CN105403654B - A kind of method for improving the identification of Radix Astragali thin-layer chromatography - Google Patents
A kind of method for improving the identification of Radix Astragali thin-layer chromatography Download PDFInfo
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- CN105403654B CN105403654B CN201510923327.0A CN201510923327A CN105403654B CN 105403654 B CN105403654 B CN 105403654B CN 201510923327 A CN201510923327 A CN 201510923327A CN 105403654 B CN105403654 B CN 105403654B
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Abstract
The invention discloses a kind of method for improving the identification of Radix Astragali thin-layer chromatography, comprises the following steps that：(1) Radix Astragali is ground to into powder first，2 3g of the powder is weighed accurately with balance is weighed，Add chloroform n-butanol 75ml，It is heated to reflux，After 3h，Filter，Then filtrate is evaporated，Residue adds the KOH methyl alcohol saponification liquor saponification process of 8mL 10mL，The KOH methyl alcohol saponification liquors of 8mL 10mL are added again，It is heated to reflux 0.5 1h，It is evaporated，The residue 30ml that adds water makes dissolving，After ultrasonic extraction 30min 40min，Add ethyl acetate this is extracted twice as supplying sample，Point sample is on same silica gel g thin-layer plate，Same solvent，First launch，Further take out，Dry again，Put under JL P10A viewboxs or daylight UV light lamp 365nm under inspect，Finally take pictures，Solve the problems, such as that definition of the Astragaloside IV in chromatogram be not high，It is a kind of accurate、Method that is clear and quickly differentiating the Radix Astragali.
Description
Technical field
The invention belongs to biological technical field, and in particular to a kind of method of raising Radix Astragali thin-layer chromatography identification.
Background technology
This product is the dry root of legume astragalus mongolicus or Astragalus membranacus, and spring, the excavation of two season of autumn remove fibrous root and root
Head, rinses well, takes advantage of fresh-cut sheet, is dried, referred to as " astragalus mongholicus tablet ", this product surface light brown yellow or light brown brown, has irregular
Longitudinal furrow line or Zou's pleat that shrinks.Matter is hard and tough, section fibrous, and aobvious mealiness, and skin zone's yellow-white, woody part are faint yellow, have radiation
Shape texture, or tool crack.Gas is micro-, and taste is micro- sweet, and that what is chewed micro- has beany flavor.
The work of quality standards in Chinese drugs has been in full swing, and traditional Chinese medicine scholar is asked with reference to relevant in current Quality research on standard
Topic, it is proposed that some views.It is drafting for title first, it is therefore desirable to embody the foundation of the method for inspection and the formulation of standard specification
Two contents, secondly it is important that identification experiment, mainly solves the authenticity of tested medicine, have proterties discriminating, microscopical characters
With physics and chemistry differentiate etc..In physics and chemistry discriminating in addition to general chemical experiment such as color reaction, current extensive application is chromatography, and
It is again most widely used with thin-layer chromatography, because its easy, easy, sensitivity is high, specificity is strong, with separation and the dual work(of identification
Can, the discriminating of the Chinese medicine and its preparation of complicated component is particularly well-suited to, as long as some characteristic spots have repeatability, so that it may as true
Recognize foundation, control can be done in thin layer experiment from chemical monomer, extract, Authentic plant drugs etc. and differentiated.
Chinese Pharmacopoeia 2010, (VI B of annex), there is provided test according to thin-layered chromatography, by being heated to reflux to sample, filter
Cross, filtrate is added on neutral alumina column, collect eluent, be evaporated, residue dissolves, the step such as extraction, washing is completed, used as confession examination
Product solution, carries out point sample.But which needed neutral alumina column, high cost, its chromatogram definition be not high.
The content of the invention
The present invention is in order to overcome above-mentioned not enough problem in prior art, there is provided a kind of side of raising Radix Astragali thin-layer chromatography identification
Method, adds saponification liquor saponification in the residue after reflux and filter, and method is simple, and removal of impurity effect is obvious and improves Radix Astragali first
Definition of the glycosides in chromatogram.
