CN109682919A - A kind of discrimination method improving pseudo-ginseng based on thin-layer chromatography - Google Patents
A kind of discrimination method improving pseudo-ginseng based on thin-layer chromatography Download PDFInfo
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Abstract
The present invention provides a kind of discrimination method that pseudo-ginseng is improved based on thin-layer chromatography, this method comprises the following steps: step 1) takes medicinal powder 0.5g, it is accurately weighed, it sets in stuffed conical flask, is subject to water saturated n-butanol 20mL, close plug, ultrasound, filtering, the water that filtrate adds 40mL to be saturated with n-butanol, it shakes up, is layered；N-butanol liquid is taken, is evaporated, residue adds methanol 1mL to make to dissolve, as test solution；Step 2) separately takes ginsenoside Rg1's reference substance, ginsenoside Re's reference substance, ginsenoside Rb1's reference substance and notoginsenoside R reference substance, adds methanol that reference substance solution is made；Step 3) is tested according to thin-layered chromatography, draws each l μ l of above two solution, is put respectively on same silica gel g thin-layer plate, using methylene chloride-dehydrated alcohol-water-glacial acetic acid as solvent, is unfolded, takes out, dry；It is clear that step 4) spray color developing agent is heated to spot Xian Se Cheongju.
Description
Technical field
The invention belongs to the field of quality control of pseudo-ginseng, and in particular to the mirror of pseudo-ginseng is improved based on thin-layer chromatography
Other method.
Background technique
Radix Notoginseng is the drying of Araliaceae (Araliaceae) plant Radix Notoginseng Panaxnotoginseng (Burk.) F.H.Chen
Root and rhizome, the quality in " Chinese Pharmacopoeia " version in 2015 there are many method for medicinal material control.Wherein thin layer identifies to be easy to
The color atlas that visual pattern compares identifies, so have its unique advantages.
Pseudo-ginseng discrimination method disclosed in " Chinese Pharmacopoeia " are as follows: take this product powder 0.5g, add water 5 to drip, stir evenly, then be subject to
Water saturated n-butanol 5mL, close plug shake 10 minutes, place 2 hours, and centrifugation is taken supernatant, 3 times of amounts is added to be saturated with n-butanol
Water, shake up, placement makes layering (when necessary be centrifuged), takes n-butanol layer, is evaporated, and residue adds methanol 1mL to make to dissolve, as examination
Product solution.Separately take ginsenoside Rg1's reference substance, ginsenoside Re's reference substance, ginsenoside Rb1's reference substance and notoginsenoside R pair
According to product, add methanol that every lmL is made respectively containing the mixed solution of 0.5mg, as reference substance solution.According to thin-layered chromatography (general rule 0502)
Test, draws each l μ l of above two solution, is put respectively on same silica gel g thin-layer plate, with chloroform-ethyl acetate-first
10 DEG C of alcohol-water (15:40:22:10) lower layer's solution arranged below is solvent, is unfolded, and takes out, dries, and is sprayed with sulfuric acid solution
(1 → 10) it is clear to be heated to spot Xian Se Cheongju at 105 DEG C.In sample chromatogram, at the position corresponding to the chromatogram of the reference substance, show
The spot of same color；It sets and is inspected under ultraviolet lamp (365nm), show identical fluorescence spot.
There is sample when doing pseudo-ginseng and Chinese patent drug experiment containing pseudo-ginseng in the above method and control point fails point
From result；One long-term unsolved problem existing for the chromatographic condition that more document report Chinese Pharmacopoeias record is the failure to
The characteristic component notoginsenoside R of ginsenoside Re and Radix Notoginseng is separated.In addition, in discrimination method disclosed in " Chinese Pharmacopoeia "
One of solvent chloroform be precursor chemicals, and unfolding condition need to be at 10 DEG C hereinafter, not easy to control；In addition
Color developing agent sulfuric acid solution is not also volatile.
