CN115436557B - Thin-layer identification method for humifuse euphorbia herb and preparation thereof - Google Patents
Thin-layer identification method for humifuse euphorbia herb and preparation thereof Download PDFInfo
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Abstract
The invention discloses a thin-layer identification method of humifuse euphorbia herb and a preparation thereof, which comprises the steps of preparing a control medicinal material solution, a decoction piece test sample solution, formula particles and a standard decoction test sample solution, taking the control medicinal material solution and the test sample solution to be respectively spotted on the same thin-layer plate, developing by using developing agents, spraying a color developing agent for developing, and obtaining a thin-layer chromatogram to finish identification operation. The method is simple and quick to operate, does not need an acid hydrolysis step, does not damage chemical components of the humifuse euphorbia herb, presents prototype components of the humifuse euphorbia herb to the greatest extent, and is rich in chromatographic spot information; the consistency of the reference medicinal materials is adopted for evaluation, so that the evaluation is more accurate and scientific.
Description
Technical Field
The invention relates to the field of traditional Chinese medicine quality control, in particular to a thin-layer identification method of humifuse euphorbia herb and a preparation thereof.
Background
Herba Euphorbiae Humifusae (also called herba Chenopodii, herba Hedyotidis Diffusae, herba Crotalariae sessiliflorae, herba Euphorbiae Humifusae) is dried whole herb of Euphorbiae Humifusae Euphorbia humifusa Willd or Euphorbiae Humifusa Euphorbia maculate L. Not only is a common clinical traditional Chinese medicine, but also is a Uygur medicinal material and a Mongolian medicinal material. The main chemical components of herba Euphorbiae Humifusae include coumarin, palmitic acid, gallic acid, methyl gallate and myo-inositol. Herba Euphorbiae Humifusae has effects of clearing heat and detoxicating, cooling blood and stopping bleeding, promoting diuresis and eliminating jaundice, and is clinically used for treating dysentery, diarrhea, hemoptysis, hematuria, hematochezia, metrorrhagia, sore, furuncle, carbuncle, and jaundice due to damp-heat, with definite curative effect and small side effect.
In the existing thin-layer identification method of herba Euphorbiae Humifusae and preparation thereof, hydrochloric acid hydrolysis is adopted in the preparation process of the sample solution, so that flavonoid glycoside components in herba Euphorbiae Humifusae are hydrolyzed into flavonoid aglycone (quercetin), and quality evaluation is carried out by using single thin-layer spots of quercetin reference substances. The methods can not fully reflect the flavonoid components of the prototype, and have the advantages of complex operation and less chromatographic spot information. A plurality of traditional Chinese medicinal materials contain quercetin components, so that the prior evaluation method cannot distinguish confusing products containing the quercetin components.
Disclosure of Invention
The invention aims to: aiming at the defects and shortcomings of the prior art, the invention provides a thin-layer identification method of humifuse euphorbia herb and preparation thereof, which is simple and quick to operate, does not need an acid hydrolysis step, does not damage chemical components of the humifuse euphorbia herb, presents prototype components of the humifuse euphorbia herb to the greatest extent and has rich chromatographic spot information; the consistency of the reference medicinal materials is adopted for evaluation, so that the evaluation is more accurate and scientific.
The technical scheme is as follows: the invention relates to a thin layer identification method of humifuse euphorbia herb and a preparation thereof, which comprises the following steps:
1) Decocting herba Euphorbiae Humifusae control medicinal material and herba Euphorbiae Humifusae decoction pieces with water or heating and refluxing respectively, filtering, shaking and extracting with ethyl acetate solution, standing for layering, collecting supernatant, evaporating to dryness, dissolving residue with alcohol solvent to obtain control medicinal material solution and decoction piece test sample solution;
2) Dissolving herba Euphorbiae Humifusae formula particles and a standard decoction sample in water respectively, shaking and extracting with ethyl acetate solution, standing for layering, taking supernatant, evaporating to dryness, and dissolving residues with alcohol solvent to obtain formula particles and a standard decoction sample solution;
3) And respectively dispensing the control medicinal material solution and the sample solution on the same thin layer plate, developing by using developing agent, and spraying a developing agent for developing color to obtain a thin layer chromatogram to finish the identification operation.
