CN111693641A - Thin-layer identification method for renshu stomach-invigorating granules - Google Patents
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Abstract
The invention discloses a thin-layer identification method of Renzhu stomach-invigorating granules, which comprises identification of a zedoary medicinal material, identification of a coix seed medicinal material, identification of baicalin, identification of a bighead atractylodes rhizome medicinal material, identification of spreading hedyotis herb, identification of hairyvein agrimony and identification of Chinese lobelia herb. The thin-layer identification method of the Renzhu stomach-invigorating granules provided by the invention screens out the optimal preparation process of a sample and the optimal conditions of thin-layer chromatography identification for each medicinal material, has reasonable process design and strong operability, can accurately identify the Atractylodes macrocephala, the coix seed, the scutellaria baicalensis, the agrimony, the zedoary, the Chinese lobelia and the oldenlandia diffusa, has high identification speed, high identification accuracy and low detection cost, and has important significance in the quality control of the Renzhu stomach-invigorating granules and the guarantee of the clinical efficacy of the Renzhu stomach-invigorating granules.
Description
Technical Field
The invention relates to an identification method of a traditional Chinese medicine preparation, in particular to a thin-layer identification method of a Renzhu stomach-invigorating granule, belonging to the technical field of quality detection of traditional Chinese medicine preparations.
Background
The Renzhu stomach invigorating granule is researched and developed by professor sovereign single Mega of head people in the scientific operation of the spleen and stomach diseases of national traditional Chinese medicine and Jiangsu province traditional Chinese medicine institute (national traditional Chinese medicine spleen and stomach disease clinical research base), the professor single Mega of more than forty years provides that the main pathogenesis characteristic of the precancerous lesion of the gastric mucosa of atrophic gastritis is qi deficiency, blood stasis and heat depression, the main treatment rule of tonifying qi, activating blood and clearing heat is formulated, the Renzhu stomach invigorating granule is researched and developed, and the preparation in the institute is prepared from traditional Chinese medicines of astragalus, bighead atractylodes rhizome, coix seed, scutellaria baicalensis, hairyvein agrimony, curcuma zedoary, Chinese lobelia and oldenlandia. Multiple studies show that the Renzhu stomach invigorating granules have good curative effect on atrophic gastritis and precancerous lesion of gastric mucosa, the medicine has been used as an application basis of preparations in traditional Chinese medicine hospitals in Jiangsu province for more than twenty years, and about 100 ten thousand boxes are used in the past 9 months in 2004; the using amount of the traditional Chinese medicine composition in 2019 is about 20 ten thousand boxes, and the traditional Chinese medicine composition has a very good clinical curative effect. However, the preparation has not been provided with a comprehensive, objective and multi-index quality evaluation method. The invention provides a thin-layer detection method for detecting various components of the kernel stomach strengthening granules, which is simple to operate and low in detection cost.
Disclosure of Invention
The purpose of the invention is as follows: the invention aims to overcome the defects of the prior art and provide a thin-layer detection method which is simple to operate and low in detection cost and is used for detecting various components of the kernel stomach strengthening granules.
The technical scheme is as follows: in order to achieve the above purpose, the invention adopts the technical scheme that:
a thin-layer identification method for renshu stomach-invigorating granules comprises the following steps:
(1) identification of zedoary turmeric
(2) Coix seed medicinal material identification
(3) Identification of baicalin
(4) Identification of rhizoma Atractylodis Macrocephalae
(5) Identification of spreading hedyotis herb
(6) Agrimonia pilosa ledeb identification
(7) And identifying the Chinese lobelia.
