CN107543892A - The TLC Identification of evergreen mucuna stem in stilbene jujube oral liquid - Google Patents
The TLC Identification of evergreen mucuna stem in stilbene jujube oral liquid Download PDFInfo
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- CN107543892A CN107543892A CN201710582799.3A CN201710582799A CN107543892A CN 107543892 A CN107543892 A CN 107543892A CN 201710582799 A CN201710582799 A CN 201710582799A CN 107543892 A CN107543892 A CN 107543892A
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Abstract
The present invention relates to the discrimination method of evergreen mucuna stem in stilbene jujube oral liquid.This method comprises the following steps：The preparation of specific test sample, reference substance and control medicinal material solution, using by test solution volume ratio as 8:6:0.5 normal heptane ethyl acetate formic acid mixed liquor deploys for solvent；Need testing solution, reference substance solution and control medicinal material solution are put in same silica gel thin-layer plate respectively, heated 1 minute at 105 °C, put and inspected under ultraviolet lamp (254nm), have corresponding spot on a corresponding position with control medicinal material, reference substance in test sample chromatogram.The present invention be directed to the TLC Identification of evergreen mucuna stem component in stilbene jujube oral liquid.There is corresponding spot in this method test sample chromatogram on a corresponding position with control medicinal material, reference substance, corresponding clear spot, separating degree is good, can differentiate for the evergreen mucuna stem in stilbene jujube oral liquid and provide foundation.This method is simple to operate, and detection is quick, suitable for large-scale production flow or finished product detection and identification.
Description
Technical field
The present invention relates to evergreen mucuna stem discrimination method in stilbene jujube oral liquid.
Background technology
Containing the Radix Astragali, jujube, Poria cocos, evergreen mucuna stem medicinal extract four traditional Chinese medicine in stilbene jujube oral liquid prescription, by water extract-alcohol precipitation
Extraction separation and purification after, main active is the compositions such as polysaccharide, glycoside, saponins and flavonoids in stilbene jujube oral liquid.
Stilbene jujube oral liquid has blood-enrich, strengthening the spleen and stomach and other effects, is usually used in leukopenia and physically weak after being ill, liver loss institute
The diseases such as the immunity degradation of cause.Evergreen mucuna stem, it is the rattan of legume evergreen mucuna stem.It is warm-natured, bitter.Mended with promoting circulation of blood
Blood, clearing and activating the channels and collaterals effect, for controlling articular rheumatic pain, traumatic injury, the deficiency of blood, irregular menstruation and Amenorrhea.Evergreen mucuna stem is made
For the key component of stilbene jujube oral liquid, for effectively control quality, detection is carried out to evergreen mucuna stem therein and is very important.
The content of the invention
The invention provides a kind of TLC Identification of evergreen mucuna stem in stilbene jujube oral liquid.This method includes supplying
Prepared by test sample solution, reference substance solution and control medicinal material solution, expansion and colour developing reviewing step.This method using formoononetin as
Reference substance；Using normal heptane-acetic ether-methanoic acid solution as solvent, by volume 8:5-7:0.5 proportioning is prepared；Will be for examination
Product solution, reference substance solution and control medicinal material solution are put in same silica gel thin-layer plate respectively, are heated 1 minute, are put ultraviolet at 105 DEG C
Inspected under light lamp (254 nm).
The solvent proportioning is preferably 8:6:0.5.
The preferred point sample amount of need testing solution, reference substance solution and control medicinal material solution is respectively in deployment step：15μL、
2 μ L and 15 μ L.
The preferred silica G F of described silica gel thin-layer plate254Lamellae.
The preferably 15 minutes presaturation time of the deployment step, preferably humidity are 72%, and preferable temperature is 25 DEG C.
The need testing solution preparation process is:Stilbene jujube oral liquid is taken to be extracted with ethyl acetate, solid-liquid ratio 1: 2-4 is excellent
Sorting liquor ratio is 3: 8；Extract solution is evaporated, residue is dissolved with methanol, is produced.
The reference substance solution preparation process is：Formoononetin reference substance is taken, it is 0.4- to add methanol that concentration is made
The concentration of 0.7mg/mL solution, preferably reference substance solution is 0.5mg/mL, is produced.
The preparation method of the control medicinal material solution is：Evergreen mucuna stem Chinese medicine is taken by solid-liquid ratio 3g:40-60ml, use
Methanol extracts；Solvent evaporated, extracted with the ethyl acetate for being equal to methanol usage, solvent evaporated, with methanol dissolved residue, i.e.,
.
