CN113514597B - Thin-layer chromatography identification method of gastrodia tuber dizziness relieving granule - Google Patents
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Classifications
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/90—Plate chromatography, e.g. thin layer or paper chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
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- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
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Abstract
The invention belongs to the technical field of analysis of traditional Chinese medicine preparations, and discloses a quality detection method of gastrodia elata vertigo-ning granules, which is based on the national standard YBZ-01412006-2009Z of gastrodia elata vertigo-ning granules, combines the product prescription and the preparation process characteristics, and increases the thin-layer identification of raw medicinal materials alisma orientale and bighead atractylodes rhizome in the prescription; meanwhile, the thin-layer identification method of the white paeony root and the dried orange peel is optimized and upgraded. The quality detection method is simple to operate, reliable, accurate, good in reproducibility and high in specificity. The technical scheme of the invention can evaluate the quality of the gastrodia elata vertigo on the basis of combining the existing quality detection method of the gastrodia elata vertigo, and ensure the stability of the quality of the product and the safety and effectiveness of clinical medication, thereby better meeting the needs of medical treatment and market.
Description
Technical Field
The invention belongs to the technical field of traditional Chinese medicines, and particularly relates to a quality control method of gastrodia elata vertigo-ning particles, in particular to a thin-layer chromatography identification method of gastrodia elata vertigo-ning particles.
Background
Vertigo (Dizziness) is a movement illusion caused by spatial orientation disorder, is a subjective reaction generated in the cerebral cortex of a patient due to balance disorder, is often expressed as rotation of visual objects, rotation of the visual objects, floating feeling and the like, is sometimes accompanied with symptoms such as nausea, vomiting, hyperhidrosis and the like, and is a common syndrome in clinic. It has been reported that vertigo has a prevalence of 0.5% in China, which is inferior to fever and pain. And the incidence of dizziness is continuously increasing along with the aging of population and the change of life habits. The etiology and classification of dizziness and its complexity are generally classified into 2 major categories, vestibular systemic dizziness, common etiology is vertebrobasilar artery insufficiency, cerebral infarction, cerebral hemorrhage, brain tumor, meniere's disease, vestibular neuritis, benign paroxysmal positional dizziness, otitis media, etc.; non-systemic vertigo, common causes include hypertension, hypotension, arrhythmia, endocrine disorders, infection, neurosis, etc.
The Gastrodia elata vertigo-treating homologous products comprise Gastrodia elata vertigo-treating mixture and Gastrodia elata vertigo-treating granule, are classical prescriptions for treating vertigo, are prepared from Gastrodia elata, ramulus Uncariae cum Uncis, rhizoma alismatis, pinellia ternate, rhizoma Atractylodis Macrocephalae, poria cocos, radix paeoniae alba, caulis Bambusae in Taenia, ligusticum wallichii, radix Glycyrrhizae, dried orange peel, ginger and the like, have the effects of eliminating phlegm and relieving dizziness, harmonizing stomach and preventing vomiting, are used for vertigo, nausea, vomiting, pale tongue and white and slippery coating, and are especially suitable for Meniere's disease (Meniere disease), labyrinthine, inner ear drug poisoning, positional vertigo, motion sickness and the like, and have definite curative effects. In the recipe, gastrodia tuber and uncaria stem with hooks for calming endogenous wind and relieving dizziness, pinellia tuber for drying dampness and resolving phlegm, white atractylodes rhizome for strengthening spleen and stomach, bamboo shavings and rhizoma alismatis for clearing heat and resolving phlegm, poria cocos and liquorice for strengthening spleen and stomach, dried orange peel for regulating qi and resolving phlegm, ligusticum wallichii for promoting blood circulation and activating qi-flowing, white peony root for calming liver and relieving pain, nourishing blood and regulating menstruation, ginger for relieving vomiting and resolving phlegm and dispelling cold, so that 'no phlegm does not cause dizziness', so that the recipe is suitable for drying dampness and resolving phlegm, promoting blood circulation and activating qi-flowing, and the medicines have the effects of eliminating phlegm and relieving dizziness and harmonizing stomach and relieving vomiting.