To achieve these goals, a kind of method for improving the identification of Radix Astragali thin-layer chromatography of the present invention is comprised the following steps：
(1) Radix Astragali is ground to into powder first, powder 2-3g is accurately weighed with balance is weighed, add chloroform-just
Butanol 75ml, is heated to reflux, and after 3h, filters, is then evaporated filtrate, and residue adds the KOH- methyl alcohol saponification of 8mL-10mL
Liquid, is placed in 60 DEG C of -65 DEG C of water bath with thermostatic control 30min-40min；Filtration, adds the KOH- methyl alcohol saponification liquors of 8mL-10mL again, puts
100 DEG C of heating water baths flow back 0.5-1h, are evaporated, and the residue 30ml that adds water makes dissolving, moves in separatory funnel；Add 2mL methyl alcohol
After Radix Astragali residue is fully dissolved, after ultrasonic extraction 30min-40min, add ethyl acetate and be extracted twice, each 30mL steams
Dry extract, adds methyl alcohol to be allowed to dissolve, and this is used as supplying sample；
(2) draw the above-mentioned solution of 5 μ l to be put on same silica gel g thin-layer plate respectively, same solvent first launches, further takes out,
Dry again, put under JL-P10A viewboxs or inspect under ultraviolet lamp 365nm, finally take pictures, can be very stable aobvious on thin plate
Clear band is shown, and band presents the uniformity of rule in sample, orange-yellow colour developing is relatively stable in 3 hours, you can
It is judged as the Radix Astragali.
In described step (1), chloroform and n-butanol volume ratio are 2：1.
In described step (1), ultrasonic extraction power is 40-90W, and ultrasonic temperature is 4 DEG C -10 DEG C, is extracted 1-4 time.
Middle KOH- methyl alcohol saponification liquor mass concentration described in described step (1)：20%.
Solvent described in described step (2) is：Chloroform and n-hexane, wherein chloroform：N-hexane=
3：1.
Solvent described in described step (2) is：Petroleum ether and ethyl acetate, wherein petroleum ether：Ethyl acetate=
7：1.
Beneficial effects of the present invention：Compared with prior art, the present invention is added in the residue after first reflux and filter
Good fortune liquid saponification, method are simple, and removal of impurity effect substantially, solves the problems, such as that definition of the Astragaloside IV in chromatogram be not high,
It is a kind of method for accurately, clearly and quickly differentiating the Radix Astragali.
Description of the drawings
Fig. 1 be fluorescent lamp astragalus mongholicus tablet indentification by TLC figure, S- Astragaloside IV reference substances, No. 1-10 be Radix Astragali sample.
Fig. 2 be ultraviolet lamp astragalus mongholicus tablet indentification by TLC figure, S- Astragaloside IV reference substances, No. 1-10 be Radix Astragali sample.
Specific embodiment
Below by way of specific embodiment, the invention will be further described, but the interest field protected by the present invention is not only
It is limited to following examples.
The experimental technique and parameter of the present invention：
1. main material：
2. main agents：
Chloroform, n-butanol, KOH, methyl alcohol, ethyl acetate, n-hexane, petroleum ether, ethyl acetate.Silica gel g thin-layer plate,
Polyamide thin plate, distilled water, 90% ethanol solution etc..
Embodiment 1
(1) 10 kinds of different Radix Astragali materials in the place of production are ground to into powder first, cross the sieve of 200 mesh, balance is accurate with weighing
Powder 2g is weighed, adds volume ratio to be 2：1 chloroform-n-butanol 75ml, is heated to reflux, and after 3h, filters, then will filter
Liquid is evaporated, and residue adds the KOH- methyl alcohol saponification liquors that mass fraction is 20%, 8mL, is placed in 60 DEG C of water bath with thermostatic control 30min；Filter
Cross, add the KOH- methyl alcohol saponification liquors of 8mL again, put 100 DEG C of heating water baths backflow 1h, be evaporated, the residue 30ml that adds water makes dissolving,
Move in separatory funnel；Add after 2mL methyl alcohol makes Radix Astragali residue fully dissolve, ultrasonic extraction 30min, ultrasonic power are 50W,
Ultrasonic temperature is 4 DEG C, after extracting 2 times, adds ethyl acetate and is extracted twice, and each 30mL is evaporated extract, adds methyl alcohol to make
Dissolving, this is used as supplying sample；
(2) draw the above-mentioned solution of 5 μ L to be put on same silica gel g thin-layer plate respectively, same solvent is chloroform：Just oneself
Alkane=3：1, first launch, further take out, then dry, put under JL-P10A viewboxs, finally take pictures, can be very stable on thin plate
Clear band is shown, and band presents the uniformity of rule in sample, orange-yellow colour developing is relatively stable in 3 hours, i.e.,
Can determine whether as the Radix Astragali.Referring to Fig. 1.