The present invention is to be directed to the TLC Identification of evergreen mucuna stem component in stilbene jujube oral liquid first.This method supplies
There are corresponding spot, corresponding clear spot, separating degree in test product chromatogram on a corresponding position with control medicinal material, reference substance
It is good, it can differentiate for the evergreen mucuna stem in stilbene jujube oral liquid and foundation is provided.And it is simple to operate, detection is quick, is given birth to suitable for scale
Produce flow in or finished product detection and identification.
Brief description of the drawings
Fig. 1 is that the thin layer of the evergreen mucuna stem of embodiment 1 differentiates collection of illustrative plates；
Fig. 2 is difference of embodiment of the present invention lamellae expansion effect collection of illustrative plates；
Fig. 3 is different temperatures of embodiment of the present invention expansion effect collection of illustrative plates；
Fig. 4 is different humidity of embodiment of the present invention expansion effect collection of illustrative plates；
Fig. 5 is that repeatability of the embodiment of the present invention investigates collection of illustrative plates；
Fig. 6 is difference sample solution preparation method Comparative map of the embodiment of the present invention；
Fig. 7 is the effect Comparative map of difference solvent of the embodiment of the present invention.
Embodiment
With reference to specific embodiment, the present invention will be further described.
Embodiment 1
First, experiment material
Experiment 10 batches of stilbene jujube oral liquids used are provided by Hang Seng of Zhongshan city medicine company, and its lot number is：20130901,
20130902,20130903,20131001,20131002,20131003,20131101,20131102,20131103,
20131104。
2nd, instrument, reagent and reagent
Lamellae：Silica G F254(Taizhou road and bridge tetramethyl biochemistry plastic molding and processing plant), silica G F254(Merck KGaA company).Balance：
One thousandth balance (plum Teller ME203E), a ten thousandth balance (plum Teller ME204), ten a ten thousandth balance (plum Tellers
MS105)；Supersonic generator (Kunshan Ultrasonic K Q-700DE 40KHz, 280W)；Ultrapure water system：German Millipore is (close
Li Bo) company；Thin-layer chromatography digital image-forming instrument (the biochemical Co., Ltd GOOD LOOK-1000 of Shanghai section wise man).Methanol etc. is state
Production analysis is pure, and water is ultra-pure water (resistivity 18.2mQ.cm).Methanol etc. is that domestic analysis is pure, and water is ultra-pure water (resistivity
18.2mQ.cm).Formoononetin reference substance (lot number：F111388；CAS:485-72-3, content>98%) it is purchased from Chinese food
Drug assay research institute.Evergreen mucuna stem medicinal material is accredited as pulse family evergreen mucuna stem Mucuna by south China Institute of Zoology
Sempervirens drying rattan.
3rd, method and result
(1) preparation of solution
1. the preparation of need testing solution：This product 15mL is taken, with ethyl acetate shaking extraction 3 times, each 40mL, merges acetic acid
Ethyl ester liquid, is evaporated, and residue methanol 2mL dissolves, and produces.
2. the preparation of reference substance solution：Formoononetin reference substance is taken, adds methanol that 0.512mg/mL solution is made, i.e.,
.
3. the preparation of control medicinal material solution：3 grams of samples (crossing No. three sieves) are taken, add methanol 40mL ultrasound 40min, filtering is evaporated
Solvent, water 20mL low-grade fevers are added to dissolve, ethyl acetate 40mL is extracted 3 times, solvent evaporated, methanol 2mL dissolved residues, is produced.
(2) discrimination method
Lamellae：Silica GF254 prefabricated board；
Point sample amount：The μ L of test sample 15, the μ L of reference substance solution 2, the μ L of control medicinal material 15；
Solvent：Normal heptane-acetic ether-methanoic acid=8:6:0.5(v/v)；It is 64% to deploy humidity, and temperature is 28 DEG C.
Presaturation 15min, open up away from：8cm；
Inspect：Dry, heated 1 minute at 105 DEG C, put and inspected under ultraviolet lamp (254nm).
(3) identification result
As can be seen that in test sample chromatogram with control medicinal material, reference substance on a corresponding position under uviol lamp (254nm)
There is corresponding spot, correspond to clear spot, separating degree is good.As a result Fig. 1 is seen.In Fig. 1, each numbering is corresponding：1. test sample (batch
Number： 20130901)；2. test sample (lot number：20131002)；3. test sample (lot number：20131103)；4. control medicinal material； 5.
Control medicinal material；6. formoononetin.