The current domestic market varieties are Gastrodia elata vertigo-ning granule and Gastrodia elata vertigo-ning mixture, the prescription of Gastrodia elata vertigo-ning mixture and preparation of Gastrodia elata vertigo-ning mixture are carried in a fourteenth book (number: WS 3 -B-2662-97) of a standard Chinese medicinal prescription preparation of Ministry of health, and are produced by pharmaceutical factories of Shanxi Chinese medicine college. Gastrodia elata vertigo treating granule is produced by Lunan Sanpu pharmaceutical Co., ltd, and has current standard of national standard YBZ-01412006-2009Z, and is prepared by identifying ramulus Uncariae cum Uncis, radix Paeoniae alba, rhizoma Ligustici Chuanxiong, glycyrrhrizae radix, hesperidin, etc. by thin layer chromatography, and measuring gastrodin content by high performance liquid chromatography.
CN1616013a discloses a traditional Chinese medicine composition for treating dizziness, a preparation method and a quality control method thereof, identification of uncaria, white paeony root, szechuan lovage rhizome and liquorice in the preparation is disclosed, and high performance liquid chromatography is used for content determination of gastrodin and paeoniflorin. However, the gastrodia tuber vertigo treating granule has complex medicine taste and less medicine taste identified by the current standard, so that the identification of other medicine taste needs to be developed as the improvement and supplement of the existing detection method so as to provide a more comprehensive and accurate quality control method and improve the quality control level of the gastrodia tuber vertigo treating granule.
Disclosure of Invention
In view of the above shortcomings of the prior art, the invention aims to provide a method for identifying gastrodia elata vertigo-ning particle thin-layer chromatography, which is used as a perfect and supplement of the existing detection method to improve the quality detection level of gastrodia elata vertigo-ning particles.
A thin-layer identification method of Gastrodia elata vertigo treating granule is characterized in that qualitative identification is carried out on Gastrodia elata vertigo treating preparation, and whether the preparation contains ramulus Uncariae cum Uncis, radix Paeoniae alba, pericarpium Citri Tangerinae, alismatis rhizoma or Atractylodis rhizoma as raw materials is judged.
The thin-layer chromatography identification of the white paeony root and dried orange peel raw medicinal materials comprises the following steps of:
(1) Taking gastrodia elata vertigo treating particles, adding methanol for ultrasonic treatment, filtering, evaporating filtrate, dissolving residues in water, shaking and extracting by diethyl ether, discarding diethyl ether phase, extracting by water saturated n-butanol solution, evaporating n-butanol phase, dissolving residues in water, loading to a polyamide column, washing with water until the residues are colorless, and collecting effluent; eluting the polyamide column with 70% ethanol, and collecting eluate for use; evaporating the water washing effluent to dryness, and dissolving the residue with methanol to obtain a sample solution;
(2) Dissolving paeoniflorin reference in methanol to obtain reference solution;
(3) Sucking the sample solution in the step (1) and the reference substance solution in the step (2) to be respectively spotted on the same silica gel G thin layer, developing by taking chloroform-ethyl acetate-methanol-formic acid as developing agent, taking out, airing, spraying 5% vanillin sulfuric acid solution, and drying at 105 ℃ until the spots are clear in color development; in the chromatogram of the sample, spots with the same color appear at the positions corresponding to the chromatogram of the reference sample;
(4) Taking 70% ethanol eluent under the white paeony root item in the step (2), evaporating to dryness, and dissolving residues with methanol to obtain a sample solution;
(5) Taking hesperidin reference substance, adding methanol to prepare saturated solution as reference substance solution;
(6) Taking the sample solution and the reference substance solution according to a thin layer chromatography test, respectively spotting the sample solution and the reference substance solution on a silica gel G thin layer plate prepared from the same 0.1% sodium hydroxide, developing by using ethyl acetate-methanol-water as developing agent, taking out, airing, spraying an aluminum trichloride test solution, and inspecting under a 365nm ultraviolet lamp; in the sample chromatogram, fluorescent spots of the same color appear at positions corresponding to the control chromatogram.