Embodiment 2
(1) 10 kinds of different Radix Astragali materials in the place of production are ground to into powder first, cross the sieve of 200 mesh, balance is accurate with weighing
Powder 2g is weighed, adds volume ratio to be 2：1 chloroform-n-butanol 75ml, is heated to reflux, and after 3h, filters, then will filter
Liquid is evaporated, and residue adds the KOH- methyl alcohol saponification liquors that mass fraction is 20%, 8mL, is placed in 60 DEG C of water bath with thermostatic control 30min；Filter
Cross, add the KOH- methyl alcohol saponification liquors of 8mL again, put 100 DEG C of heating water baths backflow 1h, be evaporated, the residue 30ml that adds water makes dissolving,
Move in separatory funnel；Add after 2mL methyl alcohol makes Radix Astragali residue fully dissolve, ultrasonic extraction 30min, ultrasonic power are 50W,
Ultrasonic temperature is 4 DEG C, after extracting 2 times, adds ethyl acetate and is extracted twice, and each 30mL is evaporated extract, adds methyl alcohol to make
Dissolving, this is used as supplying sample；
(2) draw the above-mentioned solution of 5 μ L to be put on same silica gel g thin-layer plate respectively, same solvent is chloroform：Just oneself
Alkane=3：1, first launch, further take out, then dry, inspect under ultraviolet lamp 365nm, finally take pictures, can be very stable on thin plate
Show clear band, and band presents the uniformity of rule in sample, and in 3 hours, orange-yellow colour developing is relatively stable,
The Radix Astragali can be judged as.Referring to Fig. 2.
Embodiment 3
(1) 10 kinds of different Radix Astragali materials in the place of production are ground to into powder first, cross the sieve of 200 mesh, balance is accurate with weighing
Powder 3g is weighed, adds volume ratio to be 2：1 chloroform-n-butanol 75ml, is heated to reflux, and after 3h, filters, then will filter
Liquid is evaporated, and residue adds the KOH- methyl alcohol saponification liquors that mass fraction is 20%, 10mL, is placed in 60 DEG C of water bath with thermostatic control 30min；Filter
Cross, add the KOH- methyl alcohol saponification liquors of 10mL again, put 100 DEG C of heating water baths backflow 1h, be evaporated, residue add water 30ml make it is molten
Solution, moves in separatory funnel；Add after 2mL methyl alcohol makes Radix Astragali residue fully dissolve, ultrasonic extraction 30min, ultrasonic power is
50W, ultrasonic temperature are 4 DEG C, after extracting 2 times, add ethyl acetate and are extracted twice, and each 30mL is evaporated extract, adds first
Alcohol is allowed to dissolve, and this is used as supplying sample；
(2) draw the above-mentioned solution of 5 μ L to be put on same silica gel g thin-layer plate respectively, same solvent is petroleum ether：Acetic acid second
Ester=7：1, first launch, further take out, then dry, put under JL-P10A viewboxs, finally take pictures, can be very stable on thin plate
Clear band is shown, and band presents the uniformity of rule in sample, orange-yellow colour developing is relatively stable in 3 hours, i.e.,
Can determine whether as the Radix Astragali.Clearly chromatogram qualification figure can equally be obtained.
