CN103399120B - Thin-layer identification method of medicine linearstripe rabdosia herb - Google Patents
Thin-layer identification method of medicine linearstripe rabdosia herb Download PDFInfo
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Abstract
The invention discloses a thin-layer identification method of medicine linearstripe rabdosia herb. The method comprises the steps of pre-treating samples to be identified respectively by adopting the same way to obtain a solution of test articles, pre-treating a control medicine to obtain a control medicine solution, and identifying and analyzing the solution of test articles through thin-layer chromatography, wherein petroleum ether-ethyl acetate is adopted as a developer in the step of identifying and analyzing through thin-layer chromatography, and the volume ratio of petroleum ether to ethyl acetate is (9:1)-(8:2). According to the method, the medicine linearstripe rabdosia herb is identified by thin-layer chromatography; and as the developer for thin-layer chromatography is selected properly, the medicine does not have toxicity and the method is simple and convenient to operate, thus improving the identification efficiency.
Description
Technical field
The present invention relates to the discrimination method of medicinal material rabdosia lophanthide, particularly relate to the thin-layer identification method of a kind of medicinal material rabdosia lophanthide.
Background technology
Chinese medicine rabdosia lophanthide is among the peoplely commonly use herbal medicine, is used for the treatment of damp-heat dysentery, falls and beat that the stasis of blood is swollen, acute icteric hepatitis, acute cholecystitis and other, because being born in small stream limit and the fresh leaf of plant is rubbed rear tool and oozed out the feature of yellow juice and gain the name.Source resource is labiate Rabdosia lophanthoides Rabdosia lophanthoides(Buch.-Ham.ex D.Don) H.Hara and mutation fibre flower Rabdosia amethystoides Rabdosia lophanthoides(Buch.-Ham.ex D.Don) H.Hara var.graciliflora (Benth.) H.Hara.
Existing rabdosia lophanthide discrimination method is generally and first carries out pre-treatment to test sample, then differentiates with thin-layer method, and pre-treating method is generally comparatively loaded down with trivial details.TLC distinguish method is one qualitative identification method fast, and at present, the thin-layer identification method had been reported about rabdosia lophanthide adopts following five kinds of developping agents respectively:
(1) methenyl choloride-butanone-methyl alcohol-formic acid (10:1.5:0.8:0.15);
(2) chloroform-methanol (95:5);
(3) methylene chloride-butanone-methyl alcohol-formic acid (10:1.5:0.8:0.15)
(4) benzene-ethyl acetate (19:1);
(5) cyclohexane-acetone-ethyl acetate (4:2:1);
But these methods above have improves part not to the utmost, if most developping agent is more than two kinds, operate comparatively loaded down with trivial details, and other two relatively simple unfolding conditions " chloroform-methanol (95:5) " and " benzene-ethyl acetate (19:1) " employ the larger organic reagent of toxicity " benzene " and " chloroform ", this is intended to be avoided in new edition pharmacopeia as far as possible.Wherein, the coloration method of the point observed in method 1,2,3,5 comparatively complexity is waited a moment, and the reagent used in method 4 is poisonous.
As can be seen here, how to provide a kind of easy and simple to handle, thin-layer identification method of rabdosia lophanthide of reducing toxicity, this is the current technical issues that need to address in this area.
Summary of the invention
In view of this, the object of the present invention is to provide the thin-layer identification method of a kind of medicinal material rabdosia lophanthide, simplify the operation course, improve the security of operation.
For solving above technical matters, technical scheme of the present invention is:
The thin-layer identification method of a kind of medicinal material rabdosia lophanthide, comprise adopt respectively sample to be identified is carried out in a like fashion pre-treatment obtain need testing solution step, control medicinal material is carried out the step that pre-treatment obtains control medicinal material solution, also comprise the step of need testing solution being carried out to indentification by TLC analysis; Wherein, adopt petroleum ether-ethyl acetate as developping agent in the step of indentification by TLC analysis, the volume ratio of sherwood oil and ethyl acetate is 9:1 ~ 8:2.
Preferably, sample to be identified is carried out the step that pre-treatment obtains need testing solution to be specially: get testing sample powder and add organic solvent supersonic 5 ~ 60 minutes, filter, filtrate evaporate to dryness, adds organic solvent dissolution by residue, as need testing solution.
Preferably, described organic solvent is any one or the two or more potpourri in methyl alcohol, ethanol, ethyl acetate, sherwood oil.
