CN106370766A - Method for identifying atractylodes macrocephala koidz in donkey-hide glue blood-enriching preparation - Google Patents
Method for identifying atractylodes macrocephala koidz in donkey-hide glue blood-enriching preparation Download PDFInfo
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Abstract
The invention provides a method for identifying atractylodes macrocephala koidz in a donkey-hide glue blood-enriching preparation by using a thin layer chromatography method, wherein the thin layer chromatography method comprises: sucking 5-20 [mu]l of a test product solution and 5-20 [mu]l of a reference product solution, respectively loading onto a thin layer chromatography plate, developing by adopting a n-hexane-ethyl acetate-formic acid mixed solution as a developing agent, taking out, carrying out air drying, spraying a coloring agent, placing at a 105 DEG C place, baking until the spot color is clear, placing under a 365 nm ultraviolet lamp, carrying out visual inspection, and in a test product chromatogram, displaying the fluorescent spots having the same color at the positions corresponding to the reference product chromatogram and the reference herb chromatogram. According to the present invention, the method has advantages of simple operation, rapid separation, accurate separation effect, good reproducibility and strong specificity, and provides the basis for the further quality control of the donkey-hide glue blood-enriching preparation.
Description
Technical field
The invention belongs to Chinese medicine preparation detection technique field and in particular in a kind of discriminating 'Lujiaobuxue ' the Rhizoma Atractylodis Macrocephalae method.
Background technology
The Rhizoma Atractylodis Macrocephalae has an invigorating the spleen and benefiting QI, eliminate dampness and have diuretic effect, hidroschesis, antiabortive effect, and for spleen eating less, abdominal distention diarrhea, phlegm retention is dizzy
Throb with fear, edema, spontaneous perspiration, the disease such as frequent fetal movement, is traditional Chinese medical science spleen reinforcing key medicine.The main component of the Rhizoma Atractylodis Macrocephalae has atractylone, atractylodes lactone etc.,
Modern pharmacological research proves, atractylone and lactone constituents are Rhizoma Atractylodis Macrocephalae antiinflammatory, the effective ingredient of spleen invigorating.
In 2010 version " Chinese Pharmacopoeias " one, under the discriminating item of LVJIAO BUXUE KELI, using thin layer chromatography, to Radix Angelicae Sinensis and
The Radix Astragali has carried out qualitative identification, the Rhizoma Atractylodis Macrocephalae is not differentiated, therefore can not preferably control its quality.At present, existing more Chinese medicine
Compound preparation has carried out qualitative identification to the Rhizoma Atractylodis Macrocephalae therein, and the fat TONGMAI KELI that such as disappears (Ma Qiuju, Sun Ping. the matter of the fat TONGMAI KELI that disappears
Amount research on standard [j]. China Dispensary, 2013,35:3325-3327.), ball in fragrant sand reason (gold ring. in fragrant sand reason, ball quality standard improves
Research [j]. China Dispensary, 2010,47:4489-4491.) etc..But the inspection of these tlc methods is known result and is substantially: test sample
In chromatograph, it is on the corresponding position of control medicinal material chromatograph, the speckle of aobvious same color, and should show and have a pink principal spot (grey
Art ketone).
Atractylone belongs to volatile ingredient, and in 'Lujiaobuxue ', Rhizoma Atractylodis Macrocephalae the technique such as need to concentrate, be dried through extracting
Process, the volatile component content in preparation is already very low.In addition, atractylone is very unstable, heat, see that light can be into the Rhizoma Atractylodis Macrocephalae
Ester conversion (Ye Yan, Cheng Xuemei, Gui Xin. thin layer chromatography research [j] of Rhizoma Atractylodis Macrocephalae. when precious traditional Chinese medical science traditional Chinese medicines, 2009,20
(7):1702-1703.).Therefore the method differentiating the Rhizoma Atractylodis Macrocephalae in the even related compound Chinese medicinal preparation of 'Lujiaobuxue ' with atractylone
It is inappropriate.
