CN104133034B - The detection method that a kind of agalloch eaglewood is loose - Google Patents

The detection method that a kind of agalloch eaglewood is loose Download PDF

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CN104133034B
CN104133034B CN201410343365.4A CN201410343365A CN104133034B CN 104133034 B CN104133034 B CN 104133034B CN 201410343365 A CN201410343365 A CN 201410343365A CN 104133034 B CN104133034 B CN 104133034B
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agalloch eaglewood
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ethyl acetate
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CN104133034A (en
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贺敬竹
耿秋霞
***
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Jiangsu 707 Natural Pharmaceutical Co Ltd
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Abstract

The present invention discloses the loose quality determining method of a kind of agalloch eaglewood, the quality determining method that agalloch eaglewood is loose: the indentification by TLC comprising the indentification by TLC magnolia obovata of Ligusticum wallichii.The quality determining method that a kind of agalloch eaglewood provided by the invention is loose, add the thin-layer identification method of Ligusticum wallichii, the bark of official magnolia, the method can evaluate the loose quality of agalloch eaglewood objective, comprehensively and accurately, to the quality of production control process, ensures that the curative effect of product is significant.

Description

The detection method that a kind of agalloch eaglewood is loose
Technical field
The present invention relates to the quality determining method that a kind of agalloch eaglewood is loose, belong to traditional Chinese medicine quality detection field.
Background technology
Along with socioeconomic fast development, the life and work of people also slowly enter allegro state.It is all that fast food solves that young man saves time in order to the Chinese meal that works, and dinner is more and more richer on the contrary, and each side factor causes increasing people to occur inferior health.Eat good of supper and be fullly easy to cause the disease such as abdominal distension, stomachache.The agalloch eaglewood that the natural pharmaceutical Co. Ltd in Jiangsu 707 produces falls apart, traditional Chinese medical science prescription, and thin tableization is stagnant.For invading outside chill, the stagnation of the circulation of vital energy is not transported, and gastral cavity abdomen ruffian is swollen.The prescription that agalloch eaglewood falls apart is agalloch eaglewood 30g, fructus amomi 30g, rhizoma atractylodis 40g, dried immature fruit of citron orange 50g, Fructus Hordei Germinatus (stir-bake to brown) 40g, rascal 50g, perilla leaf 40g, root of Chinese wild ginger 20g, Ligusticum wallichii 40g, balloonflower root 30g, Poria cocos 40g, Radix Glycyrrhizae 10g, cape jasmine 40g, the bark of official magnolia (ginger system) 30g, rhizoma cyperi (vinegar system) 40g, banksia rose 30g, hawthorn (Jiao) 50g, dried orange peel 40g Pogostemon cablin 40g, schizonepeta 40g, root of Dahurain angelica 30g, windproof 20g, peppermint 40g, the tuber of pinellia (ginger system) 40g, root of herbaceous peony 30g, root of kudzu vine 40g.The method for making that agalloch eaglewood falls apart is above 20 Six-elements, is ground into fine powder, sieves, and mixing, to obtain final product.Agalloch eaglewood proterties of faling apart is brown color to tan powder; The special fragrance of tool agalloch eaglewood, mildly bitter flavor.And in existing quality standard, only have proterties and check item, without discrimination method, well product quality can not be controlled.
The agalloch eaglewood Ligusticum wallichii in prescription that falls apart has blood-activating and qi-promoting, wind-expelling pain-stopping effect, is described as " the gas medicine in blood " by ancients.Ligusticum wallichii this product is samphire Ligusticum wallichii ligusticumchuanxionghort. dry rhizome.The joint dish that summer works as on stem is significantly outstanding, and excavates during purplish, and removing silt, shines post-drying, then remove fibrous root.
