CN110702835A - Thin-layer chromatography identification method of traditional Chinese medicine oral preparation - Google Patents
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Abstract
The invention relates to the technical field of traditional Chinese medicines, in particular to a thin-layer chromatography identification method of a traditional Chinese medicine oral preparation, which comprises the traditional Chinese medicine oral preparation, wherein the traditional Chinese medicine oral preparation comprises ginseng, mulberry leaves, liquorice, fried bitter apricot kernels and loquat leaves, and the thin-layer chromatography identification method of the ginseng comprises the following steps: s1, taking 1-5 g of the decoction granules, adding 10-100 ml of water, dissolving by ultrasonic, filtering, washing the filtrate with ethyl acetate, shaking and extracting the water solution with water saturated n-butyl alcohol, combining the n-butyl alcohol solution, washing with sodium hydroxide solution, discarding the sodium hydroxide solution, and washing with water saturated by n-butyl alcohol. According to the invention, by designing the method, complex reagents, instruments or equipment are not needed, the multi-flavor traditional Chinese medicinal materials in the lung clearing and relieving soup can be rapidly identified, the identification result is visual and easy to identify, the sensitivity and specificity are higher than those of a conventional thin-layer chromatography identification method, and a convenient and practical way is provided for qualitatively identifying the multi-flavor traditional Chinese medicinal materials in the lung clearing and relieving soup.
Description
Technical Field
The invention relates to the technical field of traditional Chinese medicines, in particular to a thin-layer chromatography identification method of a traditional Chinese medicine oral preparation.
Background
The decoction for clearing dryness and rescuing lung is derived from the theory of clearing and leading to the medical laws of Chang, and consists of mulberry leaf, gypsum, liquorice, ginseng, linseed, real donkey-hide gelatin, ophiopogon root, almond and loquat leaf, and has the main functions of clearing dryness and moistening lung, and nourishing yin and tonifying qi. It is mainly used for treating warm-dryness impairment of lung and qi and yin impairment. Fever, headache, dry cough without phlegm, dyspnea due to adverse rise of qi, dry throat, dry nose, restlessness, thirst, fullness in the chest, hypochondriac pain, dry tongue with little coating, and deficient, large and rapid pulse.
The decoction for clearing dryness and relieving lung has wide clinical application range, and relates to cough, hemoptysis, pulmonary fistula, pharyngitis, dermatosis, amenorrhea, pruritus, constipation, watery urine, fistula and other diseases, wherein the cough, the hemoptysis and other lung diseases account for the main part. From the perspective of modern medicine, the decoction for removing dryness and relieving lung can be used in clinical departments such as internal medicine, five sense organs, dermatology and the like, wherein the most common is to treat respiratory diseases.
The traditional Chinese medicine compound prescription consists of a plurality of medicinal materials, the ingredients are complex after decoction, the drug effect is not only exerted by a single ingredient, a detection method capable of quickly, simply and conveniently detecting a plurality of medicinal materials in a medicinal preparation is established, and the method has important significance for comprehensive quality detection and overall quality control.
The prescription of the decoction for removing dryness and rescuing lung comprises frosted mulberry leaf, gypsum, dwarf lilyturf tuber, fried black sesame, ginseng, donkey-hide gelatin, honey loquat leaf, liquorice and fried bitter apricot seed, wherein the monarch drug is mulberry leaf, the ministerial drug is calcined gypsum and dwarf lilyturf tuber, the adjuvant drug is ginseng, fried black sesame, donkey-hide gelatin, fried bitter apricot seed and honey loquat leaf, and the conductant drug is liquorice, so that the product quality can be quickly and effectively controlled, and the thin-layer chromatography identification method of the multiple medicinal materials such as ginseng, mulberry leaf, liquorice, fried bitter apricot seed, honey loquat leaf and donkey-hide gelatin in the traditional Chinese medicine oral preparation is established.
In conclusion, the invention provides a thin-layer chromatography identification method of a traditional Chinese medicine oral preparation to solve the problems.
Disclosure of Invention
The invention aims to provide a thin-layer chromatography identification method of a traditional Chinese medicine oral preparation, so as to solve the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme:
a thin layer chromatography identification method of a traditional Chinese medicine oral preparation comprises the traditional Chinese medicine oral preparation, and the traditional Chinese medicine oral preparation comprises ginseng, mulberry leaf, liquorice, fried bitter apricot kernel and honey loquat leaf.