In one embodiment, a thin layer identification method of white peony root medicinal materials in gastrodia tuber vertigo granule comprises the following steps:
(1) Taking 5g of gastrodia elata vertigo granule sample, adding 80ml of methanol for ultrasonic extraction for 60min, filtering, evaporating filtrate to dryness, adding 20ml of water into residues, dissolving, shaking and extracting with diethyl ether for 2 times, 20ml of diethyl ether each time, discarding diethyl ether phase, extracting with water saturated n-butanol solution for 3 times, 20ml of water saturated n-butanol solution each time, merging n-butanol phases, evaporating to dryness, adding 5ml of water into residues for dissolution, loading the residues on a treated polyamide column (30-60 meshes, column height of 15cm and inner diameter of 1.5 cm), washing with water until the residues are colorless, and collecting effluent; eluting the polyamide column with 50ml of 70% ethanol, and collecting eluent for later use; evaporating the water washing effluent to dryness, and dissolving the residue with 1ml of methanol to obtain a sample solution;
(2) Dissolving paeoniflorin reference in methanol to obtain reference solution containing 1mg paeoniflorin per 1 ml;
(3) Taking 10 mu l of each of the sample solution and the reference substance solution according to a thin layer chromatography test, respectively spotting on the same silica gel G thin layer, developing by taking chloroform-ethyl acetate-methanol-formic acid with the volume ratio of 20:2:5:0.1 as developing agent, taking out, airing, spraying 5% vanillin sulfuric acid solution, and drying at 105 ℃ until the spots develop clearly; spots of the same color appear in the sample chromatogram at positions corresponding to those of the control chromatogram.
In one embodiment, the thin-layer chromatography identification method of the dried orange peel medicinal materials in the gastrodia elata vertigo-treating granule comprises the following steps:
(1) Taking 70% ethanol eluent under the condition of [ white peony root identification ], evaporating to dryness, and adding 1ml of methanol into residues to dissolve, so as to obtain a sample solution;
(2) Adding methanol into hesperidin reference substance to obtain saturated solution as reference substance solution;
(3) According to a thin layer chromatography test, 10 mu l of each of the sample solution and the reference solution is absorbed and respectively spotted on the same silica gel G thin layer plate prepared by 0.1% sodium hydroxide, and the mixture is spread by taking ethyl acetate-methanol-water with the volume ratio of 100:17:13 as a developing agent, taken out, dried, sprayed with an aluminum trichloride test solution and inspected under an ultraviolet lamp (365 nm). In the sample chromatogram, fluorescent spots of the same color appear at positions corresponding to the control chromatogram.
The method for identifying the rhizoma alismatis comprises the steps of respectively dispensing the rhizoma gastrodiae vertigo-ning particles and a reference substance 2, 3-acetyl alisol B on a silica gel G thin layer plate after extraction, and identifying by taking cyclohexane-trichloromethane-methyl acetate as a developing agent.
Specifically, the method for identifying the rhizoma alismatis comprises the following steps:
(1) Taking gastrodia elata vertigo treating particles, adding absolute ethyl alcohol, carrying out ultrasonic extraction, filtering, evaporating filtrate to dryness, dissolving residues in water, extracting ethyl acetate, taking an ethyl acetate phase, fully washing with ammonia test solution, discarding ammonia solution, washing with water, evaporating ethyl acetate solution to dryness, and dissolving residues in methanol to serve as a sample solution;
(2) Adding methanol into 2, 3-acetyl alisol B reference substance to obtain reference substance solution;
(3) Sucking the sample solution and the reference substance solution, respectively spotting on the same silica gel G thin layer plate, spreading with cyclohexane-chloroform-methyl acetate as developing agent, taking out, air drying, spraying 10% sulfuric acid ethanol solution, and drying at 105deg.C until the color of spots is clear.
Preferably, the volume ratio of the developing agent is cyclohexane: trichloromethane: methyl acetate=3-5:1-3:3-5.
In one embodiment, the thin-layer chromatography identification method of the rhizoma alismatis medicinal material in the gastrodia elata vertigo-ning particles comprises the following steps of:
(1) Taking 8g of gastrodia elata vertigo treating granule sample, adding 50ml of absolute ethyl alcohol, carrying out ultrasonic extraction for 30min, filtering, evaporating filtrate to dryness, adding 20ml of water into residues, dissolving the residues, extracting with ethyl acetate for 2 times, 30ml each time, combining ethyl acetate solutions, fully washing with ammonia test solution for 2 times, 30ml each time, discarding ammonia solution, washing with water for 3 times, 30ml each time, evaporating ethyl acetate solution to dryness, and dissolving residues with 2ml of methanol to serve as a sample solution;
(2) Adding methanol into 23-acetyl alisol B reference substance to prepare a reference substance solution containing about 1mg of 23-acetyl alisol B reference substance per 1 ml;
(3) According to a thin layer chromatography test, 10 mu l of each of the test sample solution and the reference substance solution is absorbed and respectively spotted on the same silica gel G thin layer plate, and the cyclohexane-chloroform-methyl acetate with the volume ratio of 4:2:4 is used as a developing agent to develop, taken out, dried, sprayed with 10% sulfuric acid ethanol solution and baked at 105 ℃ until the spot color is clear. Spots of the same color appear in the sample chromatogram at positions corresponding to the control chromatogram.