Preferably, the condition of inspecting in the step of described indentification by TLC analysis is: observe under visible ray.
Preferably, sample to be identified is carried out the step that pre-treatment obtains need testing solution to be specially: get testing sample powder and add organic solvent supersonic 10 ~ 40 minutes, filter, filtrate evaporate to dryness, adds organic solvent dissolution by residue, as need testing solution.
Preferably, sample to be identified is carried out the step that pre-treatment obtains need testing solution to be specially: get testing sample powder and add organic solvent supersonic 15 ~ 35 minutes, filter, filtrate evaporate to dryness, adds organic solvent dissolution by residue, as need testing solution.
Preferably, sample to be identified is carried out the step that pre-treatment obtains need testing solution to be specially: get testing sample powder and add organic solvent supersonic 20 ~ 30 minutes, filter, filtrate evaporate to dryness, adds organic solvent dissolution by residue, as need testing solution.
Preferably, sample to be identified is carried out the step that pre-treatment obtains need testing solution to be specially: get testing sample powder and add organic solvent supersonic 30 minutes, filter, filtrate evaporate to dryness, adds organic solvent dissolution by residue, as need testing solution.
Compared with prior art, the thin-layer identification method of medicinal material rabdosia lophanthide of the present invention, adopt thin-layered chromatography to differentiate, the developping agent due to thin-layered chromatography selects sherwood oil and ethyl acetate, and sherwood oil and ethyl acetate do not have toxicity, improves the security of operation; In developping agent, the volume ratio of sherwood oil and ethyl acetate is set to the so appropriate scope of 9:1 ~ 8:2, clear spot can be made to distinguish, make easy and simple to handle, improve identification efficiency.
Further, the condition of inspecting in tlc identification method is observe under visible ray, and this makes discrimination method be more prone to operation, and spot is more obvious, makes discriminating more quick and easy.
Embodiment
In order to make those skilled in the art understand technical scheme of the present invention better, below by specific embodiment, the present invention is described in further detail.
Discrimination method of the present invention comprises the steps:
Sample to be identified and control medicinal material are carried out pre-treatment respectively, then adopts thin-layered chromatography to differentiate.Wherein, the step of pre-treatment can select pre-treatment means of the prior art.
Specifically, discrimination method of the present invention specifically comprises the steps:
1, the preparation of need testing solution:
Get test sample (sample namely to be identified) powder and add organic solvent, ultrasonic 5 ~ 50 minutes, filter, filtrate evaporate to dryness, residue adds organic solvent makes it dissolve, as need testing solution;
2, the preparation of control medicinal material solution: get control medicinal material powder and make control medicinal material solution according to need testing solution preparation method;
3, tlc identification method is adopted to differentiate test sample:
Thin layer condition is as follows:
Thin layer plate: silica G from making sheet, common silica G prefabricated board;
Point sample: need testing solution and control medicinal material solution point sample 2 μ l ~ 6 μ l respectively;
Developping agent: volume ratio is the sherwood oil of 9:1 ~ 8:2: ethyl acetate;
Expansion mode: ascending development;
Inspect: observe under visible ray;
Chromatogram identification: in test sample chromatogram, if on the position corresponding to control medicinal material chromatogram, the spot of aobvious same color, then illustrate that test sample is certified products.
Wherein, the present invention's test material used can select following material, but is not limited to following material during actual enforcement:
Reagent: silica G (lot number 051007) Haiyang Chemical Plant, Qingdao produces, self-control plate gauge lattice 10 × 20mm, thickness 0.5mm; Prefabricated board is that Haiyang Chemical Plant, Qingdao produces, and specification is 10 × 20mm, thickness 0.2 ~ 0.25mm.Other agents useful for same is pure for analyzing.
Control medicinal material: rabdosia lophanthide control medicinal material (lot number 121488-200501), is purchased from Nat'l Pharmaceutical & Biological Products Control Institute.
Test sample: Rabdosia lophanthoides three batches (01,02,03), the place of production is respectively Guangzhou Guangdong, Guangdong Qingyuan); Fine flower Rabdosia amethystoides three batches (01,02,03), the place of production is Guangzhou Guangdong, Fujian Xia Ba, Guangdong peace respectively).
Embodiment one
The discrimination method of the present embodiment comprises the steps:
1, the preparation of need testing solution:
Get test sample powder 1g, add organic solvent 30ml, ultrasonic 30 minutes, filter, filtrate evaporate to dryness, residue adds corresponding solvent 10ml makes dissolving, as need testing solution.