Summary of the invention
Based on the above technical problem, the present invention provides one kind, and the safety is improved, extraction time shortens and solves ginseng soap
Glycosides Re and notoginsenoside R can not separation problem the discrimination method that pseudo-ginseng is improved based on thin-layer chromatography, this method includes such as
Lower step:
Step 1) takes medicinal powder 0.5g, accurately weighed, sets in stuffed conical flask, is subject to water saturated n-butanol 20mL,
Close plug, ultrasound, filtering, the water that filtrate adds 40mL to be saturated with n-butanol shake up, and are layered；N-butanol liquid is taken, is evaporated, residue adds first
Alcohol 1mL makes to dissolve, as test solution；
Step 2) separately takes ginsenoside Rg1's reference substance, ginsenoside Re's reference substance, ginsenoside Rb1's reference substance and Radix Notoginseng
Saponin(e R1 reference substance adds methanol that every 1mL is made respectively containing the mixed solution of 2mg, as reference substance solution；
Step 3) is tested according to thin-layered chromatography, is drawn each l μ l of above two solution, is put respectively in same silica gel g thin-layer plate
On, using methylene chloride-dehydrated alcohol-water-glacial acetic acid as solvent, it is unfolded, takes out, dry；
Step 4) sprays color developing agent, and it is clear to be heated to spot Xian Se Cheongju, in sample chromatogram, in position corresponding with reference substance chromatography
It sets, shows the spot of same color；It sets and is inspected under ultraviolet light (365nm), show identical fluorescence spot.
The present invention using methylene chloride system substitute chloroform system, and methylene chloride be methane chloride Poisoning most
It is small, personnel safety can be improved, the another sample treatment that changes can effectively shorten extraction time, improve efficiency, and after improving
Method efficiently and conveniently solve the problems, such as that ginsenoside Re separates with notoginsenoside R.
It is further preferred that in the step 3) in solvent methylene chloride, dehydrated alcohol, water, glacial acetic acid volume ratio
Example is 14:9:1:0.5.
It is further preferred that spraying 10% ethanol solution of sulfuric acid in the step 4), spot Xian Se Cheongju being heated at 105 DEG C
It is clear
It is further preferred that the ultrasonic time is 30min in the step 1).
It is further preferred that the method being layered in the step 1) is to place layering or centrifuge separation.
Compared with existing pseudo-ginseng discrimination method, the invention has the following advantages:
1. Radix Notoginseng discrimination method disclosed in raw medicine allusion quotation is that shaking is extracted, and shaking extraction time is 10 minutes 2 hours, then is shaken
Liquid separation extraction is shaken, extracting method is now changed to ultrasonic treatment 30 minutes, then shakes liquid separation extraction, extraction time will shorten 1.5
Hour, extraction time has been saved, has been improved efficiency.
2. original method solvent is that chloroform -10 DEG C of acetate-methanol-water (15:40:22:10) is arranged below
Lower layer's solution need to be unfolded at 10 DEG C or less, and 4 points of controls are not easy to separate (see Fig. 1,2), and wherein chloroform is easy system poison
Chemicals is harmful to the human body.Solvent is now changed to methylene chloride-dehydrated alcohol-water-glacial acetic acid (14:9:1:0.5), this exhibition
Opening agent can be unfolded under ambient temperature and moisture, and 4 points of controls are separated clearly (see Fig. 3,4), and all reagents are not that easy system poisons
Product, support personnel's safety.
3. it is 0.5mg that the mixing of raw medicine allusion quotation, which compares each control content, point sample amount is 1 μ l, needs 4 μ of point sample in right practical operation
L, control point is just clear, therefore control is changed to the respectively mixing containing 2mg and is compareed, and 1 μ l of point sample reduces point sample amount in this way, can make a little
Sampling point is not easy to expand.
4. original method uses sulfuric acid solution (1 → 10) for color developing agent, color developing agent is now changed to 10% ethanol solution of sulfuric acid, this
The more former color developing agent of color developing agent is more volatile.