Preferably, the ginseng thin layer identification method comprises the following steps:
s1, taking 1-5 g of the dry lung-relieving decoction particles, adding 10-100 ml of water, ultrasonically dissolving, filtering, washing the filtrate with ethyl acetate, shaking and extracting the water solution with water-saturated n-butyl alcohol, combining the n-butyl alcohol solution, washing with a sodium hydroxide solution, discarding the sodium hydroxide solution, washing with the water-saturated n-butyl alcohol, discarding the water solution, evaporating the n-butyl alcohol solution to dryness, and dissolving the residue with methanol to obtain a sample solution;
s2, taking 1-5 g of ginseng reference drug, adding 20-100 ml of water, decocting, filtering, preparing a reference drug solution by the same method, taking a ginsenoside Rb1 reference substance, a ginsenoside Re reference substance, a ginsenoside Rf reference substance and a ginsenoside Rg1 reference substance, and adding methanol to prepare a mixed solution as a reference substance solution;
s3, identifying by thin-layer chromatography, namely respectively sucking 1-2 mu l of each of the three solutions, respectively dropping the three solutions on the same silica gel G thin-layer plate, developing by using chloroform-methanol-water (13:7:2) as a developing agent, taking out, drying by airing, spraying 10% sulfuric acid ethanol solution, heating at 105 ℃ until the color development of spots is clear, respectively inspecting under sunlight and ultraviolet light (365nm), and respectively displaying spots or fluorescent spots with the same color on positions corresponding to the chromatogram of a reference medicinal material and the chromatogram of the reference medicinal material in the chromatogram of a test product;
s4, respectively taking 3 batches of the Chinese medicinal oral preparation, preparing a test solution by the same test preparation method, and performing thin-layer identification.
Preferably, the mulberry leaf thin layer identification method comprises the following steps:
s1, taking 10-50 ml of ethyl acetate solution for the thin-layer identification method of the identified ginseng, evaporating to dryness, and dissolving the residue in 1-5 ml of ethyl acetate to obtain a test solution;
s2, taking 1-5 g of mulberry leaf control medicinal material, adding 20-100 ml of water, decocting, filtering, washing the filtrate with ethyl acetate, combining ethyl acetate solutions, evaporating to dryness, and adding ethyl acetate into residues to dissolve the residues to obtain a control medicinal material solution;
s3, identifying by thin-layer chromatography, namely, respectively absorbing the two solutions, respectively dropping the two solutions on the same silica gel G thin-layer plate, developing by using toluene-ethyl acetate-formic acid (5:2:1) as a developing agent, taking out, drying in the air, placing under an ultraviolet lamp (365nm) for inspection, and displaying fluorescent main spots with the same color on the positions corresponding to the reference medicinal material chromatogram in the test sample chromatogram;
s4, respectively taking 3 batches of the Chinese medicinal oral preparation, preparing a test solution by the same test preparation method, and performing thin-layer identification.
Preferably, the liquorice thin-layer identification method comprises the following steps:
s1, taking 1-5 g of the product, adding 10-100 ml of water, dissolving with ultrasound, filtering, extracting the filtrate with water saturated n-butanol by shaking, combining n-butanol solutions, extracting with sodium hydroxide solution by shaking, combining sodium hydroxide solution layers, adjusting the pH value to 2-6 with hydrochloric acid, extracting with ethyl acetate by shaking, combining ethyl acetate solutions, steaming to dry, and dissolving the residue with methanol to obtain a sample solution;
s2, taking 1-5 g of licorice contrast drug, adding 10-100 ml of water, decocting for 20-50 minutes, filtering, extracting with water saturated n-butanol, combining n-butanol liquid, the other operations are the same as the preparation method of the sample, dissolving residue with methanol, taking the liquiritin contrast drug as the contrast drug solution, adding methanol to prepare a solution containing 1-5 mg of liquiritin per 1ml, and taking the solution as the contrast drug solution;
s3, identifying by thin-layer chromatography, namely, sucking 1-10 mu l of each solution, respectively dropping the solution on the same silica gel G thin-layer plate, developing by using chloroform-methanol-water (13:7:2) as a developing agent, taking out, drying in the air, spraying 10% sulfuric acid ethanol solution, heating at 105 ℃ until the color development of spots is clear, respectively viewing by using sunlight and ultraviolet lamps (365nm), displaying spots or fluorescent spots with the same color on the positions corresponding to the color spectrum of a reference drug in the color spectrum of a test product, and displaying the same orange yellow fluorescent spots on the positions corresponding to the color spectrum of the reference drug;
s4, taking 15 batches of oral Chinese medicinal preparations, preparing test solution by the same method for preparing the test, and performing thin-layer identification.