2, the preparation of control medicinal material solution: get control medicinal material powder 1g, make control medicinal material solution according to need testing solution preparation method.
3, tlc identification method is adopted to differentiate test sample:
Thin layer condition is as follows:
Thin layer plate: silica G from making sheet, common silica G prefabricated board;
Point sample: need testing solution and control medicinal material solution is point sample 6 μ l respectively;
Developping agent: volume ratio is sherwood oil and the ethyl acetate of 9:1;
Expansion mode: ascending development;
Inspect: observe under visible ray;
Chromatogram identification: in test sample chromatogram, if on the position corresponding to control medicinal material chromatogram, the spot of aobvious same color, then illustrate that test sample is certified products.
Embodiment two
The discrimination method of the present embodiment comprises the steps:
1, the preparation of need testing solution:
Get test sample powder 1g, add organic solvent 30ml, ultrasonic 5 minutes, filter, filtrate evaporate to dryness, residue adds corresponding solvent 6ml makes dissolving, as need testing solution.
2, the preparation of control medicinal material solution: get control medicinal material powder 1g, make control medicinal material solution according to need testing solution preparation method.
3, tlc identification method is adopted to differentiate test sample:
Thin layer condition is as follows:
Thin layer plate: silica G from making sheet, common silica G prefabricated board;
Point sample: need testing solution and control medicinal material solution is point sample 4 μ l respectively;
Developping agent: volume ratio is sherwood oil and the ethyl acetate of 7:1;
Expansion mode: ascending development;
Inspect: observe under visible ray;
Chromatogram identification: in test sample chromatogram, if on the position corresponding to control medicinal material chromatogram, the spot of aobvious same color, then illustrate that test sample is certified products.
Embodiment three
The discrimination method of the present embodiment comprises the steps:
1, the preparation of need testing solution:
Get test sample powder 1g, add organic solvent 30ml, ultrasonic 30 minutes, filter, filtrate evaporate to dryness, residue adds corresponding solvent 10ml makes dissolving, as need testing solution.
2, the preparation of control medicinal material solution: get control medicinal material powder 1g, make control medicinal material solution according to need testing solution preparation method.
3, tlc identification method is adopted to differentiate test sample:
Thin layer condition is as follows:
Thin layer plate: silica G from making sheet, common silica G prefabricated board;
Point sample: need testing solution and control medicinal material solution is point sample 6 μ l respectively;
Developping agent: volume ratio is sherwood oil and the ethyl acetate of 6:1;
Expansion mode: ascending development;
Inspect: observe under visible ray;
Chromatogram identification: in test sample chromatogram, if on the position corresponding to control medicinal material chromatogram, the spot of aobvious same color, then illustrate that test sample is certified products.
Embodiment four
The discrimination method of the present embodiment comprises the steps:
1, the preparation of need testing solution:
Get test sample powder 1g, add organic solvent 30ml, ultrasonic 40 minutes, filter, filtrate evaporate to dryness, residue adds corresponding solvent 10ml makes dissolving, as need testing solution.
2, the preparation of control medicinal material solution: get control medicinal material powder 1g, make control medicinal material solution according to need testing solution preparation method.
3, tlc identification method is adopted to differentiate test sample:
Thin layer condition is as follows:
Thin layer plate: silica G from making sheet, common silica G prefabricated board;
Point sample: need testing solution and control medicinal material solution is point sample 6 μ l respectively;
Developping agent: volume ratio is sherwood oil and the ethyl acetate of 5:1;
Expansion mode: ascending development;
Inspect: observe under visible ray;
Chromatogram identification: in test sample chromatogram, if on the position corresponding to control medicinal material chromatogram, the spot of aobvious same color, then illustrate that test sample is certified products.
Embodiment five
The discrimination method of the present embodiment comprises the steps:
1, the preparation of need testing solution:
Get test sample powder 1g, add organic solvent 30ml, ultrasonic 50 minutes, filter, filtrate evaporate to dryness, residue adds corresponding solvent 10ml makes dissolving, as need testing solution.
2, the preparation of control medicinal material solution: get control medicinal material powder 1g, make control medicinal material solution according to need testing solution preparation method.