The thin-layer identification of rhizoma Gastrodiae is carried out by ultrasonic treating rhizoma Gastrodiae with giddiness, hydrolyzing precipitate with acid to obtain sample solution, taking amino acid as reference substance, and identifying with n-butanol-acetic acid as developing agent according to thin-layer chromatography test;
The amino acid is one or more of aspartic acid, threonine, serine, glutamic acid, glycine, alanine, cysteine, valine, methionine, isoleucine, leucine, tyrosine, phenylalanine, lysine, histidine or arginine.
Preferably, the thin-layer identification of bighead atractylodes rhizome comprises the following steps:
(1) Grinding rhizoma Gastrodiae vertigo granule sample, adding methanol, ultrasonic treating, centrifuging, removing methanol solution, dissolving precipitate with hydrochloric acid solution, transferring into ampoule bottle, sealing, hydrolyzing in boiling water bath, filtering, evaporating filtrate, and dissolving with methanol to obtain sample solution;
(2) Weighing amino acid reference substance, adding methanol to prepare reference substance solution;
(3) Sucking the sample solution and the reference substance solution, respectively spotting on the same silica gel G thin layer plate, spreading with water saturated n-butanol-acetic acid as developing agent, taking out, air drying, spraying 0.5% ninhydrin ethanol solution, and drying at 105deg.C until the color of spots is clear.
Preferably, the volume ratio of the developing agent is water saturated n-butanol: acetic acid=7-9:2-4.
In one embodiment, a thin-layer chromatography identification method of bighead atractylodes rhizome medicinal materials in gastrodia elata vertigo-ning particles comprises the following steps:
(1) Taking 1g of gastrodia elata vertigo treating granule sample, grinding, adding 10ml of methanol, carrying out ultrasonic treatment for 30min, centrifuging, removing methanol liquid, dissolving precipitate with 4ml of 6mol/L hydrochloric acid solution, transferring into a 5ml ampoule bottle, sealing, placing into a boiling water bath, boiling for 1 hour, taking out, and adding 4ml of water. Shaking, filtering, washing the filter and filter residue with a small amount of water, evaporating the filtrate to dryness, and dissolving the residue with 10ml of methanol to obtain a sample solution;
(2) Adding methanol into glycine reference substance to obtain 1mg solution per 1ml, and taking as reference substance solution;
(3) According to a thin layer chromatography test, 5 mu l of each of the two solutions is adsorbed, the two solutions are respectively spotted on the same silica gel G thin layer plate, water saturated n-butanol-acetic acid with the volume ratio of 8:3 is used as a developing agent, and the developing agent is developed, taken out, dried, sprayed with 0.5% ninhydrin ethanol solution and baked at 105 ℃ until the spots develop clearly. Spots of the same color appear in the sample chromatogram at positions corresponding to those of the control chromatogram.
Compared with the prior art, the quality detection method of the gastrodia elata vertigo treating granule has the following beneficial effects:
(1) The invention adds thin layer identification of rhizoma alismatis and bighead atractylodes rhizome serving as raw materials in the prescription based on the quality standard of the traditional gastrodia tuber vertigo-ning particles, upgrades and perfects the identification method of white paeony root and dried orange peel, thereby realizing qualitative identification of 8 raw materials in the preparation under the condition of combining the prior art, perfecting the thin layer identification system of the gastrodia tuber vertigo-ning particles and achieving the aim of multi-component joint control.
(2) In order to simplify the analysis operation steps, the invention adopts a step-by-step sample preparation method for TLC identification of both white paeony root and dried orange peel by comparing and analyzing the polarity and physicochemical properties of chemical components of prescription medicinal materials and repeatedly searching and verifying, and particularly adopts a polyamide column 70% ethanol eluent in the TLC identification of white paeony root as a starting material for TLC identification of dried orange peel.
(3) The thin-layer identification method for four medicinal materials in the gastrodia elata vertigo treating granule has the advantages of simplicity in operation, no negative interference and clear and distinguishable color development.