The agalloch eaglewood bark of official magnolia in prescription of faling apart is the key medicine of abdominal distention caused by treatment dampness, dyspepsia, the stagnation of the circulation of vital energy.The bark of official magnolia (system) this product is the Magnoliacea plant bark of official magnolia magnoliaofficinalisor Magnolia bilola Rehd.etWils. magnoliaofficinalisrehd.etWils.var. bilobarehd.etWils. dry dry hide, Gen Pi and branch skin.4 ~ June strips, Gen Pi and branch skin Directly Dried in Shadow; Dry hide put in boiling water micro-boil after, dark and damp place of banking up, when " sweating " is to endepidermis purpling brown or sepia, steams soft, takes out, is rolled into tubular, dry.
The standard that agalloch eaglewood falls apart is ministerial standard the tenth (standard No.: WS3-B-1944-95), only has microscopical characters in primary standard, does not have other to detect the requirement of compositions.In order to the quality of effective production control process, the curative effect of guarantee product, research and design is needed to go out the detection method that accurately can detect effective constituent in agalloch eaglewood powder preparation.And the function that agalloch eaglewood falls apart cures mainly middle Ligusticum wallichii magnolia obovata effect obviously, in order to control product quality, the thin-layer identification method being badly in need of a kind of Ligusticum wallichii magnolia obovata of invention controls effect and the quality of product.
Summary of the invention
The object of this invention is to provide the quality determining method that a kind of agalloch eaglewood is loose, to improve the loose quality control standard of agalloch eaglewood.The object of the invention is to overcome the deficiencies in the prior art, provide the discrimination method that a kind of Chinese medicine agalloch eaglewood is loose, the method is simple, easy to operate, can differentiate that Chinese medicine agalloch eaglewood falls apart fast and accurately.
Technical scheme of the present invention is such: the quality determining method that a kind of agalloch eaglewood is loose, and the quality determining method that agalloch eaglewood falls apart is as follows:
1) indentification by TLC of Ligusticum wallichii:
The preparation of need testing solution: get agalloch eaglewood and to fall apart 5g, add diethyl ether 30ml, adds hot reflux 1 hour, let cool, and filter, filtrate flings to ether, and residue adds ethyl acetate 5ml makes dissolving, as need testing solution.
The preparation of control medicinal material solution: get Ligusticum wallichii control medicinal material 1g, add diethyl ether 30ml, adds hot reflux 1 hour, lets cool, and filter, filtrate flings to ether, and residue adds ethyl acetate 5ml makes dissolving, makes control medicinal material solution.
Thin-layered chromatography develops the color: according to thin-layered chromatography (" Chinese Pharmacopoeia " version in 2010 annex VI B) test, draw each 5 ~ 10 μ l of above-mentioned two kinds of solution, put respectively in same with sodium carboxymethyl cellulose be binder silica gel g thin-layer plate on, with normal hexane-ethyl acetate (9: 1) for developping agent, launch, take out, dry, inspect under putting ultraviolet lamp (365nm).In test sample chromatogram, on the position corresponding to control medicinal material chromatogram, the fluorescence spot of aobvious same color.
2) indentification by TLC of the bark of official magnolia:
The preparation of need testing solution: get agalloch eaglewood and to fall apart 5g, add methyl alcohol 10ml, close plug, ultrasonic 30 minutes, filter, filtrate is as need testing solution.
The preparation of reference substance solution: get Magnolol and Honokiol reference substance, adds methyl alcohol and makes every 1ml respectively containing the mixed solution of 1mg, product solution in contrast.
Thin-layered chromatography develops the color: according to thin-layered chromatography (" Chinese Pharmacopoeia " version in 2010 annex VI B) test, draw each 5 μ l of above-mentioned two kinds of solution, put respectively in same with sodium carboxymethyl cellulose be binder silica gel g thin-layer plate on, launch at developping agent, take out, dry, spray with 5% vanillin-sulfuric acid solution, be heated to spot development at 105 DEG C clear.In test sample chromatogram, on the position corresponding to reference substance chromatogram, the spot of aobvious same color.
Further improvement, the preparation of need testing solution in the indentification by TLC of described Ligusticum wallichii: get agalloch eaglewood and to fall apart 5g, add diethyl ether 30ml, adds hot reflux 1 hour, let cool, filter, filtrate flings to ether, and residue adds after ethyl acetate 5ml makes dissolving, with ammonia scrubbing, then divide and get ethyl acetate layer, as need testing solution.