Preferably, the identification method of the fried bitter almond thin layer comprises the following steps:
s1, taking 1-5 g of the product, adding 10-100 ml of methanol, carrying out ultrasonic treatment for 10-50 minutes, filtering, evaporating filtrate to dryness, dissolving residues by adding 1-10 ml of water, passing through a macroporous adsorption resin column, respectively adding 10-50 ml of water and 10-50 ml of ammonia solution for elution, eluting by using ethanol, collecting eluent, evaporating to dryness, dissolving residues by adding acetone, and taking supernate as a test solution;
s2, adding methanol into amygdalin as reference substance to obtain 1-5 mg/1 ml solution as reference substance solution;
s3, identifying by thin-layer chromatography, namely respectively sucking 1-10 mu l of the solutions, respectively dropping the solutions on the same silica gel G thin-layer plate, respectively taking the upper layer solution of n-butyl alcohol-acetic acid-water (19:1:5) as a developing agent, developing, taking out, drying in the air, spraying a 10% sulfuric acid ethanol solution of 2% phosphomolybdic acid, heating at 105 ℃ until spots are clearly developed, and displaying main spots with the same color on positions corresponding to the reference medicine chromatogram and the reference substance chromatogram in the test substance chromatogram;
s4, taking 15 batches of oral Chinese medicinal preparations, preparing test solution by the same method for preparing the test, and performing thin-layer identification.
Preferably, the method for identifying the meliloti folium laminae comprises the following steps:
s1, taking 1-5 g of the product, adding 10-100 ml of water to dissolve the product, adjusting the pH value to 8-11 with a sodium hydroxide test solution, shaking and extracting with ethyl acetate, combining ethyl acetate solutions, evaporating to dryness, and adding 1ml of methanol to dissolve residues to obtain a test solution;
s2, taking 1-5 g of loquat leaf control medicinal material, adding 10-100 ml of water, decocting, filtering, adjusting the pH value of the filtrate to 8-11 by using sodium hydroxide test solution, preparing loquat leaf control medicinal material solution by the same method, taking bear fruit acid control, adding methanol to prepare 0.1-0.5 mg of solution in each 1ml as control solution;
s3, identifying by thin layer chromatography, respectively sucking 5 μ l of each of the four solutions, respectively dropping on the same silica gel G thin layer plate, spreading with toluene-ethyl acetate-formic acid (10:2:0.2) as developing agent, taking out, air drying, spraying 10% sulfuric acid ethanol solution, heating at 105 deg.C until the spots are clearly developed, and inspecting with ultraviolet lamp (365 nm).
Compared with the prior art, the invention has the beneficial effects that:
according to the method, complex reagents, instruments or equipment are not needed, the traditional Chinese medicinal materials in the lung clearing and relieving soup can be rapidly identified, the identification result is visual and easy to identify, the sensitivity and specificity are higher than those of a conventional thin-layer chromatography identification method, and meanwhile, the method is not only suitable for detecting granules in a traditional Chinese medicine oral preparation, but also suitable for detecting capsules, oral preparations, tablets and the like, so that the detection is more comprehensive, and a convenient and practical way is provided for qualitatively identifying the traditional Chinese medicinal materials in the lung clearing and relieving soup.
Detailed Description
The technical solutions in the embodiments of the present invention will be described below clearly and completely with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, rather than all embodiments, and all other embodiments obtained by a person of ordinary skill in the art without creative efforts based on the embodiments of the present invention belong to the protection scope of the present invention.
The invention provides a technical scheme that:
a thin layer chromatography identification method of a traditional Chinese medicine oral preparation comprises the traditional Chinese medicine oral preparation, and the traditional Chinese medicine oral preparation comprises ginseng, mulberry leaf, liquorice, fried bitter apricot kernel and honey loquat leaf.