Claims (6)
1. it is a kind of to improve the method that Radix Astragali thin-layer chromatography is identified, it is characterised in that to comprise the following steps：
(1) Radix Astragali is ground to into powder first, powder 2-3g is accurately weighed with balance is weighed, add chloroform-n-butanol
75ml, is heated to reflux, and after 3h, filters, is then evaporated filtrate, and residue adds the KOH- methyl alcohol saponification liquors of 8mL-10mL, puts
In 60 DEG C of -65 DEG C of water bath with thermostatic control 30min-40min；Filtration, adds the KOH- methyl alcohol saponification liquors of 8mL-10mL again, puts 100 DEG C
Heating water bath flows back 0.5-1h, is evaporated, and the residue 30ml that adds water makes dissolving, moves in separatory funnel；Adding 2mL methyl alcohol makes the Radix Astragali
After residue fully dissolves, after ultrasonic extraction 30min-40min, add ethyl acetate and be extracted twice, each 30mL is evaporated extraction
Liquid, adds methyl alcohol to be allowed to dissolve, and this is used as supplying sample；
(2) draw the above-mentioned solution of 5 μ L to be put on same silica gel g thin-layer plate respectively, same solvent first launches, further takes out, then dries in the air
It is dry, put under JL-P10A viewboxs or inspect under ultraviolet lamp 365nm, finally take pictures, on thin plate very it is stable show it is clear
In band, and sample, band presents the uniformity of rule, and in 3 hours, orange-yellow colour developing is relatively stable, that is, be judged as the Radix Astragali.
2. the method that a kind of raising Radix Astragali thin-layer chromatography according to claim 1 is identified, it is characterised in that the step 1)
Middle chloroform is 2 with n-butanol volume ratio：1.
3. the method that a kind of raising Radix Astragali thin-layer chromatography according to claim 1 is identified, it is characterised in that the step 1)
Middle ultrasonic extraction power is 40-90W, and ultrasonic temperature is 4 DEG C -10 DEG C, ultrasonic extraction 1-4 time.
4. the method that a kind of raising Radix Astragali thin-layer chromatography according to claim 1 is identified, it is characterised in that the step 1)
Described in middle KOH- methyl alcohol saponification liquor mass concentration：20%.
5. the method that a kind of raising Radix Astragali thin-layer chromatography according to claim 1 is identified, it is characterised in that the step 2)
In solvent be：Chloroform and n-hexane, wherein chloroform：N-hexane=3：1.
6. the method that a kind of raising Radix Astragali thin-layer chromatography according to claim 1 is identified, it is characterised in that the step 2)
In solvent be：Petroleum ether and ethyl acetate, wherein petroleum ether：Ethyl acetate=7：1.
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| GB2411114B (en) * | 2004-02-19 | 2006-08-16 | Phynova Ltd | A botanical drug or dietary supplement |
| CN1265196C (en) * | 2004-08-30 | 2006-07-19 | 广州中一药业有限公司 | <<Xiaokewan>> medicine quality control method for treating diabetes |
| CN100543470C (en) * | 2005-04-22 | 2009-09-23 | 安徽科创中药天然药物研究所有限责任公司 | A kind of quality determining method of compound pyrrosia leaf particle |
| CN1726990A (en) * | 2005-07-26 | 2006-02-01 | 中国人民解放军军事医学科学院基础医学研究所 | Application and the extraction process of natural Chinese medicinal herb in drug-breaking medicine that contains effective alkaloid |
| CN100594034C (en) * | 2006-07-28 | 2010-03-17 | 贵州泰尔医药研究所 | Blood-sugar lowering A preparation for treating diabetes, its preparation method and quality-control method |
| GB2463531B (en) * | 2008-09-23 | 2012-08-08 | Kenneth Davison | The sub-critical water extraction of Baikal Skullcap |
| WO2010034971A2 (en) * | 2008-09-23 | 2010-04-01 | Gary William Wheatley | Sub-critical water extraction of medicinal plants |
| CN101670041A (en) * | 2009-07-17 | 2010-03-17 | 贵州信邦制药股份有限公司 | Method for controlling quality of astragalus in Chinese medicine preparation |
| CN104165962B (en) * | 2013-05-15 | 2016-03-16 | 广州白云山中一药业有限公司 | The quality determining method of WEINAIAN sheet |
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