Wherein, when the humifuse euphorbia herb control medicinal material and the humifuse euphorbia herb decoction pieces in the step 1) are decocted by adding water, the mass volume of the control medicinal material, the humifuse euphorbia herb decoction pieces and the water is 1:20 g/mL-200 g/mL, the treatment time of decoction or heating reflux is 15 min-60 min, the times of shaking and extracting the ethyl acetate solution are 1-4 times, and the volume ratio of the ethyl acetate solution to the control medicinal material aqueous solution is 0.5:2-1.
Wherein, when the humifuse euphorbia herb formula particles and the standard decoction in the step 2) are dissolved in water, the mass volume of the humifuse euphorbia herb formula particles, the standard decoction and the water is 1:50 g/mL-500 g/mL, the times of the shaking extraction of ethyl acetate are 1-4 times, and the volume ratio of the ethyl acetate solution to the aqueous solution of the sample is 0.5:2-1.
Wherein the volume ratio of toluene to ethyl acetate to formic acid to water in the developing agent in the step 3) is 1:4-12:1-4:0.5-2.
Wherein, the sample application amount of the control medicinal material solution and the test sample solution in the step 3) is 1-10 mu l.
Wherein, the color reagent in the step 3) is aluminum trichloride ethanol test solution, and is sprayed with the color reagent and then dried by hot air, and the inspection is carried out under a 365nm ultraviolet lamp.
Wherein, the thin layer plate in the step 3) is a polyamide film.
Wherein, on the thin-layer chromatogram in the step 3), fluorescent spots with the same color appear on the position corresponding to the chromatogram of the control medicinal material solution in the chromatogram of the test solution.
Principle analysis: according to the chemical structure and the property of each active ingredient of the traditional Chinese medicine, the method adopts a proper extraction solvent to simply and rapidly prepare the test sample and the control medicinal material solution according to the extraction principle of similar compatibility. And then a proper developing agent is adopted for developing, and various chemical components can be well separated on the thin layer plate along with the selected developing agent according to different adsorption, desorption, reabsorption and reabsorption capacities. And then, by means of various effective components with similar polarities, spots with different colors are displayed on the same thin layer plate under different inspection conditions, and a thin layer chromatogram with multiple information is obtained.
The beneficial effects are that: compared with the prior art, the invention has the following remarkable advantages: the invention adopts a simple and quick pretreatment method to obtain a sample solution and a reference medicinal material solution, which are respectively spotted on the same thin layer plate, and the thin layer plate is unfolded by a proper developing agent, and is inspected under ultraviolet light to obtain a multi-information humifuse euphorbia herb thin layer chromatogram. Compared with pharmacopoeia methods and existing literature reports, the method is simple and rapid to operate, does not need an acid hydrolysis step, does not damage chemical components of the humifuse euphorbia herb, presents prototype components of the humifuse euphorbia herb to the greatest extent, and is rich in chromatographic spot information; the consistency of the reference medicinal materials is adopted for evaluation, so that the evaluation is more accurate and scientific.
Drawings
FIG. 1 is a thin layer chromatogram of the herba Euphorbiae Humifusae formulation granule of example 1 of the present invention;
FIG. 2 is a thin-layer chromatogram of the standard decoction of herba Euphorbiae Humifusae in example 1 of the present invention;
FIG. 3 is a thin-layer chromatogram of herba Euphorbiae Humifusae decoction pieces in example 1 of the present invention;
FIG. 4 is a thin layer chromatogram of different spotting amounts in example 2 of the present invention;
FIG. 5 is a thin layer chromatogram of example 2 of the present invention at different temperatures;
FIG. 6 is a thin layer chromatogram of different humidity in example 2 of the present invention;
FIG. 7 is a thin-layer chromatogram of herba Euphorbiae Humifusae decoction pieces in comparative example 1 of the present invention;
FIG. 8 is a thin layer chromatogram of the herba Euphorbiae Humifusae formulation granule of comparative example 2 of the present invention.