Detailed description of the invention
The TLC chromatogram of Fig. 1 and Fig. 2 difference raw medicine allusion quotation discrimination method reference substance and pseudo-ginseng；
Fig. 3 and Fig. 4 is the TLC chromatogram of discrimination method reference substance provided by the invention and pseudo-ginseng.
Specific embodiment
Ginsenoside Rg1's reference substance, ginsenoside Re's reference substance, ginsenoside Rb1's reference substance and Radix Notoginseng used herein
Saponin(e R1 reference substance is identical as used in " Chinese Pharmacopoeia " version in 2015, and should explain according to this publication.
Unless stated otherwise, all technical and scientific terms used herein has and the common skill in field belonging to the present invention
Art personnel are generally understood identical meaning.
A kind of discrimination method that pseudo-ginseng is improved based on thin-layer chromatography of embodiment 1
Take three parts of sample pseudo-ginsengs, the extract containing pseudo-ginseng, the extract for lacking pseudo-ginseng；Repeat following
Test procedure；
Step 1) takes powder 0.5g, accurately weighed, sets in stuffed conical flask, is subject to water saturated n-butanol 20mL, close plug,
Ultrasound 30 minutes, filtering, the water that filtrate adds 40mL to be saturated with n-butanol shake up, and placement makes to be layered, and takes n-butanol liquid, is evaporated, residual
Slag adds methanol 1mL to make to dissolve, as test solution；
Step 2) separately takes ginsenoside Rg1's reference substance, ginsenoside Re's reference substance, ginsenoside Rb1's reference substance and Radix Notoginseng
Saponin(e R1 reference substance adds methanol that every 1mL is made respectively containing the mixed solution of 2mg, as reference substance solution；
Step 3) is tested according to thin-layered chromatography (general rule 0502), is drawn each l μ l of above two solution, is put respectively in same silicon
On glue G lamellae, with methylene chloride-dehydrated alcohol-water-glacial acetic acid (14:9:1:0.5) for solvent, it is unfolded, takes out, dry；
Step 4) spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to spot Xian Se Cheongju at 105 DEG C, as shown in figure 3, test sample
In chromatography, at the position corresponding to the chromatogram of the reference substance, the spot of same color is shown；It sets and is inspected under ultraviolet light (365nm), show phase
Same fluorescence spot (referring to Fig. 4).
As a result as shown in Figure 3 and Figure 4,1. panax mixeds control；2. pseudo-ginseng；3. the extract containing pseudo-ginseng；4.
Lack the extract of pseudo-ginseng.1. representing ginsenoside Rg1；2. notoginsenoside R；3. representing ginsenoside Re；4. representing ginseng
Saponin(e Rb1.Can be seen that method provided in this embodiment from the clear spot degree and Rf value Rf of each sample can be fast
Speed identifies pseudo-ginseng, and 4 points of ginsenoside Rg1, notoginsenoside R, ginsenoside Re and ginsenoside Rb1 control separation
Clearly；It can also carry out efficiently separating identification particularly with ginsenoside Re-notoginsenoside R that raw medicine allusion quotation can not separate.It is right
As usual
Pseudo-ginseng discrimination method disclosed in reference " Chinese Pharmacopoeia " 2015 editions, takes 4 parts of sample pseudo-ginsengs, medicines containing Radix Notoginseng
The extract of material, the extract for lacking pseudo-ginseng；Repeat following tests step；
Step 1) takes this product powder 0.5g, adds water 5 to drip, stirs evenly, then be subject to water saturated n-butanol 5mL, close plug, shaking 10
Minute, place 2 hours, centrifugation takes supernatant, add 3 times to measure the water that be saturated with n-butanol, shake up, placement make to be layered (when necessary from
The heart), n-butanol layer is taken, is evaporated, residue adds methanol 1mL to make to dissolve, as test solution；
Step 2) separately takes ginsenoside Rg1's reference substance, ginsenoside Re's reference substance, ginsenoside Rb1's reference substance and Radix Notoginseng
Saponin(e R1 reference substance adds methanol that every lmL is made respectively containing the mixed solution of 0.5mg, as reference substance solution；
Step 3) is tested according to thin-layered chromatography (general rule 0502), is drawn each l μ l of above two solution, is put respectively in same silicon
On glue G lamellae, it is with chloroform -10 DEG C of acetate-methanol-water (15:40:22:10) lower layer's solution arranged below
Solvent is unfolded, and takes out, dries；
Step 4) is sprayed with sulfuric acid solution (1 → 10), and it is clear that spot Xian Se Cheongju is heated at 105 DEG C.In sample chromatogram, with
On the corresponding position of reference substance chromatography, the spot of same color is shown；It sets and is inspected under ultraviolet lamp (365nm), show identical fluorescence
Spot.