(4) durability is investigated
1. the investigation of different lamellaes
It has chosen Taizhou silica G F254Prefabricated sheets plate and Merk GF254Prefabricated sheets plate is respectively by the test method drafted
Experiment, the results showed that：Above-mentioned different silica gel plates can reach the requirement of discriminating, and spot is clear, concentrates, and separating degree is good, its
Middle Merk plates it is better.As a result Fig. 2 is seen, it is illustrated that sample is corresponding to numbering：1. test sample (lot number：20130901)；2.
Test sample (lot number：20131002)；3. control medicinal material；4. control medicinal material；5. formoononetin.
2. different temperatures is investigated
The lamellae after point sample, deploy at a temperature of being respectively placed in 4 DEG C and 30 DEG C, inspect, the results showed that：In the method
The test sample chromatogram spot corresponding with reference substance spot under 4 DEG C and 30 DEG C of humidity is clear, and separating degree is good.Opened up at 4 DEG C
Spot is opened relatively to concentrate, but development rate is slower, relatively evenly, effect is preferable for spot at room temperature.As a result such as Fig. 3, Fig. 1
In, each numbering is corresponding：1. test sample (lot number：20130901)；2. test sample (lot number：20131002)；3. control medicinal material；4.
Formoononetin.
3. investigate different humidity
The lamellae after point sample, it is respectively placed in 32% and 72% humidity and deploys in chromatography cylinder, inspect, as a result table
It is bright：The method is under 32% and 72% humidity, and test sample chromatogram has corresponding spot to reference substance chromatogram, and spot is clear, point
From spending.Spot is not enough concentrated under wherein 32% humidity, slightly edge effect, is deployed spot under 72% humidity and is more concentrated, effect
Preferably, therefore suggest deploying under the higher environment of humidity.As a result such as Fig. 4.
(5) repeatability is investigated
10 batches of samples are taken, need testing solution is prepared according to the method for drafting, are deployed according to method is drafted in chromatography cylinder,
Inspected under 254nm ultraviolet lights.As a result show：There is the spot with control medicinal material, reference substance in relevant position in ten batches of samples,
Spot is more clear, and method is reproducible.As a result such as Fig. 5, it is illustrated that numbering counter sample：1. test sample 20130901；2. for examination
Product 20130902；3. test sample 20130903；4. test sample 20131001；5. test sample 20131002；6. test sample
20131003；7. test sample 20131101；8. test sample 20131102；9. test sample 20131103；10. test sample
20131104；11. control medicinal material；12. control medicinal material；13. formoononetin.
(6) investigation of thin-layer chromatography condition
1. the selection of thin-layer chromatography extracting method
Extracting method A：This product 3g is taken, adds methanol 50mL to be heated to reflux 1h, is filtered, filtrate is evaporated, made with methanol 2mL molten
Solution, is produced.
Extracting method B：This product 3g is taken, adds methanol 50mL cold soakings to extract 4h, filtration, filtrate is evaporated, made with methanol 2mL molten
Solution, is produced.
Extracting method C：This product 3g is taken, adds methanol 50mL, is ultrasonically treated 1h, filtration, filtrate is evaporated, and uses ethyl acetate
30mL is extracted 3 times, and filtrate is evaporated, and makes dissolving with methanol 2mL, produces.
Extracting method D：This product 3g is taken, adds methanol 50rnL, is ultrasonically treated 40min, filtration, filtrate is evaporated, and uses ethyl acetate
Extraction 2 times, each 30mL, merging filtrate is evaporated, and is made dissolving with methanol 2mL, is produced.
Extracting method E：This product powder 1.5g is taken, adds methanol 50mL, is ultrasonically treated 40min, filtration, filtrate is evaporated, and uses second
Acetoacetic ester is extracted 1 time, and each 30mL, merging filtrate is evaporated, and is made dissolving with methanol 2mL, is produced.
Draw each 15 μ L of above-mentioned sample solution and the μ L of reference substance solution 2 are put in same silica G F respectively254On lamellae,
Respectively with normal heptane-acetic ether-methanoic acid=8:6:0.5 (v/v), deploy, take out, dry, inspected under ultraviolet light (254nm).
Test sample chromatogram shows the spot of same color respectively on position corresponding with reference substance chromatogram.As a result Fig. 6 is seen, it is illustrated that numbering
Counter sample is：1. extracting method A；2. extracting method B；3. extracting method C；4. extracting method D；5. extracting method E；6. pair
According to the formoononetin of medicinal material 7..As seen from the figure, extracting method C spot is more visible, and Chromatographic information is more, therefore selects C to be used as and carry
Take method.