(4) The invention optimizes and upgrades the existing quality standard, establishes a scientific, reasonable and feasible component identification method, newly adds TLC identification of 2 medicinal materials of rhizoma alismatis and bighead atractylodes rhizome, improves and improves the existing preparation detection method, achieves the aim of multi-component combined control, can effectively detect the dosage condition of gastrodia elata vertigo and ensures the clinical curative effect of the preparation.
Drawings
Fig. 1: the thin-layer identification map of uncaria in the embodiment 1, wherein 2 is uncaria control medicine, and 1,3 and 4 are gastrodia elata vertigo-ning particles;
fig. 2: embodiment 2a thin-layer identification pattern of radix Paeoniae alba, wherein 2 is paeoniflorin reference substance, 1,3,4 is rhizoma Gastrodiae vertigo treating granule;
Fig. 3: embodiment 3a thin-layer identification map of rhizoma Ligustici Chuanxiong, wherein 2 is rhizoma Ligustici Chuanxiong reference medicine, 1,3,4 are rhizoma Gastrodiae vertigo treating granule;
fig. 4: embodiment 4a thin-layer identification map of Glycyrrhrizae radix, wherein 2 is Glycyrrhrizae radix reference medicine, and 1,3,4 are rhizoma Gastrodiae vertigo treating granule;
fig. 5: embodiment 5 a thin-layer identification map of pericarpium Citri Tangerinae, wherein 2 is hesperidin reference substance, and 1,3,4 are rhizoma Gastrodiae vertigo treating granule;
Fig. 6: example 6 thin-layer identification map of Alismatis rhizoma, wherein 2 is 23-acetyl alisol B reference substance, and 1,3,4 are rhizoma Gastrodiae granule for vertigo;
Fig. 7: example 7 thin-layer identification map of Alismatis rhizoma, wherein 4 is 23-acetyl alisol B reference substance, and 1,2,3 are rhizoma Gastrodiae vertigo treating granule;
fig. 8: example 8 thin-layer chromatography for identifying Atractylodis rhizoma, wherein 4 is glycine reference substance, and 1,2, and 3 are Gastrodia elata vertigo treating granule;
Fig. 9: example 9A thin-layer identification map of Atractylodis rhizoma, wherein 1 is glycine reference substance, and 2,3,4 are Gastrodia elata vertigo treating granule.
Detailed Description
The following detailed description of the present invention is provided in connection with specific embodiments, it being understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention. The specific techniques or conditions are not identified in the examples and are conventional in the art or are in accordance with the product specifications. The reagents and apparatus used are commercially available.
In this example, the gastrodia elata vertigo granule (national medicine standard Z20060009) was produced by Lunan Torpedo pharmaceutical Co., ltd.
Example 1 Uncaria identification
(1) Taking 8g of the product powder, adding 60ml of ethyl acetate and 6ml of concentrated ammonia water, carrying out ultrasonic extraction for 30min, taking the supernatant, evaporating to dryness, and adding 1ml of ethyl acetate into the residue to dissolve the residue to obtain a sample solution.
(2) The preparation method comprises the steps of preparing a medicinal solution of uncaria control by adding 20ml of ethyl acetate and 2ml of concentrated ammonia water into 2g of uncaria control medicinal powder.
(3) Taking 10 μl of each of the sample solution and the control medicinal solution, respectively spotting on the same silica gel G thin layer plate, spreading with lower solution of dichloromethane-methanol-ammonia water (volume ratio of 20:1:1) as developing agent, taking out, air drying, spraying modified bismuth potassium iodide test solution, and inspecting under fluorescent lamp, wherein the chromatogram is shown in figure 1; in the chromatogram of the test sample, the same orange-red spots appear at the positions corresponding to the chromatograms of the control medicinal materials.
EXAMPLE 2 identification of white peony root
(1) Taking 5g of gastrodia elata vertigo granule sample, adding 80ml of methanol for ultrasonic extraction for 60min, filtering, evaporating filtrate to dryness, adding 20ml of water into residues, dissolving, shaking and extracting with diethyl ether for 2 times, 20ml of diethyl ether each time, discarding diethyl ether phase, extracting with water saturated n-butanol solution for 3 times, 20ml of water saturated n-butanol solution each time, merging n-butanol phases, evaporating to dryness, adding 5ml of water into residues for dissolution, loading the residues on a treated polyamide column (30-60 meshes, column height of 15cm and inner diameter of 1.5 cm), washing with water until the residues are colorless, and collecting effluent; eluting the polyamide column with 50ml of 70% ethanol, and collecting eluent for later use; the effluent of the water washing was evaporated to dryness, and the residue was dissolved in 1ml of methanol to give a sample solution.
