography, reference substance chromatography corresponding position, is shown identical
The spot of color contains dried orange peel ingredient as in tonifying speen and tonifying kidney liquid medicine.
2. a kind of thin-layered chromatography detection method of tonifying speen and tonifying kidney liquid medicine according to claim 1, which is characterized in that radix aucklandiae
Thin-layered chromatography detection method, comprising the following steps:
1) prepared by test solution: taking tonifying speen and tonifying kidney liquid medicine, water-bath is evaporated to no alcohol taste, moves in separatory funnel, uses dichloromethane
Alkane extracts 2~3 times, collects dichloromethane solution, water-bath concentration, after with methylene chloride be settled to 1mL, obtain test solution；
2) prepared by control medicinal material solution: radix aucklandiae control medicinal material being added into methylene chloride, 30~60min of ultrasound, is filtered, filtrate
It is concentrated into 1mL, obtains control medicinal material solution；
It 3) is expansion with dichloromethane-cyclohexane by test solution, control medicinal material solution difference point sample in same silica gel plate
Agent is unfolded, and takes out, dries, using vanillin-sulfuric acid test solution as color developing agent, inspect, wherein the volume ratio of methylene chloride, hexamethylene
For (5~10): (1~3)；
4) sample chromatogram is compared with the spot on reference medicine chromatography corresponding position, shows the spot of same color,
Contain radix aucklandiae ingredient as in tonifying speen and tonifying kidney liquid medicine.
3. a kind of thin-layered chromatography detection method of tonifying speen and tonifying kidney liquid medicine according to claim 1, which is characterized in that system what
The thin-layered chromatography detection method of the tuber of multiflower knotweed, comprising the following steps:
1) prepared by test solution: taking tonifying speen and tonifying kidney liquid medicine, water-bath is evaporated to no alcohol taste, moves in separatory funnel, extracted with chloroform
It takes 2~3 times, merges chloroformic solution, add anhydrous sodium sulfate, shake, filtering, filtrate is concentrated into 1mL, obtains test solution；
2) prepared by reference substance solution: take rheum emodin, 2,3,5,4 '-tetrahydroxystilbene -2-O- β-D-Glucose glycosides reference substance,
Respectively plus the solution of 1~2mg/mL, respectively reference substance solution one, reference substance solution two is made in dehydrated alcohol；
3) test solution, reference substance solution one, reference substance solution two are distinguished into point sample in same silica gel plate, with ethyl acetate-
Acetone-water-toluene upper solution is solvent, is unfolded, and takes out, dries, inspect under ultraviolet light, wherein ethyl acetate,
Acetone, water, toluene volume ratio be (6.5~7.5): (5.5~7.5): (1.2~2.0): (0.7~1.5)；
4) sample chromatogram is compared with the spot on reference substance chromatography corresponding position, shows the spot of same color, i.e.,
To contain prepared fleece flower root ingredient in tonifying speen and tonifying kidney liquid medicine.
4. a kind of thin-layered chromatography detection method of tonifying speen and tonifying kidney liquid medicine according to claim 1, which is characterized in that fructus lycii
Thin-layered chromatography detection method, comprising the following steps:
1) prepared by test solution: taking tonifying speen and tonifying kidney liquid medicine, water-bath is evaporated to no alcohol taste, moves in separatory funnel, with acetic acid second
Ester extracts 2~3 times, merges ethyl acetate solution, and water-bath concentration, afterwards plus ethyl acetate is settled to 1mL, obtains test solution；
2) control medicinal material solution prepare: take fructus lycii control medicinal material, add volume fraction be 60% alcohol reflux extract 30~
60min, filtering, filtrate water bath is evaporated to no alcohol taste, moves in separatory funnel, with ethyl acetate extraction 2~3 times, merges vinegar
Acetate solution, water-bath concentration, afterwards plus ethyl acetate is settled to 1mL, obtains control medicinal material solution；
3) by test solution, control medicinal material solution difference point sample in same silica gel plate, with ethyl acetate-dichloromethane-formic acid
For solvent, it is unfolded, takes out, dry, inspected under ultraviolet light, wherein the volume ratio of ethyl acetate, methylene chloride, formic acid
For (2~4): (6~8): (1~2)；
4) sample chromatogram is compared with the spot on reference medicine chromatography corresponding position, shows the spot of same color,
Contain fructus lycii ingredient as in tonifying speen and tonifying kidney liquid medicine.