2. the selection of different solvents
Solvent A：Chloroform-acetone-formic acid=8:1:0.5(v/v)
Solvent B：Hexamethylene-butyl acetate-formic acid=8:6:0.5(v/v)
Solvent C：Normal heptane-acetic ether-methanoic acid=8:6:0.5(v/v)
It is each with sample solution to draw above-mentioned reference substance, puts respectively in same silica G F254On lamellae, respectively with above-mentioned
Solvent A, B, C, deploy, take out, dry, heated several minutes at 105 DEG C, put inspected under ultraviolet lamp (254nm) respectively.For
In test product chromatogram, on position corresponding with reference substance chromatogram, show the spot of same color respectively.As a result 7 are seen, it is illustrated that corresponding to compile
Number：1. test sample (lot number：20130901)；2. test sample (lot number：20131002)；3. test sample (lot number 20131103) 4.
The control medicinal material of control medicinal material 5.；6. formoononetin.As seen from the figure, solvent C expansion effect is good, and test sample chromatogram is with compareing
Show the spot of same color on the corresponding position of product chromatogram, and clear spot is concentrated, Rf values are moderate, and separating degree is good.Therefore selection is just
Heptane-ethyl acetate-formic acid=8:6:0.5 is solvent.
Claims (10)
1. the TLC Identification of evergreen mucuna stem in stilbene jujube oral liquid, including need testing solution, reference substance solution and right
According to medicinal material solution preparation step, expansion and colour developing reviewing step, it is characterised in that：Using formoononetin as reference substance；With positive heptan
Alkane-acetic ether-methanoic acid is solvent, and proportioning by volume is 8:5-7:0.5；By need testing solution, reference substance solution and
Control medicinal material solution is put in same silica gel thin-layer plate respectively, is heated 1 minute at 105 DEG C, is put and inspected under ultraviolet lamp (254nm).
2. discrimination method as claimed in claim 1, it is characterised in that：The solvent proportioning is 8:6:0.5.
3. discrimination method as claimed in claim 1 or 2, it is characterised in that：Need testing solution, reference substance solution in deployment step
And the point sample amount of control medicinal material solution is respectively：15 μ L, 2 μ L and 15 μ L.
4. discrimination method as claimed in claim 1 or 2, it is characterised in that：The deployment step also includes presaturation step, in advance
Saturation time is 15 minutes, humidity 72%, and temperature is 25 DEG C.
5. discrimination method as claimed in claim 1 or 2, it is characterised in that：The need testing solution preparation process is:Take stilbene jujube
Oral liquid is extracted with ethyl acetate, is evaporated extract solution, and residue is dissolved with methanol, is produced.
6. discrimination method as claimed in claim 5, it is characterised in that：The stilbene jujube oral liquid is with ethyl acetate extraction step
Solid-liquid ratio be 1: 2-4.
7. discrimination method as claimed in claim 6, it is characterised in that：Described solid-liquid ratio is 3: 8.
8. discrimination method as claimed in claim 1 or 2, it is characterised in that described reference substance solution preparation process is：Take thorn
Onocerin reference substance, it is 0.4-0.7mg/mL solution to add methanol that concentration is made, and is produced.
9. discrimination method as claimed in claim 8, it is characterised in that the concentration of the reference substance solution is 0.5mg/mL.
10. discrimination method as claimed in claim 1 or 2, it is characterised in that the control medicinal material solution is prepared as：Take often
Spring mucuna Chinese medicine presses solid-liquid ratio 3g:40-60ml, extracted with methanol；Solvent evaporated, with the acetic acid second for being equal to methanol usage
Ester extracts, and solvent evaporated, with methanol dissolved residue, produces.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102406720A (en) * | 2011-11-30 | 2012-04-11 | 中山市中智药业集团有限公司 | Radix astragali and Chinese date oral liquid |
| CN104926774A (en) * | 2015-07-10 | 2015-09-23 | 南京大学 | Formononetin Schiff base derivative and synthesizing method and application thereof |
-
2017
- 2017-07-17 CN CN201710582799.3A patent/CN107543892A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102406720A (en) * | 2011-11-30 | 2012-04-11 | 中山市中智药业集团有限公司 | Radix astragali and Chinese date oral liquid |
| CN104926774A (en) * | 2015-07-10 | 2015-09-23 | 南京大学 | Formononetin Schiff base derivative and synthesizing method and application thereof |
Non-Patent Citations (1)
| Title |
|---|
| 刘星云 等: "芪枣口服液薄层鉴别研究", 《中华中医药学会中成药分会2016年学术研讨会论文集》 * |
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