Specifically, the thin-layer identification method for the nucleolus stomachic granules comprises the following steps:
(1) identification of zedoary turmeric
Adding petroleum ether into Curcumae rhizoma powder, ultrasonic treating, filtering, and concentrating the filtrate to obtain sample solution; preparing Curcumae rhizoma reference medicinal material powder, and preparing reference medicinal material solution by the same method; performing thin layer chromatography test, sucking the sample solution and the reference solution, respectively dropping on the same silica gel G thin layer plate, developing with petroleum ether-ethyl acetate as developing agent, taking out, air drying, and spraying vanillin sulfuric acid ethanol solution; spots of the same color appear in the chromatogram of the test solution at the positions corresponding to those in the chromatogram of the reference solution; (2) coix seed medicinal material identification
Adding petroleum ether into Coicis semen powder, ultrasonic treating, filtering, and collecting filtrate as sample solution; preparing a reference medicinal material of semen Coicis, and preparing a reference medicinal solution by the same method; performing thin-layer chromatography test, sucking Coicis semen sample solution and control medicinal material solution, respectively dropping on the same silica gel G thin-layer plate, developing with petroleum ether-diethyl ether-glacial acetic acid as developing agent, taking out, air drying, spraying vanillin sulphuric acid ethanol solution, heating until the color development of spots is clear, and in the sample chromatogram, spots with the same pigment color appear at the position corresponding to the control extract chromatogram;
(3) identification of baicalin
Taking scutellaria baicalensis powder, adding methanol, heating and refluxing, filtering, evaporating filtrate to dryness, dissolving residues in water, adjusting the pH value to about 2-3 by using dilute hydrochloric acid, shaking and extracting by using ethyl acetate, combining extracting solutions, evaporating to dryness, and dissolving residues in methanol to obtain a test solution; adding methanol into baicalin reference substance to obtain baicalin reference substance solution; absorbing the above two solutions, respectively dropping on the same silica gel G thin layer plate, developing with ethyl acetate-butanone-formic acid-water as developing agent, taking out, air drying, spraying ferric trichloride ethanol solution, and allowing spots of the same color to appear in the chromatogram of the test solution at the positions corresponding to those of the chromatogram of the control solution;
(4) identification of rhizoma Atractylodis Macrocephalae
Taking rhizoma Atractylodis Macrocephalae, adding ethanol, performing ultrasonic treatment, filtering, evaporating filtrate to dryness, and dissolving residue with ethanol to obtain rhizoma Atractylodis test solution; preparing Atractylodis rhizoma reference material, and making reference material solution by the same method; sucking rhizoma Atractylodis Macrocephalae sample solution and control solution, and respectively dropping on the same silica gel G thin layer plate by thin layer chromatography, adding petroleum ether: developing with ethyl acetate as developing agent, taking out, air drying, and inspecting under ultraviolet lamp; in the chromatogram of the test solution, fluorescent spots with the same color appear at the corresponding positions of the chromatogram of the reference solution;
(5) identification of spreading hedyotis herb
Taking oldenlandia diffusa powder, adding normal hexane, carrying out ultrasonic treatment and filtering, and taking filtrate as oldenlandia diffusa test solution; taking another Atractylodis rhizoma reference medicinal material, preparing reference medicinal material solution by the same method, subjecting to thin layer chromatography, sucking herba Hedyotidis Diffusae sample solution and reference medicinal material solution, respectively dropping on the same silica gel G thin layer plate, developing with petroleum ether-ethyl acetate as developing agent, taking out, air drying, spraying vanillin-sulfuric acid ethanol solution, and heating until spots appear clearly; spots of the same color appear in the chromatogram of the test solution at the positions corresponding to those in the chromatogram of the reference solution;
(6) agrimonia pilosa ledeb identification
Taking hairyvein agrimony powder, adding petroleum ether, carrying out ultrasonic treatment, filtering, evaporating filtrate to dryness, dissolving residues by adding trichloromethane, extracting by using an oxygen sodium oxide solution, discarding three-peaches liquid, adjusting the pH value to 1-2 by using dilute hydrochloric acid, shaking and extracting by using three-hydrogen methane, combining the three-peaches liquid, adding water for washing, discarding water liquid, concentrating the three-peaches liquid, and taking the three-peaches liquid as a hairyvein agrimony test solution; preparing herba et Gemma Agrimoniae control medicinal material by the same method; taking a hairyvein agrimony phenol B reference substance, and adding three peaches to prepare a hairyvein agrimony phenol B reference substance solution; according to thin and thick chromatography, sucking the three agrimony test solution, agrimony reference medicinal material solution and agrimophol B reference solution, respectively dropping on -silica gel G thin layer plate, developing with petroleum ether-acetic acid ethyl alcohol-acetic acid upper layer solution as developing agent, taking out, air drying, spraying sulfuric acid ethanol solution, and heating until the spots are clearly developed; spots of the same color appear in the chromatogram of the test solution at the positions corresponding to the chromatograms of the reference medicinal material and the reference solution;
(7) identification of Chinese Lobelia
Taking the Chinese lobelia powder, adding methanol for ultrasonic treatment, cooling and filtering, evaporating the filtrate to dryness and dissolving the residue methanol to obtain a Chinese lobelia test solution; preparing herba Lobeliae chinensis control medicinal material, and making into herba Lobeliae chinensis control medicinal material solution by the same method; according to thin-layer chromatography, sucking the herba Lobeliae chinensis sample solution and herba Lobeliae chinensis control solution, respectively dropping on the same silica gel G thin-layer plate, developing with trimethyl-methanol as developing agent, taking out, air drying, and heating with ethanol sulfate solution until the color spot is clearly developed, and respectively inspecting under sunlight and ultraviolet lamp; in the chromatogram of the test solution, spots or fluorescent spots of the same color appear at the corresponding positions of the chromatogram of the reference solution.