Content of the invention
The invention provides a kind of method that employing thin layer chromatography differentiates the Rhizoma Atractylodis Macrocephalae in 'Lujiaobuxue '.The method is easy and simple to handle,
Separating effect is quick, accurate, and repeatability is good, and specificity is strong, and the further quality control for 'Lujiaobuxue ' provides foundation,
Technical solution of the present invention is as follows:
A kind of method that employing thin layer chromatography differentiates the Rhizoma Atractylodis Macrocephalae in 'Lujiaobuxue ', comprises the following steps:
(1) preparation of need testing solution:
Take this product 15～25g, grind well, add diethyl ether 50ml, be heated to reflux 1-2 hour, take out, let cool, filtration, filtrate is waved
Dry, residue adds ethyl acetate 1-2ml makes dissolving, as need testing solution；
(2) preparation of control medicinal material solution:
Take Rhizoma Atractylodis Macrocephalae control medicinal material 0.5-1g, same to step (1) method makes control medicinal material solution；
(3) preparation of reference substance solution:
Take atractylodes lactone 0.5-1mg, accurately weighed, plus methanol dissolving make every 1ml contain 0.05-0.1mg atractylodes lactone right
According to product solution；
(4) thin layer chromatography differentiates:
In aspiration step (1)-(3), need testing solution, control medicinal material solution, reference substance solution each 5-20 μ l, put respectively in thin
On laminate, with volume ratio be 8.5～9.5:3.5～4.5:0.1 n-hexane-ethyl acetate-formic acid mixed solution as developing solvent, launch,
Take out, dry, spray, with 40% ethanol solution of sulfuric acid of 2% paradime thylaminobenzaldehyde or 10% ethanol solution of sulfuric acid, puts 105 DEG C
It is baked to spot development clear, put and inspect under 365nm ultra-violet lamp.
In discriminating 'Lujiaobuxue ' of the present invention, the method for the Rhizoma Atractylodis Macrocephalae is preferably:
(1) preparation of need testing solution:
Take this product 20g, grind well, add diethyl ether 50ml, be heated to reflux 1 hour, take out, let cool, filtration, filtrate volatilizes, residual
Slag adds ethyl acetate 1ml makes dissolving, as need testing solution；
(2) preparation of control medicinal material solution:
Take Rhizoma Atractylodis Macrocephalae control medicinal material 0.5g, same to step (1) method makes control medicinal material solution；
(3) preparation of reference substance solution:
Take atractylodes lactone 0.5mg, accurately weighed, plus methanol 10ml dissolving, make every 1ml atractylodes lactone containing 0.05mg
Reference substance solution；
(4) thin layer chromatography differentiates:
In aspiration step (1)-(3), need testing solution, control medicinal material solution, each 5 μ l of reference substance solution, put respectively in thin layer
On plate, with volume ratio be 8.5～9.5:3.5～4.5:0.1 n-hexane-ethyl acetate-formic acid mixed solution as developing solvent, launch, take
Go out, dry, spray, with 40% ethanol solution of sulfuric acid of 2% paradime thylaminobenzaldehyde or 10% ethanol solution of sulfuric acid, puts 105 DEG C of bakings
It is clear to spot development to bake, and puts and inspects under 365nm ultra-violet lamp.
Further, described lamellae is silica gel g lamellae or silica gel gf254Lamellae.
Further, the volume ratio of described developing solvent n-hexane-ethyl acetate-formic acid mixed solution is 9:4:0.1.
Further, described developer is preferably 40% ethanol solution of sulfuric acid of 2% paradime thylaminobenzaldehyde.
In discriminating 'Lujiaobuxue ' of the present invention, 'Lujiaobuxue ' described in the method for the Rhizoma Atractylodis Macrocephalae is granule or capsule or piece
Agent.