3, tlc identification method is adopted to differentiate test sample:
Thin layer condition is as follows:
Thin layer plate: silica G from making sheet, common silica G prefabricated board;
Point sample: need testing solution and control medicinal material solution is point sample 6 μ l respectively;
Developping agent: volume ratio is sherwood oil and the ethyl acetate of 8:2;
Expansion mode: ascending development;
Inspect: observe under visible ray;
Chromatogram identification: in test sample chromatogram, if on the position corresponding to control medicinal material chromatogram, the spot of aobvious same color, then illustrate that test sample is certified products.
Compliance test result:
Different developping agent ratio, is petroleum ether-ethyl acetate (95:5) respectively relatively below; Petroleum ether-ethyl acetate (9:1); Petroleum ether-ethyl acetate (8:2); Petroleum ether-ethyl acetate (7:3).
Result shows: petroleum ether-ethyl acetate (95:5) and petroleum ether-ethyl acetate (7:3) are the expansion limit at two ends respectively, petroleum ether-ethyl acetate (95:5) starts the existence showing yellow spotting, overlaps to petroleum ether-ethyl acetate (7:3) punctation and blue spot.Wherein with petroleum ether-ethyl acetate (9:1) ~ petroleum ether-ethyl acetate (8:2) degree of separation better (i.e. technical scheme of the present invention), chromatogram is clear.
Below be only the preferred embodiment of the present invention, it should be pointed out that above-mentioned preferred implementation should not be considered as limitation of the present invention, protection scope of the present invention should be as the criterion with claim limited range.For those skilled in the art, without departing from the spirit and scope of the present invention, can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (8)
1. the thin-layer identification method of a medicinal material rabdosia lophanthide, it is characterized in that, comprise adopt respectively sample to be identified is carried out in a like fashion pre-treatment obtain need testing solution step, control medicinal material is carried out the step that pre-treatment obtains control medicinal material solution, also comprise the step of need testing solution being carried out to indentification by TLC analysis; Wherein, adopt silica gel plate as thin layer plate in the step of indentification by TLC analysis, adopt petroleum ether-ethyl acetate as developping agent, the volume ratio of sherwood oil and ethyl acetate is 9:1 ~ 8:2.
2. the thin-layer identification method of medicinal material rabdosia lophanthide as claimed in claim 1, it is characterized in that, sample to be identified is carried out the step that pre-treatment obtains need testing solution to be specially: get testing sample powder and add organic solvent supersonic 5 ~ 50 minutes, filter, filtrate evaporate to dryness, residue is added organic solvent dissolution, as need testing solution.
3. the thin-layer identification method of medicinal material rabdosia lophanthide as claimed in claim 2, it is characterized in that, described ultrasonic time organic solvent and described dissolving time organic solvent be any one or two or more potpourris in methyl alcohol, ethanol, ethyl acetate, sherwood oil.
4. the thin-layer identification method of medicinal material rabdosia lophanthide as claimed in claim 2, it is characterized in that, the condition of inspecting in the step of described indentification by TLC analysis is: observe under visible ray.
5. the thin-layer identification method of medicinal material rabdosia lophanthide as claimed in claim 1, it is characterized in that, sample to be identified is carried out the step that pre-treatment obtains need testing solution to be specially: get testing sample powder and add organic solvent supersonic 10 ~ 40 minutes, filter, filtrate evaporate to dryness, residue is added organic solvent dissolution, as need testing solution.
6. the thin-layer identification method of medicinal material rabdosia lophanthide as claimed in claim 5, it is characterized in that, sample to be identified is carried out the step that pre-treatment obtains need testing solution to be specially: get testing sample powder and add organic solvent supersonic 15 ~ 35 minutes, filter, filtrate evaporate to dryness, residue is added organic solvent dissolution, as need testing solution.
7. the thin-layer identification method of medicinal material rabdosia lophanthide as claimed in claim 5, it is characterized in that, sample to be identified is carried out the step that pre-treatment obtains need testing solution to be specially: get testing sample powder and add organic solvent supersonic 20 ~ 30 minutes, filter, filtrate evaporate to dryness, residue is added organic solvent dissolution, as need testing solution.
8. the thin-layer identification method of medicinal material rabdosia lophanthide as claimed in claim 1, it is characterized in that, sample to be identified is carried out the step that pre-treatment obtains need testing solution to be specially: get testing sample powder and add organic solvent supersonic 30 minutes, filter, filtrate evaporate to dryness, residue is added organic solvent dissolution, as need testing solution.
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