As a result as depicted in figs. 1 and 2,1- lacks the extract of pseudo-ginseng, the control of 2- panax mixed, 3- pseudo-ginseng, 4-
Extract containing pseudo-ginseng, 5- methanol solvate.1. representing ginsenoside Rg1；2. representing ginsenoside Re- notoginsenoside R；
3. representing ginsenoside Rb1.It is smaller to can be seen that separation degree by clear spot degree and Rf value Rf from figure, and identify
It is more difficult；And ginsenoside Re-notoginsenoside R can not be separated.
Although this specification has had been transmitted through embodiment and the invention of front is described in detail, cited embodiment is only
Preferred embodiment.Those skilled in the art can the spirit and scope protected without departing substantially from invention herein described and claimed it
It is inside changed and corrects；Using described above, those skilled in the art should be able to easily implement the present invention.
Claims (5)
1. a kind of discrimination method for improving pseudo-ginseng based on thin-layer chromatography, it is characterised in that: this method comprises the following steps:
Step 1) takes medicinal powder 0.5g, accurately weighed, sets in stuffed conical flask, is subject to water saturated n-butanol 20mL, close plug,
Ultrasound, filtering, the water that filtrate adds 40mL to be saturated with n-butanol shake up, and are layered；N-butanol liquid is taken, is evaporated, residue adds methanol 1mL
Make to dissolve, as test solution；
Step 2) separately takes ginsenoside Rg1's reference substance, ginsenoside Re's reference substance, ginsenoside Rb1's reference substance and notoginsenoside
R1 reference substance adds methanol that every 1mL is made respectively containing the mixed solution of 2mg, as reference substance solution；
Step 3) is tested according to thin-layered chromatography, draws each l μ l of above two solution, is put respectively on same silica gel g thin-layer plate, with
Methylene chloride-dehydrated alcohol-water-glacial acetic acid is solvent, is unfolded, and takes out, dries；
Step 4) sprays color developing agent, and it is clear to be heated to spot Xian Se Cheongju, in sample chromatogram, in position corresponding with reference substance chromatography
On, show the spot of same color；It sets and is inspected under ultraviolet light (365nm), show identical fluorescence spot.
2. the discrimination method according to claim 1 for improving pseudo-ginseng based on thin-layer chromatography, it is characterised in that: the step
It is rapid 3) in methylene chloride in solvent, dehydrated alcohol, water, glacial acetic acid volume ratio be 14:9:1:0.5.
3. the discrimination method according to claim 1 for improving pseudo-ginseng based on thin-layer chromatography, it is characterised in that: the step
It is rapid 4) in, spray 10% ethanol solution of sulfuric acid, it is clear that spot Xian Se Cheongju is heated at 105 DEG C.
4. the discrimination method according to claim 1 for improving pseudo-ginseng based on thin-layer chromatography, it is characterised in that: the step
It is rapid 1) in, the ultrasonic time be 30min.
5. the discrimination method according to claim 1 for improving pseudo-ginseng based on thin-layer chromatography, it is characterised in that: the step
Rapid 1) the middle method being layered is to place layering or be centrifugated.
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Application publication date: 20190426 |