In the present invention, " 40% ethanol solution of sulfuric acid of 2% paradime thylaminobenzaldehyde " can be prepared with the following method:
The preparation of (1) 40% ethanol solution of sulfuric acid: measure 40ml sulphuric acid, be slowly added in 60ml ethanol, and be stirred continuously,
Let cool, obtain final product 40% ethanol solution of sulfuric acid；
The preparation of 40% ethanol solution of sulfuric acid of (2) 2% paradime thylaminobenzaldehydes: take paradime thylaminobenzaldehyde 2g, weighed,
Adding in 100ml40% ethanol solution of sulfuric acid makes dissolving, obtains final product.
Beneficial effects of the present invention:
(1) Rhizoma Atractylodis Macrocephalae content in prescription is relatively low, and technique is complex, has water distillation and decocting to boil two operation stages, thin layer reflects
Other complicated, and unstable, between each component, composition interacts, codonolactone etc. in ligustilide such as in Radix Angelicae Sinensis, Radix Codonopsis,
Thus speckle hangover is easily caused when thin layer differentiates, separate not exclusively or occur impurity component interference；The system of test sample in this method
For using " add diethyl ether 50ml, is heated to reflux 1-2 hour, takes out, lets cool, filtration, and filtrate volatilizes, and residue adds ethyl acetate
1-2ml makes dissolving " method, developing solvent is from " normal hexane, ethyl acetate, formic acid are with volume ratio for 8.5～9.5:3.5～4.5:0.1
The mixed solution that obtains of ratio ", so that atractylodes lactone is efficiently separated；
(2) 40% ethanol solution of sulfuric acid of 2% paradime thylaminobenzaldehyde or 10% ethanol solution of sulfuric acid are selected as developer,
Atractylodes lactone speckle can clearly be recognized under ultra-violet lamp (365nm)；
(3) this method is easy and simple to handle, and separating effect is quick, accurate, and repeatability is good, and specificity is strong, is 'Lujiaobuxue '
Further quality control foundation is provided.
Brief description
Fig. 1 is the Rhizoma Atractylodis Macrocephalae thin layer discriminating figure of embodiment 1-3, wherein 1- negative sample；2- Rhizoma Atractylodis Macrocephalae control medicinal material sample；3- reference substance
Atractylodes lactone；4- embodiment 1 need testing solution sample；5- embodiment 2 need testing solution sample；6- embodiment 3 is for examination
Product solution example.
Fig. 2 is the Rhizoma Atractylodis Macrocephalae thin layer discriminating figure of embodiment 4, wherein 1- negative sample；2- Rhizoma Atractylodis Macrocephalae control medicinal material sample；3- reference substance is white
Art lactone；4- embodiment 4 need testing solution sample is 1.；5- embodiment 4 need testing solution sample is 2.；6- embodiment 4 supplies
Test sample solution sample is 3..
Fig. 3 is the Rhizoma Atractylodis Macrocephalae thin layer discriminating figure of embodiment 5, wherein 1- negative sample；2- Rhizoma Atractylodis Macrocephalae control medicinal material sample；3- reference substance is white
Art lactone；4- embodiment 5 need testing solution sample is 1.；5- embodiment 5 need testing solution sample is 2.；6- embodiment 5 supplies
Test sample solution sample is 3..
Fig. 4 is the Rhizoma Atractylodis Macrocephalae thin layer discriminating figure of comparative example 5, wherein 1- negative sample；2- Rhizoma Atractylodis Macrocephalae control medicinal material sample；3- comparative example 5
Need testing solution sample is 1.；4- comparative example 5 need testing solution sample is 2.；5- comparative example 5 need testing solution sample is 3.；6- pair
According to product atractylodes lactone.