Detailed Description
The technical scheme of the invention is further described below with reference to the accompanying drawings and the specific embodiments.
The invention adopts the following instruments and reagents:
instrument: a thin-layer automatic imager (CAMAG TLC VISUALIZER), a thousandth balance (AR 223CN, orhaus), a silica gel G thin-layer plate (Qingdao ocean chemical plant), a polyamide film (four-methyl biochemical plastics plant in road and bridge of Taizhou, zhejiang), a GKC temperature-controlled water bath pot (Nantong Huatai laboratory instruments Co., ltd.), and an AS165W type centrifuge (Sunswang (Shanghai) commercial Co., ltd.).
Reagent: toluene (Shanghai Lingfeng chemical reagent Co., ltd.), ethyl acetate (Guogong chemical reagent Co., ltd.), formic acid (Guogong chemical reagent Co., ltd.), methanol (Guogong chemical reagent Co., ltd.), ethanol (Guogong chemical reagent Co., ltd.) are all analytically pure; the water is ultrapure water.
The herba Euphorbiae Humifusae control medicinal material (batch number: 121552-200902) is purchased from China medicine biological product verification institute.
The herba Euphorbiae Humifusae formula granule (lot numbers: 19120199, 19120209, 19120219), herba Euphorbiae Humifusae standard decoction (lot numbers: DG1811004, DG1905128, DG 121909135), herba Euphorbiae Humifusae decoction pieces (lot numbers: YP1811004, YP1905128, YP 121909135) are prepared by Jiangyin Tianjiang pharmaceutical industry Co.
The present invention may be carried out according to the operation or conditions of conventional experimental procedures described in the literature in the field, unless specific experimental procedures or conditions are noted. The reagents or apparatus used were conventional reagent products commercially available without the manufacturer's knowledge.
Example 1:
preparing a decoction piece sample solution: extracting herba Euphorbiae Humifusae decoction piece powder 0.5g with water 20mL under reflux for 30 min under heating with ethyl acetate for twice (20 mL each time), mixing ethyl acetate solutions, evaporating to dryness, and dissolving the residue with methanol 1mL to obtain test solution.
Preparation of formulation granules or standard decoction test sample solution: taking 0.1g of humifuse euphorbia herb formula particles or humifuse euphorbia herb standard decoction, adding 20mL of water, slightly heating to dissolve, cooling, shaking and extracting twice with 20mL of ethyl acetate each time, combining ethyl acetate liquid, evaporating to dryness, and adding 1mL of methanol into residues to dissolve to obtain a sample solution.
Preparation of control medicinal material solution: and (3) adding 20mL of water into 0.5g of humifuse euphorbia herb reference medicine, decocting for 60min, slightly boiling, cooling, shaking and extracting twice with 20mL of ethyl acetate each time, combining ethyl acetate liquid, evaporating to dryness, and adding 1mL of methanol into residues to dissolve the residues to obtain a reference medicine solution.
Thin layer identification step: sucking 2 μl of each of the sample solution and the control medicinal solution, respectively spotting on the same polyamide film, spreading with toluene-ethyl acetate-formic acid-water (1:8:2:1) as developing agent, taking out, air drying, spraying aluminum trichloride ethanol solution, blow drying with hot air, and inspecting under ultraviolet lamp (365 nm).
Evaluation requirements: in the chromatogram of the test sample, fluorescent spots with the same color appear at the positions corresponding to the chromatogram of the reference medicinal material.
Analysis of results: in fig. 1, 1-3 correspond to sample chromatograms of humifuse euphorbia herb formula particles with lot numbers of 19120199, 19120209 and 19120219 respectively, and S is a humifuse euphorbia herb control medicinal material chromatogram. In fig. 2, 1-3 correspond to sample chromatograms of humifuse euphorbia herb standard decoction with batch numbers of DG1811004, DG1905128 and DG121909135 respectively, and S is a humifuse euphorbia herb reference medicinal material chromatogram. In fig. 3, 1 to 3 correspond to sample chromatograms of herba Euphorbiae Humifusae decoction pieces with lot numbers of YP1811004, YP1905128 and YP121909135, respectively, and S is herba Euphorbiae Humifusae reference medicinal material chromatogram.