(2) Dissolving paeoniflorin reference in methanol to obtain reference solution containing 1mg paeoniflorin per 1 ml;
(3) Taking 10 μl of each of the sample solution and the reference solution according to thin layer chromatography, respectively spotting on the same silica gel G thin layer, spreading with chloroform-ethyl acetate-methanol-formic acid with volume ratio of 20:2:5:0.1 as developing agent, taking out, air drying, spraying 5% vanillin sulfuric acid solution, baking at 105deg.C until the spot color is clear, and the chromatogram is shown in figure 2; spots of the same color appear in the sample chromatogram at positions corresponding to those of the control chromatogram.
EXAMPLE 3 identification of Ligusticum chuanxiong
(1) Taking 5g of gastrodia tuber vertigo treating particles, adding 40 ethyl acetate, carrying out ultrasonic extraction for 20min, filtering, evaporating filtrate on a water bath, and dissolving residues with 0.05ml of ethyl acetate to obtain a sample solution;
(2) Preparing a control medicinal solution by taking 0.05g of a control medicinal material of ligusticum wallichii in the same way;
(3) According to thin layer chromatography test, sucking 10 μl of each of the sample solution and the control medicinal solution, respectively spotting on the same silica gel G thin layer plate, spreading with petroleum ether (60-90deg.C) -ethyl acetate with volume ratio of 10:1 as developing agent, taking out, air drying, and inspecting under 365nm of ultraviolet lamp, wherein the chromatogram is shown in figure 3; in the chromatogram of the test sample, fluorescent spots with the same color appear at the positions corresponding to the chromatogram of the control medicinal material.
EXAMPLE 4 identification of Glycyrrhiza uralensis
(1) Taking 5g of gastrodia elata vertigo granule sample, adding 40ml of water-saturated n-butanol solution, carrying out ultrasonic extraction for 30min, filtering, evaporating filtrate to dryness, dissolving residues in water, adding the residues on a treated polyamide column (30-60 meshes, column height of 15cm and inner diameter of 1.5 cm), washing with water to be colorless, eluting with 30ml of 70% ethanol, collecting eluent, evaporating to dryness in water bath, and dissolving residues in 1ml of methanol to obtain a sample solution;
(2) Adding 30ml of water saturated n-butanol solution into 0.5g of Glycyrrhrizae radix reference medicinal material, ultrasonically extracting for 20min, filtering, evaporating filtrate, and dissolving residue with 1ml of methanol to obtain reference medicinal material solution;
(3) According to the thin-layer chromatography test, 10 μl of each of the sample solution and the control medicinal solution is absorbed and respectively spotted on the same silica gel G thin-layer plate, dichloromethane-methanol-water with the volume ratio of 40:10:1 is used as developing agent, and the developing agent is developed, taken out, dried, sprayed with 10% sulfuric acid ethanol solution, heated at 105deg.C until the color of the spots becomes clear, the chromatogram is shown in figure 4, and spots with the same color are respectively displayed on the positions corresponding to the chromatogram of the control medicinal solution in the sample chromatogram.
EXAMPLE 5 identification of dried orange peel
(1) Taking 70% ethanol eluent under the identification item of white paeony root in example 2, evaporating to dryness, and adding 1ml of methanol into residues to dissolve, thereby obtaining a sample solution;
(2) Adding methanol into hesperidin reference substance to obtain saturated solution as reference substance solution;
(3) According to a thin layer chromatography test, sucking 10 μl of each of the sample solution and the reference solution, respectively spotting on the same silica gel G thin layer plate prepared from 0.1% sodium hydroxide, spreading with ethyl acetate-methanol-water as developing agent at volume ratio of 100:17:13, taking out, air drying, spraying aluminum trichloride solution, and placing under ultraviolet lamp (365 nm) for detection, wherein the chromatogram is shown in FIG. 5; in the sample chromatogram, fluorescent spots of the same color appear at positions corresponding to the control chromatogram.