5. a kind of thin-layered chromatography detection method of tonifying speen and tonifying kidney liquid medicine according to claim 1, which is characterized in that fingered citron
Thin-layered chromatography detection method, comprising the following steps:
1) prepared by test solution: taking tonifying speen and tonifying kidney liquid medicine, is concentrated, dehydrated alcohol is added to dissolve, filter, filtrate is concentrated, and use is anhydrous
Ethyl alcohol is settled to 1~2mL, obtains test solution；
2) prepared by control medicinal material solution: it takes fingered citron control medicinal material to add in dehydrated alcohol, is ultrasonically treated 20~60min, filter, filter
Liquid concentration, is settled to 0.5~1.0mL with dehydrated alcohol, obtains control medicinal material solution；
It 3) is expansion with hexamethylene-ethyl acetate by test solution, control medicinal material solution difference point sample in same silica gel plate
Agent, be unfolded, take out, dry, inspected under ultraviolet light, wherein hexamethylene, ethyl acetate volume ratio be (3~6): (1~
2)；
4) sample chromatogram is compared with the spot on reference substance chromatography corresponding position, shows the spot of same color, i.e.,
To contain fingered citron ingredient in tonifying speen and tonifying kidney liquid medicine.
6. a kind of thin-layered chromatography detection method of tonifying speen and tonifying kidney liquid medicine according to claim 1, which is characterized in that Radix Astragali
Thin-layered chromatography detection method, comprising the following steps:
1) prepared by test solution: taking tonifying speen and tonifying kidney liquid medicine, water-bath is evaporated to no alcohol taste, adds water, and flow back 1~2h, filtering, filter residue
It volatilizes, adds methanol, flow back 1~2h, filtering, and filter residue is dissolved in water, and the n-butanol shaking being saturated with water is extracted 2~3 times, goes to remove water
N-butanol liquid is evaporated by liquid, and powder adds 5~10mL of methanol to dissolve, and is set on neutral alumina column, is 40% methanol with volume fraction
Elution is collected eluent, is evaporated, and powder adds 1~1.5mL of methanol to dissolve, and obtains test solution；
2) prepared by reference substance solution: taking Astragaloside IV reference substance, the solution of 0.5~1.0mg/mL is made of methanol, is compareed
Product solution；
3) by test solution, reference substance solution difference point sample in same silica gel plate, using chloroform-methanol-water as solvent,
Expansion is taken out, is dried, the ethanol solution of sulfuric acid for being 10~15% using volume fraction is heated at 105~108 DEG C as color developing agent
Spot development is clear, wherein chloroform, methanol, water volume ratio be (13~20): (7~10): (2~3)；
4) sample chromatogram is compared with the spot on reference substance chromatography corresponding position, shows the spot of same color, i.e.,
To contain astragalus root components in tonifying speen and tonifying kidney liquid medicine.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110927322A (en) * | 2019-11-07 | 2020-03-27 | 石药集团中奇制药技术（石家庄）有限公司 | Detection method of agastache rugosus healthy energy mixture |
| CN111912916A (en) * | 2020-07-14 | 2020-11-10 | 成都中医药大学 | Method for measuring content of index components in fingered citron preparation |
| CN116338073A (en) * | 2023-05-19 | 2023-06-27 | 山东省食品药品检验研究院 | Thin-layer chromatography detection method of astragalus and leech kidney-tonifying capsules |
-
2018
- 2018-11-26 CN CN201811413527.1A patent/CN109298125A/en not_active Withdrawn
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110927322A (en) * | 2019-11-07 | 2020-03-27 | 石药集团中奇制药技术（石家庄）有限公司 | Detection method of agastache rugosus healthy energy mixture |
| CN110927322B (en) * | 2019-11-07 | 2022-05-17 | 石药集团中奇制药技术（石家庄）有限公司 | Detection method of Huoxiang Zhengqi mixture |
| CN111912916A (en) * | 2020-07-14 | 2020-11-10 | 成都中医药大学 | Method for measuring content of index components in fingered citron preparation |
| CN116338073A (en) * | 2023-05-19 | 2023-06-27 | 山东省食品药品检验研究院 | Thin-layer chromatography detection method of astragalus and leech kidney-tonifying capsules |
| CN116338073B (en) * | 2023-05-19 | 2023-07-25 | 山东省食品药品检验研究院 | Thin-layer chromatography detection method of astragalus and leech kidney-tonifying capsules |
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