Specific embodiment
In following examples and comparative example, taking LVJIAO BUXUE KELI as a example, LVJIAO BUXUE KELI used is " China to 'Lujiaobuxue '
Pharmacopeia " 2010 editions first page 795 LVJIAO BUXUE KELI recorded.Wherein it is respectively provided with a moon in each embodiment or comparative example
Property control sample (is weighed other medical materials of the scarce Rhizoma Atractylodis Macrocephalae, makes the negative control of the scarce Rhizoma Atractylodis Macrocephalae by [prescription] under LVJIAO BUXUE KELI item
Sample, is made in the same way of the negative control solution of the scarce Rhizoma Atractylodis Macrocephalae, with confession by need testing solution preparation method in each embodiment or comparative example
Test sample solution, reference substance solution, control medicinal material solution equal volume amounts point carry out thin layer discriminating on lamellae).By negative control
The thin layer identification result of sample, can be shown that the inventive method feminine gender is noiseless, specificity is strong.
Embodiment 1
A kind of method of the Rhizoma Atractylodis Macrocephalae in discriminating 'Lujiaobuxue ', comprises the following steps:
(1) preparation of need testing solution:
Take this product 20g, grind well, add diethyl ether 50ml, be heated to reflux 1 hour, take out, let cool, filtration, filtrate volatilizes, residual
Slag adds ethyl acetate 1ml makes dissolving, as need testing solution；
(2) preparation of control medicinal material solution:
Take Rhizoma Atractylodis Macrocephalae control medicinal material 0.5g, same to step (1) method makes control medicinal material solution；
(3) preparation of reference substance solution:
Take atractylodes lactone 0.5mg, accurately weighed, plus methanol 10ml dissolving, make every 1ml atractylodes lactone containing 0.05mg
Reference substance solution；
(4) thin layer chromatography differentiates:
In aspiration step (1)-(3), need testing solution, control medicinal material solution, each 5 μ l of reference substance solution, put respectively in silica gel
gf254On lamellae, the n-hexane-ethyl acetate-formic acid mixed solution with volume ratio as 9:4:0.1, as developing solvent, launches,
Take out, dry, spray, with 40% ethanol solution of sulfuric acid of 2% paradime thylaminobenzaldehyde, is put 105 DEG C and is baked to spot development clearly,
Put and inspect under 365nm ultra-violet lamp；In test sample chromatograph, with reference substance chromatograph, the corresponding position of control medicinal material chromatograph,
The fluorescence spot of aobvious same color.
Embodiment 2
A kind of method of the Rhizoma Atractylodis Macrocephalae in discriminating 'Lujiaobuxue ', comprises the following steps:
(1) preparation of need testing solution:
Take this product 15g, grind well, add diethyl ether 50ml, be heated to reflux 2 hours, take out, let cool, filtration, filtrate volatilizes, residual
Slag adds ethyl acetate 1ml makes dissolving, as need testing solution；
(2) preparation of control medicinal material solution:
Take Rhizoma Atractylodis Macrocephalae control medicinal material 0.5g, same to step (1) method makes control medicinal material solution；
(3) preparation of reference substance solution:
Take atractylodes lactone 0.5mg, accurately weighed, plus methanol 10ml dissolving, make every 1ml atractylodes lactone containing 0.05mg
Reference substance solution；
(4) thin layer chromatography differentiates:
In aspiration step (1)-(3), need testing solution, control medicinal material solution, each 5 μ l of reference substance solution, put respectively in silica gel
gf254On lamellae, the n-hexane-ethyl acetate-formic acid mixed solution with volume ratio as 9:4:0.1, as developing solvent, launches,
Take out, dry, spray, with 40% ethanol solution of sulfuric acid of 2% paradime thylaminobenzaldehyde, is put 105 DEG C and is baked to spot development clearly,
Put and inspect under 365nm ultra-violet lamp；In test sample chromatograph, with reference substance chromatograph, the corresponding position of control medicinal material chromatograph,
The fluorescence spot of aobvious same color.