In the step of the indentification by TLC of the bark of official magnolia, developping agent is benzene-ethyl acetate is the mixed solution of 27:1 by volume.
In the step of the indentification by TLC of the bark of official magnolia, developping agent is benzene-ethyl acetate-chloroform is the mixed solution of 27:1:1 by volume.
beneficial effect
The quality determining method that agalloch eaglewood of the present invention falls apart is that method is simple, accurately, improves the quality control standard that agalloch eaglewood is loose, add the TLC Identification of Ligusticum wallichii magnolia obovata, ensure that the quality standard level that this compound preparation is higher.
Accompanying drawing explanation
Fig. 1 is the indentification by TLC comparison diagram of the Ligusticum wallichii that the agalloch eaglewood of embodiment 2 in the present invention falls apart.
Fig. 2 is the indentification by TLC comparison diagram of the bark of official magnolia that the agalloch eaglewood of embodiment 3 in the present invention falls apart.
Embodiment
embodiment 1,the preparation that agalloch eaglewood is loose
The recipe quantity that agalloch eaglewood is loose: agalloch eaglewood 30g, fructus amomi 30g, rhizoma atractylodis 40g, dried immature fruit of citron orange 50g, Fructus Hordei Germinatus (stir-bake to brown) 40g, rascal 50g, perilla leaf 40g, root of Chinese wild ginger 20g, Ligusticum wallichii 40g, balloonflower root 30g, Poria cocos 40g, Radix Glycyrrhizae 10g, cape jasmine 40g, the bark of official magnolia (ginger system) 30g, rhizoma cyperi (vinegar system) 40g, banksia rose 30g, hawthorn (Jiao) 50g, dried orange peel 40g Pogostemon cablin 40g, schizonepeta 40g, root of Dahurain angelica 30g, windproof 20g, peppermint 40g, the tuber of pinellia (ginger system) 40g, root of herbaceous peony 30g, root of kudzu vine 40g.
Method for making: above 20 Six-elements, are ground into fine powder, sieve, mixing, to obtain final product.
embodiment 2,the indentification by TLC of Ligusticum wallichii
Prepared by need testing solution: get agalloch eaglewood and to fall apart 5g, add diethyl ether 30ml, adds hot reflux 1 hour, let cool, and filter, filtrate flings to ether, and residue adds ethyl acetate 5ml makes dissolving, as need testing solution.
The agalloch eaglewood of getting 3 different lot numbers that Jiangsu 707 Natural Pharmaceutical Co., Ltd. produces falls apart, according to above-mentioned need testing solution preparation method, and obtained 3 parts of need testing solutions respectively.
Reference substance solution: get Ligusticum wallichii control medicinal material 1g, add diethyl ether 30ml, adds hot reflux 1 hour, lets cool, and filter, filtrate flings to ether, and residue adds ethyl acetate 5ml makes dissolving, medicinal material solution in contrast;
Negative controls: the negative sample 5g getting scarce Ligusticum wallichii, by the preparation method identical with need testing solution, obtained Ligusticum wallichii negative controls respectively.
Thin-layer chromatography: according to thin-layered chromatography (" Chinese Pharmacopoeia " version in 2010 annex VI B) test, draw each 5 μ l of above-mentioned various solution, put respectively in same with sodium carboxymethyl cellulose be binder silica gel g thin-layer plate on, with normal hexane-ethyl acetate by volume 9: 1 for developping agent, launch, take out, dry, inspect under putting ultraviolet lamp (365nm), accompanying drawing 1 is the indentification by TLC comparison diagram of each solution in the present embodiment.Be followed successively by from left to right in figure: negative controls band, Ligusticum wallichii reference substance solution band (middle inspection institute), (Jiangsu 707 Natural Pharmaceutical Co., Ltd. provides need testing solution 1 band, lot number: 20130501), (Jiangsu 707 Natural Pharmaceutical Co., Ltd. provides need testing solution 2 band, lot number: 20130502), (Jiangsu 707 Natural Pharmaceutical Co., Ltd. provides need testing solution 3 band, lot number: 20130503); Silica gel g thin-layer plate (Haiyang Chemical Plant, Qingdao's production) (for thin-layer chromatography), other reagent is AR level.Temperature: 23 DEG C, humidity: 56%; Developping agent: normal hexane-ethyl acetate (9: 1).