EXAMPLE 6 identification of Alisma orientale
(1) Taking 8g of gastrodia elata vertigo treating granule sample, adding 50ml of absolute ethyl alcohol, carrying out ultrasonic extraction for 30min, filtering, evaporating filtrate to dryness, adding 20ml of water into residues, dissolving the residues, extracting with ethyl acetate for 2 times, 30ml each time, combining ethyl acetate solutions, fully washing with ammonia test solution for 2 times, 30ml each time, discarding ammonia solution, washing with water for 3 times, 30ml each time, evaporating ethyl acetate solution to dryness, and dissolving residues with 2ml of methanol to serve as a sample solution;
(2) Adding methanol into 23-acetyl alisol B reference substance to prepare a reference substance solution containing about 1mg of 23-acetyl alisol B reference substance per 1 ml;
(3) According to the thin layer chromatography test, 10 μl of each of the sample solution and the reference solution is absorbed and respectively spotted on the same silica gel G thin layer plate, and the mixture is spread, taken out and dried by taking cyclohexane-chloroform-methyl acetate with the volume ratio of 4:2:4 as a developing agent, sprayed with 10% sulfuric acid ethanol solution, baked at 105 ℃ until the spots are clearly developed, and the chromatogram is shown in figure 6. Spots of the same color appear in the sample chromatogram at positions corresponding to the control chromatogram.
EXAMPLE 7 identification of Alisma orientale
(1) Taking 2g of gastrodia elata vertigo treating particles, adding 20ml of ethyl acetate, carrying out ultrasonic treatment for 30min, filtering, placing filtrate on an alumina column (200-300 meshes, 5g, 1cm in inner diameter and dry column packing), eluting with 10ml of ethyl acetate, collecting eluent, evaporating to dryness, and adding 1ml of ethyl acetate into residues to dissolve, thereby obtaining a sample solution;
(2) Adding methanol into 23-acetyl alisol B reference substance to prepare a reference substance solution containing about 1mg of 23-acetyl alisol B reference substance per 1 ml;
(3) Taking 5 μl of each of the sample solution and the reference solution, respectively spotting on the same silica gel H thin layer plate, and taking cyclohexane-ethyl acetate with volume ratio of 1:1 as developing agent; spreading, taking out, air drying, spraying 5% silicotungstic acid ethanol solution, heating at 105deg.C until the spots are clear, and the chromatogram is shown in figure 7.
EXAMPLE 8 identification of Atractylodis Macrocephalae
(1) Taking 1g of gastrodia elata vertigo treating granule sample, grinding, adding 10ml of methanol, carrying out ultrasonic treatment for 30min, centrifuging, removing methanol liquid, dissolving precipitate with 4ml of 6mol/L hydrochloric acid solution, transferring into a 5ml ampoule bottle, sealing, placing into a boiling water bath, boiling for 1 hour, taking out, and adding 4ml of water. Shaking, filtering, washing the filter and filter residue with a small amount of water, evaporating the filtrate to dryness, and dissolving the residue with 10ml of methanol to obtain a sample solution;
(2) Adding methanol into glycine reference substance to obtain 1mg solution per 1ml, and taking as reference substance solution;
(3) Referring to thin layer chromatography test, adsorbing 5 μl of each of the above two solutions, respectively spotting on the same silica gel G thin layer plate, spreading with water saturated n-butanol-acetic acid with volume ratio of 8:3 as developing agent, taking out, air drying, spraying 0.5% ninhydrin ethanol solution, baking at 105deg.C until the spot color is clear, and the chromatogram is shown in figure 8; spots of the same color appear in the sample chromatogram at positions corresponding to those of the control chromatogram.
EXAMPLE 9 identification of Atractylodis Macrocephalae
(1) Taking 1g of gastrodia elata vertigo treating granule sample, grinding, adding 10ml of methanol, carrying out ultrasonic treatment for 30min, centrifuging, removing methanol liquid, dissolving precipitate with 4ml of 6mol/L hydrochloric acid solution, transferring into a 5ml ampoule bottle, sealing, placing into a boiling water bath, boiling for 1 hour, taking out, and adding 4ml of water. Shaking, filtering, washing the filter and filter residue with a small amount of water, evaporating the filtrate to dryness, and dissolving the residue with 10ml of methanol to obtain a sample solution;
(2) Adding methanol into glycine reference substance to obtain 1mg solution per 1ml, and taking as reference substance solution;
(3) Referring to thin layer chromatography test, adsorbing 5 μl of each of the above two solutions, respectively spotting on the same silica gel G thin layer plate, spreading with n-butanol-acetic acid-water with volume ratio of 8:3:1 as developing agent, taking out, air drying, spraying 2% vanillin sulfuric acid solution as developer, baking at 105deg.C until the spots develop clearly, and the chromatogram is shown in figure 9; spots of the same color appear in the sample chromatogram at positions corresponding to those of the control chromatogram.