Method 1
The ginseng thin-layer identification method comprises the following steps:
s1, taking 1-5 g of the dry lung-relieving decoction particles, adding 10-100 ml of water, ultrasonically dissolving, filtering, washing the filtrate with ethyl acetate, shaking and extracting the water solution with water-saturated n-butyl alcohol, combining the n-butyl alcohol solution, washing with a sodium hydroxide solution, discarding the sodium hydroxide solution, washing with the water-saturated n-butyl alcohol, discarding the water solution, evaporating the n-butyl alcohol solution to dryness, and dissolving the residue with methanol to obtain a sample solution;
s2, taking 1-5 g of ginseng reference drug, adding 20-100 ml of water, decocting, filtering, preparing a reference drug solution by the same method, taking a ginsenoside Rb1 reference substance, a ginsenoside Re reference substance, a ginsenoside Rf reference substance and a ginsenoside Rg1 reference substance, and adding methanol to prepare a mixed solution as a reference substance solution;
s3, identifying by thin-layer chromatography, namely respectively sucking 1-2 mu l of each of the three solutions, respectively dropping the three solutions on the same silica gel G thin-layer plate, developing by using chloroform-methanol-water (13:7:2) as a developing agent, taking out, drying by airing, spraying 10% sulfuric acid ethanol solution, heating at 105 ℃ until the color development of spots is clear, respectively inspecting under sunlight and ultraviolet light (365nm), and respectively displaying spots or fluorescent spots with the same color on positions corresponding to the chromatogram of a reference medicinal material and the chromatogram of the reference medicinal material in the chromatogram of a test product;
s4, respectively taking 3 batches of the Chinese medicinal oral preparations, preparing a test solution by the above test preparation method, and performing thin-layer identification to obtain a result: in the chromatogram of the test sample, spots or fluorescent spots with the same color are respectively displayed at the positions corresponding to the chromatogram of the reference medicinal material and the chromatogram of the reference product, and the result of a methodological test shows that the method is simple, convenient, accurate, stable and good in reproducibility, and can quickly identify the ginseng medicinal material in the Chinese medicinal oral preparation.
Method two
The mulberry leaf thin layer identification method comprises the following steps:
s1, taking 10-50 ml of ethyl acetate solution for standby under the first identification method, drying by distillation, and dissolving residues in 1-5 ml of ethyl acetate to obtain a test solution;
s2, taking 1-5 g of mulberry leaf control drug, adding 20-100 ml of water, decocting, filtering, washing the filtrate with ethyl acetate, combining ethyl acetate solutions, evaporating to dryness, and adding ethyl acetate into residues to dissolve the residues to obtain the control drug solution.
S3, identifying by thin-layer chromatography, namely, respectively absorbing the two solutions, respectively dropping the two solutions on the same silica gel G thin-layer plate, developing by using toluene-ethyl acetate-formic acid (5:2:1) as a developing agent, taking out, drying in the air, placing under an ultraviolet lamp (365nm) for inspection, and displaying fluorescent main spots with the same color on the positions corresponding to the reference medicinal material chromatogram in the test sample chromatogram;
s4, respectively taking 3 batches of the Chinese medicinal oral preparations, preparing a test solution by the above test preparation method, and performing thin-layer identification to obtain a result: 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 and the chromatogram of the reference product, and the result of methodology test shows that the method is simple, convenient, accurate, stable and good in reproducibility, and can quickly identify the mulberry leaf medicinal material in the Chinese medicinal oral preparation.
Method III
The thin layer liquorice identification method comprises the following steps:
s1, taking 1-5 g of the product, adding 10-100 ml of water, dissolving with ultrasound, filtering, extracting the filtrate with water saturated n-butanol by shaking, combining n-butanol solutions, extracting with sodium hydroxide solution by shaking, combining sodium hydroxide solution layers, adjusting the pH value to 2-6 with hydrochloric acid, extracting with ethyl acetate by shaking, combining ethyl acetate solutions, steaming to dry, and dissolving the residue with methanol to obtain a sample solution;
s2, taking 1-5 g of licorice contrast drug, adding 10-100 ml of water, decocting for 20-50 minutes, filtering, extracting with water saturated n-butanol, combining n-butanol liquid, the rest operations are the same as the preparation method of the sample, dissolving residue with methanol to serve as contrast drug solution, taking liquiritin contrast, adding methanol to prepare 1-5 mg of solution per 1ml to serve as contrast solution;
s3, identifying by thin-layer chromatography, namely sucking 1-10 mu l of each solution, respectively dropping the solution on the same silica gel G thin-layer plate, developing by using chloroform-methanol-water (13:7:2) as a developing agent, taking out, drying in the air, spraying 10% sulfuric acid ethanol solution, heating at 105 ℃ until the color development of spots is clear, respectively viewing by using sunlight and ultraviolet lamps (365nm), displaying spots or fluorescent spots with the same color on the positions corresponding to the color spectrum of a reference drug in the color spectrum of a test product, and displaying the same orange yellow fluorescent spots on the positions corresponding to the color spectrum of the reference drug;
s4, respectively taking 15 batches of the Chinese medicinal oral preparation, preparing a test solution by the same test preparation method, and performing thin-layer identification to obtain a result: in the chromatogram of the test solution, spots or fluorescent spots with the same color appear at the corresponding positions of the chromatogram of the reference medicinal material; the same orange yellow fluorescent spots are displayed at the positions corresponding to the chromatogram of the reference substance, and the methodological test result shows that the method is simple, convenient, accurate, stable and good in reproducibility, and can quickly identify the licorice medicinal material in the Chinese medicinal oral preparation.