Embodiment 3
A kind of method of the Rhizoma Atractylodis Macrocephalae in discriminating 'Lujiaobuxue ', comprises the following steps:
(1) preparation of need testing solution:
Take this product 25g, grind well, add diethyl ether 50ml, be heated to reflux 1.5 hours, take out, let cool, filtration, filtrate volatilizes,
Residue adds ethyl acetate 2ml makes dissolving, as need testing solution；
(2) preparation of control medicinal material solution:
Take Rhizoma Atractylodis Macrocephalae control medicinal material 0.5g, same to step (1) method makes control medicinal material solution；
(3) preparation of reference substance solution:
Take atractylodes lactone 0.5mg, accurately weighed, plus methanol 10ml dissolving, make every 1ml atractylodes lactone containing 0.05mg
Reference substance solution；
(4) thin layer chromatography differentiates:
In aspiration step (1)-(3), need testing solution, control medicinal material solution, each 5 μ l of reference substance solution, put respectively in silica gel
gf254On lamellae, the n-hexane-ethyl acetate-formic acid mixed solution with volume ratio as 9:4:0.1, as developing solvent, launches,
Take out, dry, spray, with 40% ethanol solution of sulfuric acid of 2% paradime thylaminobenzaldehyde, is put 105 DEG C and is baked to spot development clearly,
Put and inspect under 365nm ultra-violet lamp；In test sample chromatograph, with reference substance chromatograph, the corresponding position of control medicinal material chromatograph,
The fluorescence spot of aobvious same color.
Embodiment 4
A kind of method of the Rhizoma Atractylodis Macrocephalae in discriminating 'Lujiaobuxue ', comprises the following steps:
(1) preparation of need testing solution:
Take this product 25g, grind well, add diethyl ether 50ml, be heated to reflux 1.5 hours, take out, let cool, filtration, filtrate volatilizes,
Residue adds ethyl acetate 2ml makes dissolving, as need testing solution；
(2) preparation of control medicinal material solution:
Take Rhizoma Atractylodis Macrocephalae control medicinal material 1g, same to step (1) method makes control medicinal material solution；
(3) preparation of reference substance solution:
Take atractylodes lactone 1mg, accurately weighed, plus methanol 10ml dissolving, make every 1ml and contain the right of 0.1mg atractylodes lactone
According to product solution；
(4) thin layer chromatography differentiates:
In aspiration step (1)-(3), need testing solution, control medicinal material solution, each 20 μ l of reference substance solution, put respectively in silica gel
On g lamellae, the n-hexane-ethyl acetate-formic acid mixed solution with volume ratio as 8.5:4.5:0.1, as developing solvent, launches,
Take out, dry, spray, with 10% ethanol solution of sulfuric acid, is put 105 DEG C and is baked to spot development clearly, put under 365nm ultra-violet lamp
Inspect；In test sample chromatograph, with reference substance chromatograph, the corresponding position of control medicinal material chromatograph, the fluorescent spot of aobvious same color
Point.
Use step (1) method to prepare three batches of test samples in the present embodiment, carry out thin layer discriminating, that is, the 4- in accompanying drawing 2 is real simultaneously
Apply example 4 need testing solution sample 1., 2., 6- embodiment 4 need testing solution sample is 3. for 5- embodiment 4 need testing solution sample.
Embodiment 5
A kind of method of the Rhizoma Atractylodis Macrocephalae in discriminating 'Lujiaobuxue ', comprises the following steps:
(1) preparation of need testing solution:
Take this product 25g, grind well, add diethyl ether 50ml, be heated to reflux 1.5 hours, take out, let cool, filtration, filtrate volatilizes,
Residue adds ethyl acetate 2ml makes dissolving, as need testing solution；
(2) preparation of control medicinal material solution:
Take Rhizoma Atractylodis Macrocephalae control medicinal material 1g, same to step (1) method makes control medicinal material solution；
(3) preparation of reference substance solution:
Take atractylodes lactone 1mg, accurately weighed, plus methanol 10ml dissolving, make every 1ml and contain the right of 0.1mg atractylodes lactone
According to product solution；
(4) thin layer chromatography differentiates:
In aspiration step (1)-(3), need testing solution, control medicinal material solution, each 10 μ l of reference substance solution, put respectively in silica gel
On g lamellae, the n-hexane-ethyl acetate-formic acid mixed solution with volume ratio as 9.5:3.5:0.1, as developing solvent, launches,
Take out, dry, spray, with 40% ethanol solution of sulfuric acid of 2% paradime thylaminobenzaldehyde, is put 105 DEG C and is baked to spot development clearly,
Put and inspect under 365nm ultra-violet lamp；In test sample chromatograph, with reference substance chromatograph, the corresponding position of control medicinal material chromatograph,
The fluorescence spot of aobvious same color.