Can know from Fig. 1 and find out, in test sample chromatogram, on the position corresponding to reference substance chromatogram, the fluorescence spot of aobvious same color, test illustrates, the good separating effect of developping agent in the present embodiment, Rf value is 0.32, and characteristic spots is clear, rounding, and leaching process is pollution-free simultaneously.
embodiment 3,the indentification by TLC of the bark of official magnolia:
Need testing solution: get agalloch eaglewood and to fall apart 5g, add methyl alcohol 10ml, close plug, ultrasonic 30 minutes, filter, filtrate is as need testing solution; The agalloch eaglewood of getting 3 different lot numbers that Jiangsu 707 Natural Pharmaceutical Co., Ltd. produces falls apart, according to above-mentioned need testing solution preparation method, and obtained 3 parts of need testing solutions respectively.
Reference substance solution: get Magnolol and Honokiol reference substance, adds methyl alcohol and makes every 1ml respectively containing the mixed solution of 1mg, product solution in contrast;
Negative controls: the negative sample 5g getting the scarce bark of official magnolia, by the preparation method identical with need testing solution, obtained bark of official magnolia negative controls respectively.
Thin-layer chromatography: according to thin-layered chromatography (" Chinese Pharmacopoeia " version in 2010 annex VI B) test, draw each 5 μ l of above-mentioned various solution, put respectively in same with sodium carboxymethyl cellulose be binder silica gel g thin-layer plate on, with benzene-methyl alcohol by volume 27: 1 for developping agent, launch, take out, dry, spray, with 5% vanillin-sulfuric acid solution, is heated to spot development at 105 DEG C clear.Accompanying drawing 2 is the indentification by TLC comparison diagram of each solution in the present embodiment.Be followed successively by from left to right in figure: bark of official magnolia negative controls band, magnolol, honokiol reference substance solution band (middle inspection institute), (Jiangsu 707 Natural Pharmaceutical Co., Ltd. provides need testing solution 1 band, lot number: 20130501), (Jiangsu 707 Natural Pharmaceutical Co., Ltd. provides need testing solution 2 band, lot number: 20130502), (Jiangsu 707 Natural Pharmaceutical Co., Ltd. provides need testing solution 3 band, lot number: 20130503); Silica gel g thin-layer plate (Haiyang Chemical Plant, Qingdao's production) (for thin-layer chromatography), other reagent is AR level.Temperature: 23 DEG C, humidity: 56%; Developping agent: benzene-ethyl acetate (27: 1).
Can know from Fig. 2 and find out, in test sample chromatogram, on the position corresponding to reference substance chromatogram, the fluorescence spot of aobvious same color, lacks the bark of official magnolia in negative controls, and corresponding spot disappears.Test illustrates, the good separating effect of developping agent in the present embodiment, and to launch △ Rf value be 0.2 (△ Rf is the difference of Rf value of magnolol, honokiol spot), and characteristic spots is clear, rounding.
embodiment 4,the indentification by TLC of Ligusticum wallichii
Be with the difference of embodiment 2: in the present embodiment, need testing solution is prepared as follows: get agalloch eaglewood and to fall apart 5g, add diethyl ether 30ml, add hot reflux 1 hour, let cool, filter, filtrate flings to ether, residue adds after ethyl acetate 5ml makes dissolving, with ammonia scrubbing, then divide and get ethyl acetate layer, as need testing solution.Other step (preparation of reference substance solution, negative controls preparation, thin-layer chromatography test) is all identical with embodiment 2.The TLC distinguish result display of the Ligusticum wallichii during agalloch eaglewood is fallen apart: in test sample chromatogram, on the position corresponding to reference substance chromatogram, the fluorescence spot of aobvious same color, the good separating effect of developping agent, Rf value is 0.5, moderate, characteristic spots is clear, rounding, and leaching process is pollution-free simultaneously.Test illustrates, after ammonia scrubbing, divides the ethyl acetate layer after getting to be improved through the Rf value launched, is more conducive to detect.