Method IV
The fried bitter almond thin-layer identification method comprises the following steps:
s1, taking 1-5 g of the product, adding 10-100 ml of methanol, carrying out ultrasonic treatment for 10-50 minutes, filtering, evaporating filtrate to dryness, dissolving residues by adding 1-10 ml of water, passing through a macroporous adsorption resin column, respectively adding 10-50 ml of water and 10-50 ml of ammonia solution for elution, eluting by using ethanol, collecting eluent, evaporating to dryness, dissolving residues by adding acetone, and taking supernate as a test solution;
s2, adding methanol into amygdalin as reference substance to obtain 1-5 mg/1 ml solution as reference substance solution;
s3, identifying by thin-layer chromatography, namely respectively sucking 1-10 mu l of the solutions, respectively dropping the solutions on the same silica gel G thin-layer plate, respectively taking the upper layer solution of n-butyl alcohol-acetic acid-water (19:1:5) as a developing agent, developing, taking out, drying in the air, spraying a 10% sulfuric acid ethanol solution of 2% phosphomolybdic acid, heating at 105 ℃ until spots are clearly developed, and displaying main spots with the same color on positions corresponding to the reference medicine chromatogram and the reference substance chromatogram in the test substance chromatogram;
s4, preparing 15 batches of the Chinese medicinal oral preparation into a test sample solution by the same test sample preparation method, and performing thin-layer identification to obtain a result: in the chromatogram of the test sample, spots with the same color appear at the corresponding positions of the chromatogram of the reference medicinal material and the chromatogram of the reference product, and the result of the methodological test shows that the method is simple, convenient, accurate, stable and good in reproducibility, and can quickly identify the fried bitter almond medicinal material in the Chinese medicinal oral preparation.
Method five
The method for identifying the melia japonica leaves by using the thin layer comprises the following steps:
s1, taking 1-5 g of the product, adding 10-100 ml of water to dissolve the product, adjusting the pH value to 8-11 with a sodium hydroxide test solution, shaking and extracting with ethyl acetate, combining ethyl acetate solutions, evaporating to dryness, and adding 1ml of methanol to dissolve residues to obtain a test solution;
s2, taking 1-5 g of loquat leaf control medicinal material, adding 10-100 ml of water, decocting, filtering, adjusting the pH value of the filtrate to 8-11 by using sodium hydroxide test solution, preparing loquat leaf control medicinal material solution by the same method, taking bear fruit acid control, adding methanol to prepare 0.1-0.5 mg of solution in each 1ml as control solution;
s3, identifying by thin layer chromatography, namely respectively sucking 5 μ l of each of the four solutions, respectively dropping the four solutions on the same silica gel G thin layer plate, developing with toluene-ethyl acetate-formic acid (10:2:0.2) as a developing agent, taking out, drying by airing, spraying with 10% sulfuric acid ethanol solution, heating at 105 ℃ until the spots are clearly developed, and inspecting by an ultraviolet lamp (365 nm);
s4, the test sample chromatogram shows fluorescence spots with the same color at the corresponding positions of the reference drug chromatogram and the reference sample chromatogram.
In conclusion, the detection steps and the thin-layer chromatography identification method are not only suitable for detecting the traditional Chinese medicine oral preparation of the granules, but also suitable for detecting capsules, oral preparations, tablets and the like.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the scope of the present invention, and the technical solutions and the inventive concepts of the present invention are equivalent to or changed within the technical scope of the present invention.