Use step (1) method to prepare three batches of test samples in the present embodiment, carry out thin layer discriminating, that is, the 4- in accompanying drawing 3 is real simultaneously
Apply example 5 need testing solution sample 1., 2., 6- embodiment 5 need testing solution sample is 3. for 5- embodiment 5 need testing solution sample.
Comparative example 1
A kind of method of the Rhizoma Atractylodis Macrocephalae in discriminating 'Lujiaobuxue ', comprises the following steps:
Step (1)-(3) with embodiment 1,
Step (4): need testing solution, control medicinal material solution, each 5 μ l of reference substance solution in aspiration step (1)-(3), point
Other point is in silica gel gf254On lamellae, with n-hexane-ethyl acetate-formic acid (volume ratio is as 10:3:0.1) as developing solvent, exhibition
Open, take out, dry, spray, with 40% ethanol solution of sulfuric acid of 2% paradime thylaminobenzaldehyde, is put 105 DEG C and is baked to spot development
Clearly, put and inspect under 365nm ultra-violet lamp；In test sample chromatograph, with reference substance chromatograph, the corresponding position of control medicinal material chromatograph
Put, the rf value of atractylodes lactone speckle is bigger than normal, close to solvent front, be unfavorable for inspecting.
Comparative example 2
A kind of method of the Rhizoma Atractylodis Macrocephalae in discriminating 'Lujiaobuxue ', comprises the following steps:
Step (1)-(3) with embodiment 1,
Step (4): need testing solution, control medicinal material solution, each 5 μ l of reference substance solution in aspiration step (1)-(3), point
Other point is in silica gel gf254On lamellae, with n-hexane-ethyl acetate-formic acid (volume ratio is as 8:5:0.1) as developing solvent, exhibition
Open, take out, dry, spray, with 40% ethanol solution of sulfuric acid of 2% paradime thylaminobenzaldehyde, is put 105 DEG C and is baked to spot development
Clearly, put and inspect under 365nm ultra-violet lamp；In test sample chromatograph, with reference substance chromatograph, the corresponding position of control medicinal material chromatograph
Put, the rf value of atractylodes lactone speckle is less than normal, at initial point, substantially not deployed, is unfavorable for inspecting.
Comparative example 3
A kind of method of the Rhizoma Atractylodis Macrocephalae in discriminating 'Lujiaobuxue ', comprises the following steps:
(1) preparation of need testing solution:
Take this product 20g, grind well, plus chloroform-n-butyl alcohol (2:1) shaking is extracted 3 times, each 40ml, united extraction liquid,
It is evaporated, residue adds methanol 1ml makes dissolving, as need testing solution；
(2) preparation of control medicinal material solution:
Take Rhizoma Atractylodis Macrocephalae control medicinal material 0.5g, same to step (1) method makes control medicinal material solution；
(3) preparation of reference substance solution:
Take atractylodes lactone 0.5mg, accurately weighed, plus methanol 10ml dissolving, make every 1ml atractylodes lactone containing 0.05mg
Reference substance solution；
(4) thin layer chromatography differentiates:
In aspiration step (1)-(3), need testing solution, control medicinal material solution, each 5 μ l of reference substance solution, put respectively in silica gel
gf254On lamellae, with n-hexane-ethyl acetate-formic acid (volume ratio is as 9:4:0.1) as developing solvent, launch, take out, dry in the air
Dry, spray, with 40% ethanol solution of sulfuric acid of 2% paradime thylaminobenzaldehyde, is put 105 DEG C and is baked to spot development clearly, put 365nm
Inspect under ultra-violet lamp；In test sample chromatograph, with reference substance chromatograph, the corresponding position of control medicinal material chromatograph, in test sample
Atractylodes lactone speckle unintelligible it is difficult to detection.