Example 2:
the thin layer authentication in example 1 was subjected to durability verification, specifically including:
(1) Investigation of different spotting amounts:
preparing test solution and control medicinal solution from herba Euphorbiae Humifusae formula granule (batch number: 19120199) and herba Euphorbiae Humifusae control medicinal material according to the method described in example 1, respectively, taking 1 μl, 2 μl, 4 μl, 10 μl and 1 μl, 2 μl, 5 μl and 10 μl of herba Euphorbiae Humifusae control medicinal material solution, respectively, spotting on the same polyamide film, spreading with toluene-ethyl acetate-formic acid-water (1:8:2:1) as developing agent, taking out, air drying, spraying aluminum trichloride ethanol test solution, blow drying with hot air, and inspecting under ultraviolet lamp (365 nm). The results are shown in fig. 4, 1-4 in fig. 4 correspond to 1 mu L, 2 mu L, 5 mu L and 10 mu L of the humifuse euphorbia herb formula particle sample chromatogram, 5-8 correspond to 1 mu L, 2 mu L, 5 mu L and 10 mu L of the humifuse euphorbia herb control medicine chromatogram respectively, and when the sample application amount is 1 mu L-10 mu L, the humifuse euphorbia herb formula particle chromatogram and the control medicine chromatogram show clear spots at the corresponding positions without other interference.
(2) Investigation of different temperatures:
preparing test solution and control solution of herba Euphorbiae Humifusae formula granule (batch numbers: 19120199, 19120209, 19120219) and herba Euphorbiae Humifusae control medicinal material respectively according to the method described in example 1, respectively taking 2 μl of test solution of herba Euphorbiae Humifusae formula granule and 2 μl of herba Euphorbiae Humifusae control medicinal material solution, spotting on the same polyamide film, respectively spreading under low temperature (T: 4deg.C, RH: 35%), normal temperature (T: 20deg.C, RH: 35%) and high temperature (T: 35deg.C, RH: 35%) with toluene-ethyl acetate-formic acid-water (1:8:2:1) as spreading agent, taking out, air drying, spraying aluminum trichloride ethanol test solution, blow drying with hot air, and inspecting under ultraviolet lamp (365 nm). The results are shown in fig. 5, 1-3 in fig. 5 correspond to the sample chromatogram of the humifuse euphorbia herb formula particle, S corresponds to the control sample chromatogram of the humifuse euphorbia herb, and as can be seen from fig. 5, the sample chromatogram of the humifuse euphorbia herb formula particle and the corresponding position of the control sample chromatogram show fluorescence spots with the same color under different temperature conditions, and the separation effect is good. Experimental results show that the temperature has small influence on the thin-layer identification of the humifuse euphorbia herb formula particles, and the thin-layer identification method has good durability on different temperatures.
(3) Investigation of different humidity:
preparing test solution and control medicinal solution from herba Euphorbiae Humifusae formula granule (batch numbers: 19120199, 19120209, 19120219) and herba Euphorbiae Humifusae control medicinal material according to the method described in example 1, respectively taking 2 μl of test solution and 2 μl of herba Euphorbiae Humifusae formula granule and herba Euphorbiae Humifusae control medicinal material solution, spotting on the same polyamide film, respectively spreading under different humidity (RH: 18%, 35%, 88%) with toluene-ethyl acetate-formic acid-water (1:8:2:1) as spreading agent, taking out, air drying, spraying aluminum trichloride ethanol test solution, blow drying with hot air, and inspecting under ultraviolet lamp (365 nm). The results are shown in fig. 6, 1-3 in fig. 6 correspond to the sample chromatogram of the humifuse euphorbia herb formula granule, S corresponds to the control sample chromatogram of the humifuse euphorbia herb, and as can be seen from fig. 6, the sample chromatogram of the humifuse euphorbia herb formula granule and the corresponding position of the control sample chromatogram show fluorescence spots with the same color under different humidity conditions, and the separation effect is good. Experimental results show that the humidity has small influence on the thin-layer identification of the humifuse euphorbia herb formula particles, and the thin-layer identification method is good in durability on different humifuse euphorbia herb.