embodiment 5,the indentification by TLC of the bark of official magnolia:
Be with the difference of embodiment 3: except benzene-ethyl acetate-chloroform (27: 1:1) selected by developping agent in the present embodiment, other step (preparation of need testing solution, reference substance solution, negative controls preparation, thin-layer chromatography test) is all identical with embodiment 3.The TLC distinguish result display of the bark of official magnolia during agalloch eaglewood is fallen apart: in test sample chromatogram, on the position corresponding to reference substance chromatogram, the good separating effect of developping agent in the present embodiment, launching △ Rf value is 0.32, spacing before two spots is pulled open further, be more suitable for distinguishing and differentiate, characteristic spots is clear, rounding, and negative controls is without this spot.
reference examples 1
Being prepared as follows of this reference examples need testing solution: get agalloch eaglewood and to fall apart 5g, add diethyl ether 40ml, ultrasonic 30 minutes, filter, filtrate flings to ether, and residue adds ethyl acetate 5ml makes dissolving, as need testing solution.Other step (preparation of reference substance solution, negative controls preparation, thin-layer chromatography test) is all identical with embodiment 2.The TLC distinguish result display of the Ligusticum wallichii in faling apart to agalloch eaglewood: in test sample chromatogram, on the position corresponding to reference substance chromatogram, spot development is unclear, and negative controls is without this spot, in leaching process, ether volatilization is more simultaneously, environmental pollution.
reference examples 2
Being prepared as follows of this reference examples need testing solution: get agalloch eaglewood and to fall apart 5g, add methyl alcohol 20ml, ultrasonic 30 minutes, filter, evaporate to dryness, residue adds ethyl acetate 5ml makes dissolving, as need testing solution.Other step (preparation of reference substance solution, negative controls preparation, thin-layer chromatography test) is all identical with embodiment 2.The TLC distinguish result display of the Ligusticum wallichii during agalloch eaglewood is fallen apart: in test sample chromatogram, on the position corresponding to reference substance chromatogram, spot development is not obvious, and negative controls is without this spot.
reference examples 3
Being prepared as follows of this reference examples need testing solution: get agalloch eaglewood and to fall apart 5g, add methyl alcohol 20ml, 30 minutes, filter, evaporate to dryness, residue adds ethyl acetate 5ml makes dissolving, as need testing solution.Other step (preparation of reference substance solution, negative controls preparation, thin-layer chromatography test) is all identical with embodiment 2.The TLC distinguish result display of the Ligusticum wallichii during agalloch eaglewood is fallen apart: in test sample chromatogram, on the position corresponding to reference substance chromatogram, spot development is not obvious, and negative controls is without this spot.
reference examples 4
Except normal hexane-ethyl acetate (6: 4) selected by developping agent in this reference examples, other step (preparation of need testing solution, reference substance solution, negative controls preparation, thin-layer chromatography test) is all identical with embodiment 2.The TLC distinguish result display of the Ligusticum wallichii during agalloch eaglewood is fallen apart: in test sample chromatogram, on the position corresponding to reference substance chromatogram, launching Rf value is 0.9, and higher, spot development is not obvious, and negative controls is without this spot.
reference examples 5
Except normal hexane-benzene (7: 3) selected by developping agent in this reference examples, other step (preparation of need testing solution, reference substance solution, negative controls preparation, thin-layer chromatography test) is all identical with embodiment 2.The TLC distinguish result display of the Ligusticum wallichii during agalloch eaglewood is fallen apart: in test sample chromatogram, on the position corresponding to reference substance chromatogram, launching Rf value is 0.9, and higher, spot development is not obvious, and negative controls is without this spot.