Comparative example 4
A kind of method of the Rhizoma Atractylodis Macrocephalae in discriminating 'Lujiaobuxue ', comprises the following steps:
(1) preparation of need testing solution:
Take this product 20g, grind well, plus chloroform-n-butyl alcohol (2:1) shaking is extracted 3 times, each 40ml, united extraction liquid,
It is evaporated, residue adds methanol 1ml makes dissolving, as need testing solution；
(2) preparation of control medicinal material solution:
Take Rhizoma Atractylodis Macrocephalae control medicinal material 0.5g, same to step (1) method makes control medicinal material solution；
(3) preparation of reference substance solution:
Take atractylodes lactone 0.5mg, accurately weighed, plus methanol 10ml dissolving, make every 1ml atractylodes lactone containing 0.05mg
Reference substance solution；
(4) thin layer chromatography differentiates:
In aspiration step (1)-(3), need testing solution, control medicinal material solution, each 5 μ l of reference substance solution, put respectively in silica gel
On g lamellae, with n-hexane-ethyl acetate-formic acid (volume ratio is as 5:3:0.2) as developing solvent, launch, take out, dry,
Spray, with 40% ethanol solution of sulfuric acid of 2% paradime thylaminobenzaldehyde, is put 105 DEG C and is baked to spot development clearly, put 365nm
Inspect under ultra-violet lamp；In test sample chromatograph, with reference substance chromatograph, the corresponding position of control medicinal material chromatograph, in test sample
Atractylodes lactone speckle unintelligible it is difficult to detection.
Comparative example 5
A kind of method of the Rhizoma Atractylodis Macrocephalae in discriminating 'Lujiaobuxue ', comprises the following steps:
(1) preparation of need testing solution:
Take this product appropriate, grind well, plus take 10ml after appropriate water dissolution, plus dilute hydrochloric acid adjusts ph value 2～3, plus chloroform-just
Butanol (2:1) shaking is extracted 3 times, each 40ml, and united extraction liquid is evaporated, residue adds methanol 1ml makes dissolving, as confession
Test sample solution；
(2) preparation of control medicinal material solution:
Take Rhizoma Atractylodis Macrocephalae control medicinal material 0.5g, same to step (1) method makes control medicinal material solution；
(3) preparation of reference substance solution:
Take atractylodes lactone 0.5mg, accurately weighed, plus methanol 10ml dissolving, make every 1ml atractylodes lactone containing 0.05mg
Reference substance solution；
(4) thin layer chromatography differentiates:
In aspiration step (1)-(3), need testing solution, control medicinal material solution, each 5 μ l of reference substance solution, put respectively in silica gel
On g lamellae, with n-hexane-ethyl acetate-formic acid (volume ratio is as 5:3:0.2) as developing solvent, launch, take out, dry,
Put 105 DEG C and be baked to spot development clearly, put and inspect under 365nm ultra-violet lamp；In test sample chromatograph, with reference substance chromatograph,
On the corresponding position of control medicinal material chromatograph, atractylodes lactone speckle can not detect, and negative sample interference is big.
Use step (1) method to prepare three batches of test samples in this comparative example, carry out thin layer discriminating, i.e. 3- pair in accompanying drawing 4 simultaneously
1., 2., 5- comparative example 5 need testing solution sample is 3. for 4- comparative example 5 need testing solution sample for ratio 5 need testing solution sample.