Preferably, the thin-layer identification method of the kernel stomach strengthening granule comprises the following steps:
(1) identification of zedoary turmeric
Taking 5g of curcuma zedoary powder, adding 30ml of petroleum ether, carrying out ultrasonic treatment for 20 minutes, filtering, and concentrating the filtrate to 1ml to be used as a curcuma zedoary test solution; preparing Curcumae rhizoma control medicinal material solution by the same method with 1g of Curcumae rhizoma control medicinal material powder; performing thin layer chromatography test, sucking the two solutions, respectively dropping on the same silica gel G thin layer plate, developing with petroleum ether-ethyl acetate as developing agent at volume ratio of 10:1, taking out, air drying, and spraying 5% vanillin sulfuric acid ethanol solution; spots of the same color appear in the chromatogram of the test sample and the reference material;
(2) coix seed medicinal material identification
Taking 5g of semen Coicis powder, adding 30ml of petroleum ether, performing ultrasonic treatment for 30 min, filtering, collecting filtrate as semen Coicis sample solution, taking 1g of semen Coicis control material, and preparing semen Coicis control material solution by the same method; according to the thin layer chromatography test, 5 mul of each solution is sucked up and respectively spotted on the same silica gel G thin layer plate, and the volume ratio of the solution to the solution is 83: 17: 1, developing, taking out, airing, spraying a 5% vanillin 10% sulfuric acid ethanol solution, heating at 105 ℃ until the color development of spots is clear, and displaying spots with the same pigment color at the positions corresponding to the color spectrum of the control extract in the color spectrum of a test sample;
(3) identification of baicalin
Collecting Scutellariae radix powder 5g, adding methanol 50ml, heating under reflux for 1 hr, filtering, evaporating filtrate to dryness, dissolving residue with water 20ml, adjusting pH to about 2 with dilute hydrochloric acid, extracting with ethyl acetate under shaking for 2 times (20 ml each time), mixing extractive solutions, evaporating to dryness, dissolving residue with methanol 5ml to obtain Scutellariae radix sample solution; adding methanol into baicalin control to obtain 1mg solution per 1ml as baicalin control solution; performing thin layer chromatography test, sucking the above two solutions 5 μ l each, dropping on the same silica gel G thin layer plate respectively, developing with ethyl acetate-butanone-formic acid-water as developing agent at volume ratio of 5:3:1:1, taking out, air drying, and spraying with 2% ferric trichloride ethanol solution; spots with the same color appear on the chromatogram of the test solution at the positions corresponding to the chromatograms of the reference solution;
(4) identification of rhizoma Atractylodis Macrocephalae
Taking 5g of rhizoma atractylodis macrocephalae, adding 20ml of ethanol, carrying out ultrasonic treatment for 30 minutes, filtering, evaporating filtrate to dryness, and adding 2ml of ethanol into residues to dissolve the residues to obtain a rhizoma atractylodis macrocephalae test sample solution; preparing 1g of rhizoma Atractylodis Macrocephalae control medicinal material into rhizoma Atractylodis control medicinal material solution by the same method; and (3) performing thin-layer chromatography test, sucking 5 mu l of each of the two solutions, respectively dropping the two solutions on the same silica gel G thin-layer plate, and mixing the two solutions in a volume ratio of 5:1 petroleum ether: developing with ethyl acetate as developing agent, taking out, air drying, and inspecting under 365nm ultraviolet lamp; in the chromatogram of the test solution, fluorescent spots with the same color appear at the corresponding positions of the chromatogram of the reference solution;
(5) identification of spreading hedyotis herb
Taking 5g of spreading hedyotis herb powder, adding 20ml of normal hexane, carrying out ultrasonic treatment for 15 minutes, filtering, and taking filtrate as spreading hedyotis herb test solution; preparing herba Hedyotidis Diffusae control solution with 0.5g Atractylodis rhizoma control; according to the thin layer chromatography test, 5 mul of each solution is sucked up and respectively spotted on the same silica gel G thin layer plate, and the volume ratio is 50: 1, developing by using petroleum ether-ethyl acetate as a developing agent, taking out, airing, spraying a 5% vanillin sulfuric acid ethanol solution, and heating until spots are clearly developed; spots of the same color appear in the chromatogram of the test solution at the positions corresponding to those in the chromatogram of the reference solution;