Claims (6)
1. A thin-layer chromatography identification method of a traditional Chinese medicine oral preparation comprises the traditional Chinese medicine oral preparation, and is characterized in that the traditional Chinese medicine oral preparation comprises ginseng, mulberry leaf, liquorice, fried bitter apricot kernel and loquat leaf.
2. The thin-layer chromatography identification method of the traditional Chinese medicine oral preparation according to claim 1, wherein the ginseng thin-layer chromatography identification method comprises the following steps:
s1, taking 1-5 g of the decoction particles of the decoction for removing the dryness and relieving the lung, adding 10-100 ml of water, ultrasonically dissolving, filtering, washing the filtrate with ethyl acetate, shaking and extracting the water solution with water saturated n-butyl alcohol, combining the n-butyl alcohol solution, washing with a sodium hydroxide solution, discarding the sodium hydroxide solution, washing with water saturated n-butyl alcohol, discarding the water solution, evaporating the n-butyl alcohol solution to dryness, and dissolving the residue with methanol to obtain a test solution;
s2, taking 1-5 g of ginseng reference drug, adding 20-100 ml of water, decocting, filtering, preparing a reference drug solution by the same method, taking a ginsenoside Rb1 reference substance, a ginsenoside Re reference substance, a ginsenoside Rf reference substance and a ginsenoside Rg1 reference substance, and adding methanol to prepare a mixed solution as a reference substance solution;
s3, identifying by thin-layer chromatography, namely respectively sucking 1-2 μ l of each of the three solutions, respectively dropping the three solutions on the same silica gel G thin-layer plate, developing by using chloroform-methanol-water (13:7:2) as a developing agent, taking out, drying in the air, spraying 10% sulfuric acid ethanol solution, heating at 105 ℃ until the color development of spots is clear, respectively inspecting under sunlight and an ultraviolet lamp (365nm), and respectively displaying spots or fluorescent spots with the same color on positions corresponding to the reference drug chromatogram and the reference sample chromatogram in the sample chromatogram;
s4, respectively taking 3 batches of the Chinese medicinal oral preparation, preparing a test solution by the same test preparation method, and performing thin-layer identification.
3. The thin-layer chromatography identification method of the traditional Chinese medicine oral preparation according to claim 1, wherein the mulberry leaf thin-layer chromatography identification method comprises the following steps:
s1, taking 10-50 ml of ethyl acetate solution for the thin-layer identification method of the identified ginseng, evaporating to dryness, and dissolving the residue in 1-5 ml of ethyl acetate to obtain a test solution;
s2, taking 1-5 g of mulberry leaf control medicinal material, adding 20-100 ml of water, decocting, filtering, washing the filtrate with ethyl acetate, combining ethyl acetate solutions, evaporating to dryness, and adding ethyl acetate into residues to dissolve the residues to obtain a control medicinal material solution;
s3, identifying by thin-layer chromatography, namely, respectively absorbing the two solutions, respectively dropping the two solutions on the same silica gel G thin-layer plate, developing by using toluene-ethyl acetate-formic acid (5:2:1) as a developing agent, taking out, drying in the air, and placing under an ultraviolet lamp (365nm) for inspection, wherein in the chromatogram of the test sample, the main fluorescent spots with the same color are displayed at the positions corresponding to the chromatograms of the reference medicinal materials;
s4, respectively taking 3 batches of the Chinese medicinal oral preparation, preparing a test solution by the same test preparation method, and performing thin-layer identification.