Claims (5)
1. a kind of using thin layer chromatography differentiate 'Lujiaobuxue ' in the Rhizoma Atractylodis Macrocephalae method it is characterised in that comprising the following steps:
(1) preparation of need testing solution:
Take this product 15～25g, grind well, add diethyl ether 50ml, be heated to reflux 1-2 hour, take out, let cool, filtration, filtrate volatilizes, residual
Slag adds ethyl acetate 1-2ml makes dissolving, as need testing solution；
(2) preparation of control medicinal material solution:
Take Rhizoma Atractylodis Macrocephalae control medicinal material 0.5-1g, same to step (1) method makes control medicinal material solution；
(3) preparation of reference substance solution:
Take atractylodes lactone 0.5-1mg, accurately weighed, plus methanol dissolving make every 1ml contain 0.05-0.1mg atractylodes lactone reference substance
Solution；
(4) thin layer chromatography differentiates:
Need testing solution, control medicinal material solution, reference substance solution equal volume amounts in aspiration step (1)-(3), each absorption 5-20 μ l,
Put respectively on lamellae, with volume ratio be 8.5～9.5:3.5～4.5:0.1 n-hexane-ethyl acetate-formic acid mixed solution for launching
Agent, launches, and takes out, dries, and spray is molten with 40% ethanol solution of sulfuric acid of 2% paradime thylaminobenzaldehyde or 10% sulphuric acid ethanol
Liquid, puts 105 DEG C and is baked to spot development clearly, put and inspect under 365nm ultra-violet lamp.
2. method according to claim 1 is it is characterised in that comprise the following steps:
(1) preparation of need testing solution:
Take this product 20g, grind well, add diethyl ether 50ml, be heated to reflux 1 hour, take out, let cool, filtration, filtrate volatilizes, and residue adds
Ethyl acetate 1ml makes dissolving, as need testing solution；
(2) preparation of control medicinal material solution:
Take Rhizoma Atractylodis Macrocephalae control medicinal material 0.5g, same to step (1) method makes control medicinal material solution；
(3) preparation of reference substance solution:
Take atractylodes lactone 0.5mg, accurately weighed, plus methanol 10ml dissolving, make every 1ml and contain the right of 0.05mg atractylodes lactone
According to product solution；
(4) thin layer chromatography differentiates:
In aspiration step (1)-(3), need testing solution, control medicinal material solution, each 5 μ l of reference substance solution, put respectively on lamellae,
With volume ratio be 8.5～9.5:3.5～4.5:0.1 n-hexane-ethyl acetate-formic acid mixed solution as developing solvent, launch, take out, dry in the air
Dry, spray, with 40% ethanol solution of sulfuric acid of 2% paradime thylaminobenzaldehyde or 10% ethanol solution of sulfuric acid, is put 105 DEG C and is baked to speckle
Point colour developing is clear, puts and inspects under 365nm ultra-violet lamp.
3. method according to claim 1 and 2 is it is characterised in that described lamellae is silica gel g lamellae or silica gel gf254
Lamellae.
4. method according to claim 1 and 2 is it is characterised in that described developing solvent n-hexane-ethyl acetate-formic acid mixing is molten
The volume ratio of liquid is 9:4:0.1.
5. according to claim 1 a kind of employing thin layer chromatography differentiate the Rhizoma Atractylodis Macrocephalae in 'Lujiaobuxue ' method it is characterised in that
Described 'Lujiaobuxue ' is granule or capsule or tablet.
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| CN109507356A (en) * | 2018-12-30 | 2019-03-22 | 鲁南制药集团股份有限公司 | The quality determining method of first luxuriant growth Tongbian capsule |
| CN109580857A (en) * | 2018-12-29 | 2019-04-05 | 北京中研同仁堂医药研发有限公司 | Rhizoma Atractylodis Macrocephalae characteristic spectrum construction method and quality determining method |
| CN113640451A (en) * | 2021-03-25 | 2021-11-12 | 北京中医药大学 | Method for detecting quality standard of plant-derived traditional Chinese medicine in compound donkey-hide gelatin syrup |
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| CN113640451A (en) * | 2021-03-25 | 2021-11-12 | 北京中医药大学 | Method for detecting quality standard of plant-derived traditional Chinese medicine in compound donkey-hide gelatin syrup |
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