reference examples 6
Except toluene-ethyl acetate (7: 3) selected by developping agent in this reference examples, other step (preparation of need testing solution, reference substance solution, negative controls preparation, thin-layer chromatography test) is all identical with embodiment 2.The TLC distinguish result display of the Ligusticum wallichii during agalloch eaglewood is fallen apart: in test sample chromatogram, on the position corresponding to reference substance chromatogram, launching Rf value is 0.8, but spot development is imperfect, and negative controls is without this spot.
reference examples 7
Being prepared as follows of this reference examples need testing solution: get agalloch eaglewood and to fall apart 5g, add methyl alcohol 30ml, add hot reflux 30 minutes, filter, evaporate to dryness, residue adds methyl alcohol 5ml makes dissolving, and filtrate is as need testing solution.Other step (preparation of reference substance solution, negative controls preparation, thin-layer chromatography test) is all identical with embodiment 3.The TLC distinguish result display of the bark of official magnolia during agalloch eaglewood is fallen apart: in test sample chromatogram, on the position corresponding to reference substance chromatogram, spot development is unclear, and negative controls is without this spot, and quantity of solvent is large simultaneously, power consumption.
reference examples 8
Being prepared as follows of this reference examples need testing solution: get agalloch eaglewood and to fall apart 5g, add ethanol 20ml, add hot reflux 20 minutes, filter, filtrate is as need testing solution.Other step (preparation of reference substance solution, negative controls preparation, thin-layer chromatography test) is all identical with embodiment 3.The TLC distinguish result display of the bark of official magnolia in faling apart to agalloch eaglewood: in test sample chromatogram, on the position corresponding to reference substance chromatogram, background color is comparatively dark, and spot development is unclear, and negative controls is without this spot.
reference examples 9
Being prepared as follows of this reference examples need testing solution: get agalloch eaglewood and to fall apart 5g, add ethanol 10ml, close plug, ultrasonic 30 minutes, filter, filtrate is as need testing solution.Other step (preparation of reference substance solution, negative controls preparation, thin-layer chromatography test) is all identical with embodiment 3.The TLC distinguish result display of the bark of official magnolia in faling apart to agalloch eaglewood: in test sample chromatogram, on the position corresponding to reference substance chromatogram, background color is comparatively dark, the unclear and negative controls of spot development is without this spot.
reference examples 10
Except benzene-methyl alcohol (15: 1) selected by developping agent in this reference examples, other step (preparation of need testing solution, reference substance solution, negative controls preparation, thin-layer chromatography test) is all identical with embodiment 3.The TLC distinguish result display of the bark of official magnolia in faling apart to agalloch eaglewood: in test sample chromatogram, on the position corresponding to reference substance chromatogram, launching △ Rf value is 0.1, and on the low side, spot development is not obvious, and negative controls is without this spot.
reference examples 11
Except benzene-normal hexane (15: 3) selected by developping agent in this reference examples, other step (preparation of need testing solution, reference substance solution, negative controls preparation, thin-layer chromatography test) is all identical with embodiment 3.The TLC distinguish result display of the bark of official magnolia in faling apart to agalloch eaglewood: in test sample chromatogram, on the position corresponding to reference substance chromatogram, launching △ Rf value is 0.1, but spot development is imperfect, and negative controls is without this spot.
reference examples 12
Except benzene-methyl alcohol (20: 1) selected by developping agent in this reference examples, other step (preparation of need testing solution, reference substance solution, negative controls preparation, thin-layer chromatography test) is all identical with embodiment 3.The TLC distinguish result display of the bark of official magnolia in faling apart to agalloch eaglewood: in test sample chromatogram, on the position corresponding to reference substance chromatogram, launching △ Rf value is 0.1, and on the low side, spot development is imperfect, and negative controls is without this spot.