Claims (1)
1. A thin-layer identification method of gastrodia tuber vertigo treating granules is characterized by qualitatively identifying gastrodia tuber vertigo treating granules and judging whether the granules contain white paeony root, dried orange peel, rhizoma alismatis and bighead atractylodes rhizome raw medicinal materials or not, and comprises the following steps of:
A. Thin layer chromatography identification of white peony root and dried orange peel raw material medicines:
(1) Taking gastrodia elata vertigo treating particles, adding methanol for ultrasonic treatment, filtering, evaporating filtrate, dissolving residues in water, shaking and extracting by diethyl ether, discarding diethyl ether phase, extracting by water saturated n-butanol solution, evaporating n-butanol phase, dissolving residues in water, loading to a polyamide column, washing with water until the residues are colorless, and collecting effluent; eluting the polyamide column with 70% ethanol, and collecting eluate for use; evaporating the water washing effluent to dryness, and dissolving the residue with methanol to obtain a sample solution;
(2) Dissolving paeoniflorin reference in methanol to obtain reference solution;
(3) Drawing the sample solution in the step (1) and the reference substance solution in the step (2) to be respectively spotted on the same silica gel G thin layer, developing by taking chloroform-ethyl acetate-methanol-formic acid with the volume ratio of 20:2:5:0.1 as developing agent, taking out, airing, spraying 5% vanillin sulfuric acid solution, and drying at 105 ℃ until spots are clear in color development; in the chromatogram of the sample, spots with the same color appear at the positions corresponding to the chromatogram of the reference sample;
(4) Taking 70% ethanol eluent collected in the step (1), evaporating to dryness, and dissolving residues with methanol to obtain a sample solution;
(5) Taking hesperidin reference substance, adding methanol to prepare saturated solution as reference substance solution;
(6) According to a thin layer chromatography test, sucking the sample solution in the step (4) and the reference solution in the step (5), respectively spotting on a silica gel G thin layer plate prepared by the same 0.1% sodium hydroxide, developing by taking ethyl acetate-methanol-water with the volume ratio of 100:17:13 as developing agent, taking out, airing, spraying an aluminum trichloride test solution, and inspecting under a 365nm ultraviolet lamp; in the chromatogram of the sample, fluorescent spots with the same color appear at the positions corresponding to the chromatogram of the reference substance;
B. thin layer chromatography identification of rhizoma alismatis raw medicinal materials:
(1) Taking gastrodia elata vertigo treating particles, adding absolute ethyl alcohol, carrying out ultrasonic extraction, filtering, evaporating filtrate to dryness, dissolving residues in water, extracting ethyl acetate, taking an ethyl acetate phase, fully washing with ammonia test solution, discarding ammonia solution, washing with water, evaporating ethyl acetate solution to dryness, and dissolving residues in methanol to serve as a sample solution;
(2) Adding methanol into 2, 3-acetyl alisol B reference substance to obtain reference substance solution;
(3) Sucking the sample solution and the reference substance solution, respectively spotting on the same silica gel G thin layer plate, spreading with cyclohexane-chloroform-methyl acetate with the volume ratio of 3-5:1-3:3-5 as developing agent, taking out, air drying, spraying 10% sulfuric acid ethanol solution, and drying at 105deg.C until the spots develop clearly;
C. thin layer chromatography identification of bighead atractylodes rhizome raw material medicines:
(1) Grinding rhizoma Gastrodiae vertigo granule sample, adding methanol, ultrasonic treating, centrifuging, removing methanol solution, dissolving precipitate with hydrochloric acid solution, transferring into ampoule bottle, sealing, hydrolyzing in boiling water bath, filtering, evaporating filtrate, and dissolving with methanol to obtain sample solution;
(2) Weighing amino acid reference substance, adding methanol to prepare reference substance solution;
(3) Sucking the test solution and the reference solution, respectively spotting on the same silica gel G thin layer plate, spreading with water saturated n-butanol-acetic acid with volume ratio of 7-9:2-4 as developing agent, taking out, air drying, spraying 0.5% ninhydrin ethanol solution, and drying at 105deg.C until the spots develop clearly;
The amino acid is one or more of aspartic acid, threonine, serine, glutamic acid, glycine, alanine, cysteine, valine, methionine, isoleucine, leucine, tyrosine, phenylalanine, lysine, histidine or arginine.
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