4. The thin-layer chromatography identification method of the traditional Chinese medicine oral preparation according to claim 1, characterized in that the thin-layer chromatography identification method of liquorice comprises the following steps:
s1, taking 1-5 g of the product, adding 10-100 ml of water, dissolving with ultrasound, filtering, extracting the filtrate with water saturated n-butanol under shaking, combining n-butanol solutions, extracting with sodium hydroxide solution under shaking, combining sodium hydroxide solution layers, adjusting the pH value to 2-6 with hydrochloric acid, extracting with ethyl acetate under shaking, combining ethyl acetate solutions, evaporating to dryness, and dissolving the residue with methanol to obtain a test solution;
s2, taking 1-5 g of licorice contrast drug, adding 10-100 ml of water, decocting for 20-50 minutes, filtering, extracting with water saturated n-butanol, combining n-butanol solution, the other operations are the same as the preparation method of the sample, dissolving the residue with methanol to serve as contrast drug solution, taking the liquiritin contrast drug, adding methanol to prepare 1-5 mg of solution per 1ml to serve as contrast solution;
s3, identifying by thin-layer chromatography, namely, sucking 1-10 mu l of each solution, respectively dropping the solution on the same silica gel G thin-layer plate, developing by using chloroform-methanol-water (13:7:2) as a developing agent, taking out, drying in the air, spraying 10% sulfuric acid ethanol solution, heating at 105 ℃ until the color development of spots is clear, respectively viewing the spots under sunlight and ultraviolet lamps (365nm), displaying the spots or fluorescent spots with the same color on the positions corresponding to the color spectrum of a reference drug in the color spectrum of a test product, and displaying the same orange yellow fluorescent spots on the positions corresponding to the color spectrum of the reference drug;
s4, taking 15 batches of oral Chinese medicinal preparations, preparing test solution by the same method for preparing the test, and performing thin-layer identification.
5. The thin-layer chromatography identification method of a traditional Chinese medicine oral preparation according to claim 1, wherein the thin-layer chromatography identification method of fried bitter apricot kernels comprises the following steps:
s1, taking 1-5 g of the product, adding 10-100 ml of methanol, carrying out ultrasonic treatment for 10-50 minutes, filtering, evaporating filtrate to dryness, dissolving residues with 1-10 ml of water, passing through a macroporous adsorption resin column, respectively adding 10-50 ml of water and 10-50 ml of ammonia solution for elution, eluting with ethanol, collecting eluent, evaporating to dryness, dissolving residues with acetone, and taking supernate as a test solution;
s2, adding methanol into amygdalin as reference substance to obtain 1-5 mg/1 ml solution as reference substance solution;
s3, identifying by thin layer chromatography, namely respectively sucking 1-10 mul of the solutions, respectively dropping the solutions on the same silica gel G thin layer plate, respectively taking the upper layer solution of n-butyl alcohol-acetic acid-water (19:1:5) as a developing agent, developing, taking out, drying in the air, spraying a 10% sulfuric acid ethanol solution of 2% phosphomolybdic acid, and heating at 105 ℃ until spots are clearly developed. In the chromatogram of the test solution, main spots with the same color appear at the positions corresponding to the chromatogram of the reference solution and the chromatogram of the reference solution;
s4, taking 15 batches of oral Chinese medicinal preparations, preparing test solution by the same method for preparing the test, and performing thin-layer identification.
6. The TLC identification method of the oral traditional Chinese medicine preparation according to claim 1, wherein the TLC identification method of the leaves of eriobotrya japonica comprises the following steps:
s1, taking 1-5 g of the product, adding 10-100 ml of water to dissolve the product, adjusting the pH value to 8-11 with a sodium hydroxide test solution, shaking and extracting with ethyl acetate, combining ethyl acetate solutions, evaporating to dryness, and adding 1ml of methanol to dissolve residues to obtain a test solution;
s2, taking 1-5 g of loquat leaf control medicinal material, adding 10-100 ml of water, decocting, filtering, adjusting the pH value of the filtrate to 8-11 by using sodium hydroxide test solution, preparing loquat leaf control medicinal material solution by the same method, taking ursolic acid control, adding methanol to prepare 0.1-0.5 mg of solution in each 1ml as control solution;
s3, identifying by thin layer chromatography, respectively sucking 5 μ l of each of the four solutions, respectively dropping on the same silica gel G thin layer plate, developing with toluene-ethyl acetate-formic acid (10:2:0.2) as developing agent, taking out, air drying, spraying 10% sulfuric acid ethanol solution, heating at 105 deg.C until the spots are clearly developed, and inspecting with ultraviolet lamp (365 nm).
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113759034A (en) * | 2021-07-22 | 2021-12-07 | 广东一方制药有限公司 | Establishing method of ophiopogon japonicus soup substance standard |
| CN114740136A (en) * | 2022-04-28 | 2022-07-12 | 广西壮族自治区食品药品检验所 | Quality detection method of panax notoginseng medicinal material |
| CN114740136B (en) * | 2022-04-28 | 2024-03-19 | 广西壮族自治区食品药品检验所 | Quality detection method of pseudo-ginseng medicinal material |
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