Comparative example 1:
the comparative example adopts a method of the first edition of Chinese pharmacopoeia 2020 to carry out thin-layer chromatography detection on humifuse euphorbia herb decoction pieces, and the specific process is as follows:
preparation of test solution: taking 1g of humifuse euphorbia herb decoction piece powder, adding 50ml of 80% methanol, heating and refluxing for 1 hour, cooling, filtering, evaporating filtrate to dryness, adding 60ml of water-diethyl ether (1:1) mixed solution into residues to dissolve, standing and layering, discarding diethyl ether solution, adding diethyl ether into water solution to extract for 2 times, 20ml each time, discarding diethyl ether solution, adding 5ml of hydrochloric acid into water solution, hydrolyzing for 1 hour in a water bath, taking out, rapidly cooling, extracting for 2 times with diethyl ether, 20ml each time, combining diethyl ether solution, washing with 30ml of water, discarding water solution, volatilizing diethyl ether solution, adding 1ml of ethanol into residues to dissolve, and taking the residues as a test solution.
Preparation of a control solution: taking quercetin reference substance, adding ethanol to prepare a solution containing 1mg per 1ml, and taking the solution as reference substance solution.
Thin layer identification step: 10 μl of the sample solution and 2 μl of the control solution are sucked and respectively spotted on the same silica gel G thin layer plate, toluene-ethyl acetate-formic acid (5:4.5:0.5) is used as developing agent, developed, taken out, dried, sprayed with 3% aluminum trichloride ethanol solution, heated at 105deg.C for several minutes, and detected under ultraviolet lamp (365 nm).
Evaluation requirements: in the chromatogram of the test sample, fluorescent spots with the same color appear at the positions corresponding to the chromatogram of the reference sample.
The results are shown in FIG. 7, wherein T in FIG. 7 corresponds to a quercetin control, and 1 corresponds to a sample chromatogram of herba Euphorbiae Humifusae decoction pieces (lot number: YP 121909135).
Comparative example 2:
the comparative example adopts a method of patent (detection method of humifuse euphorbia herb traditional Chinese medicine preparation, application publication number CN 102078363A) to carry out thin-layer chromatography detection on humifuse euphorbia herb formula particles, and the specific process is as follows:
taking about 1.0g of the product, grinding, adding 50-90ml of 80% methanol, carrying out ultrasonic treatment for 30 minutes, filtering, evaporating the filtrate, adding 90ml of water-diethyl ether (1:1) into residues to dissolve, standing for layering, discarding diethyl ether solution, adding diethyl ether into water solution to extract for 2 times, 30ml each time, discarding diethyl ether solution, adding 10ml of hydrochloric acid into water solution, hydrolyzing for 1 hour in a water bath, taking out, rapidly cooling, extracting with diethyl ether for 2 times, 30ml each time, combining diethyl ether solution, washing with 50ml of water, discarding water solution, volatilizing diethyl ether solution, adding 1ml of ethanol into residues to dissolve, taking the residues as a sample solution, taking quercetin reference substance, and adding ethanol to prepare a solution containing 1mg each 1ml as a reference substance solution. Thin layer chromatography (appendix IVB) test, sucking 5ul of the above test solution and 2ul of the control solution, respectively spotting on the same silica gel G thin layer plate, spreading with toluene-ethyl acetate-formic acid (5:4:0.5) as developing agent, taking out, air drying, spraying 3% aluminum trichloride ethanol solution, heating at 105deg.C for several minutes, and placing under ultraviolet lamp (365 nm) for inspection. Spots of the same color appear in the sample chromatogram at the corresponding positions of the control chromatogram.