reference examples 13
Except 10% ethanol solution of sulfuric acid selected by developer in this reference examples, other step (preparation of need testing solution, reference substance solution, negative controls preparation, thin-layer chromatography test) is all identical with embodiment 3.The TLC distinguish result display of the bark of official magnolia during agalloch eaglewood is fallen apart: in test sample chromatogram, on the position corresponding to reference substance chromatogram, spot development is not obvious, and negative controls is without this spot.
reference examples 14
Except 10% sulfuric acid solution selected by developer in this reference examples, other step (preparation of need testing solution, reference substance solution, negative controls preparation, thin-layer chromatography test) is all identical with embodiment 3.The TLC distinguish result display of the bark of official magnolia during agalloch eaglewood is fallen apart: in test sample chromatogram, on the position corresponding to reference substance chromatogram, spot development is not obvious, and negative controls is without this spot.
reference examples 15
Except 10% potassium hydroxide sulfuric acid solution selected by developer in this reference examples, other step (preparation of need testing solution, reference substance solution, negative controls preparation, thin-layer chromatography test) is all identical with embodiment 3.The TLC distinguish result display of the bark of official magnolia during agalloch eaglewood is fallen apart: in test sample chromatogram, on the position corresponding to reference substance chromatogram, spot development is not obvious, and developing time is long simultaneously, and negative controls is without this spot.

Claims (2)

1. the detection method that agalloch eaglewood is loose, is characterized in that the detection method that agalloch eaglewood falls apart comprises the steps:
1) indentification by TLC of Ligusticum wallichii:
The preparation of need testing solution: get agalloch eaglewood and to fall apart 5g, add diethyl ether 30mL, adds hot reflux 1 hour, let cool, filter, filtrate flings to ether, and residue adds ethyl acetate 5mL makes dissolving, as need testing solution;
The preparation of reference substance solution: get Ligusticum wallichii control medicinal material 1g, add diethyl ether 30mL, adds hot reflux 1 hour, lets cool, and filter, filtrate flings to ether, and residue adds ethyl acetate 5mL makes dissolving, medicinal material solution in contrast;
Thin-layer chromatography: draw each 5 μ L of above-mentioned two kinds of solution, put respectively in same with sodium carboxymethyl cellulose be binder silica gel g thin-layer plate on, launch in developping agent, take out, dry, inspect under putting wavelength 365nm ultraviolet lamp, in test sample chromatogram, on the position corresponding to reference substance chromatogram, the fluorescence spot of aobvious same color, described developping agent to be normal hexane-ethyl acetate be by volume 9: 1 mixed solution;
2) indentification by TLC of the bark of official magnolia:
The preparation of need testing solution: get agalloch eaglewood and to fall apart 5g, add methyl alcohol 10mL, close plug, ultrasonic 30 minutes, filter, filtrate is as need testing solution;
The preparation of reference substance solution: get Magnolol and Honokiol reference substance, adds methyl alcohol and makes every 1mL respectively containing the mixed solution of 1mg, product solution in contrast;
Thin-layer chromatography: draw each 5 μ L of above-mentioned two kinds of solution, put respectively in same with sodium carboxymethyl cellulose be binder silica gel g thin-layer plate on, launch in developping agent, take out, dry, spray is with 5% vanillin-sulfuric acid solution, spot development is heated to clear at 105 DEG C, in test sample chromatogram, on the position corresponding to reference substance chromatogram, the spot of aobvious same color, described developping agent is that benzene-ethyl acetate is by volume for the mixed solution of 27:1 or benzene-ethyl acetate-chloroform are the mixed solution of 27:1:1 by volume.
2. the detection method that a kind of agalloch eaglewood according to claim 1 is loose, it is characterized in that: the preparation of need testing solution in the indentification by TLC of described Ligusticum wallichii: get agalloch eaglewood and to fall apart 5g, add diethyl ether 30mL, adds hot reflux 1 hour, let cool, filter, filtrate flings to ether, and residue adds after ethyl acetate 5mL makes dissolving, with ammonia scrubbing, then divide and get ethyl acetate layer, as need testing solution.
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