The results are shown in FIG. 8, wherein in FIG. 8, T corresponds to a quercetin control, and 1-3 corresponds to the chromatogram of the sample of the humifuse euphorbia herb formula granule (lot numbers: 19120199, 19120209, 19120219).
Comprehensive analysis: the thin-layer identification method of the humifuse euphorbia herb formula particles and the preparation thereof provided by the invention has the advantages that the preparation operation of a test sample is simpler and faster, the steps of acid hydrolysis, diethyl ether extraction and the like are not needed, the defect that acid hydrolysis is needed when the thin-layer identification is carried out on the humifuse euphorbia herb in the prior art is overcome, the use of organic reagents such as hydrochloric acid, diethyl ether and the like is avoided, and the method is safer and more environment-friendly. The thin-layer identification method provided by the invention has the advantages that chromatographic spots are more abundant, the information of the original chemical components in the sample is reflected, and the defect that the original chemical components are destroyed by acid hydrolysis in the existing thin-layer identification method is overcome, so that the obtained information of the chromatographic spots is less. The thin-layer identification method adopts the' fluorescent spots with the same color on the positions corresponding to the chromatogram of the reference medicinal materials in the chromatogram of the sample to perform quality evaluation, and the sample corresponds to more spots of the reference medicinal materials, so that compared with the prior art, the quality evaluation is performed by only adopting 1 reference substance of quercetin, the quality evaluation is more comprehensive, accurate and scientific, and the misjudgment caused by other mistakes of humifuse euphorbia herb containing quercetin can be reduced.
Claims (1)
1. A thin-layer identification method of a humifuse euphorbia herb preparation is characterized by comprising the following steps of: comprising the following steps:
1) Decocting herba Euphorbiae Humifusae control medicinal material and herba Euphorbiae Humifusae decoction pieces with water or heating and refluxing respectively, filtering, shaking and extracting with ethyl acetate, standing for layering, collecting supernatant, evaporating to dryness, dissolving residue with alcohol solvent to obtain control medicinal material solution and decoction piece test sample solution; when the humifuse euphorbia herb control medicinal material and the humifuse euphorbia herb decoction pieces are decocted in water, the mass volume of the control medicinal material, the humifuse euphorbia herb decoction pieces and the water is 1:20 g/mL-200 g/mL, the treatment time of decoction or heating reflux is 15 min-60 min, the times of shaking and extracting ethyl acetate are 1-4 times, and the volume ratio of the ethyl acetate to the control medicinal material aqueous solution is 0.5:2-1;
2) Dissolving herba Euphorbiae Humifusae formula particles and a standard decoction sample in water respectively, shaking and extracting with ethyl acetate, standing and layering, taking supernatant, evaporating to dryness, and dissolving residues in alcohol solvent to obtain formula particles and a standard decoction sample solution; when the humifuse euphorbia herb formula particles and the standard decoction are dissolved in water, the mass volume of the humifuse euphorbia herb formula particles, the standard decoction and the water is 1:50 g/mL-500 g/mL, the times of shaking and extracting ethyl acetate are 1-4 times, and the volume ratio of the ethyl acetate to the aqueous solution of the sample is 0.5:2-1;
3) Taking a control medicinal material solution and a test sample solution to be respectively spotted on the same thin layer plate, spreading with a developing agent, and then spraying a developing agent for developing color to obtain a thin layer chromatogram to finish the identification operation; the volume ratio of toluene to ethyl acetate to formic acid to water in the developing agent is 1:8:2:1; the sample application amount of the control medicinal material solution and the sample solution is 1-10 μl; the color reagent is aluminum trichloride ethanol test solution, and is sprayed with the color reagent and then dried by hot air, and inspected under a 365nm ultraviolet lamp; the thin layer plate is a polyamide film; on the thin-layer chromatogram, the sample solution chromatogram shows fluorescence spots with the same color at the positions corresponding to the control medicinal material solution chromatogram.
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| CN109085285A (en) * | 2018-10-12 | 2018-12-25 | 海南葫芦娃药业集团股份有限公司 | A kind of method of quality control of changyanning granules |
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