(6) agrimonia pilosa ledeb identification
Taking 5g of hairyvein agrimony powder, adding 40ml of petroleum ether, carrying out ultrasonic treatment for 30 minutes, filtering, and evaporating filtrate to dryness; dissolving residues with 10ml of trichloromethane, extracting with 10ml of 5% sodium oxide solution, discarding three peaches of methylene liquid, adjusting the pH value to 1-2 with dilute hydrochloric acid, shaking with three-hydrogen methane to extract for 2 times, combining the three peaches of methane, adding 10ml of water for washing, discarding water liquid, concentrating the three peaches of methylene liquid to 1ml, and using the three peaches of methylene liquid as a hairyvein agrimony test solution; preparing herba et Gemma Agrimoniae control solution by the same method, except that 2g herba et Gemma Agrimoniae control solution is prepared; taking a hairyvein agrimony phenol B reference substance, and adding three methane to prepare a hairyvein agrimony phenol B solution containing 0.5mg per 1ml, wherein the hairyvein agrimony phenol B solution is used as the hairyvein agrimony phenol B reference substance solution; according to the thin and thick chromatography test, respectively dropping 10 microliters of each of the three solutions on silica gel G thin layer plates, taking the upper layer solution of petroleum ether-acetic acid ethyl acetate-acetic acid as a developing agent in a volume ratio of 100:9:5, developing, taking out, airing, spraying with 10% sulfuric acid ethanol solution, and performing the following steps at 105 ℃: heating until the spots are clearly developed; spots of the same color appear in the chromatogram of the test solution at the positions corresponding to the chromatograms of the reference medicinal material and the reference solution;
(7) identification of Chinese Lobelia
Taking 5g of Chinese lobelia powder, adding 50ml of methanol, carrying out ultrasonic treatment for 30 minutes, cooling and filtering, evaporating filtrate to dryness, and dissolving 2ml of residue methanol to obtain a Chinese lobelia sample solution; preparing herba Lobeliae chinensis reference medicinal material lg, and preparing reference medicinal material solution by the same method; performing thin layer chromatography test, sucking the above two solutions 5 μ l each, respectively dropping on the same silica gel G thin layer plate, developing with chloroform-methanol at volume ratio of 9:1 as developing agent, taking out, air drying, spraying 10% ethanol sulfate solution, heating at 105 deg.C until the color development of spots is clear, respectively placing under sunlight and ultraviolet lamp 365nm for inspection, and displaying spots or fluorescent spots of the same color in the chromatogram of the test product at the position corresponding to the chromatogram of the control medicinal material.
Has the advantages that: the thin-layer identification method of the nucleolus stomachic granules provided by the invention has the following advantages:
the thin-layer identification method of the Renzhu stomach-invigorating granules provided by the invention screens out the optimal preparation process of a sample and the optimal conditions of thin-layer chromatography identification for each medicinal material, has reasonable process design and strong operability, can accurately identify the Atractylodes macrocephala, the coix seed, the scutellaria baicalensis, the agrimony, the zedoary, the Chinese lobelia and the oldenlandia diffusa, has high identification speed, high identification accuracy and low detection cost, and has important significance in the quality control of the Renzhu stomach-invigorating granules and the guarantee of the clinical efficacy of the Renzhu stomach-invigorating granules.
Drawings
FIG. 1 is a thin-layer identification chart of Curcumae rhizoma.
FIG. 2 is a thin-layer identification chart of Coicis semen.
FIG. 3 is a thin layer identification chart of Scutellariae radix.
FIG. 4 is a thin-layer identification chart of Atractylodis rhizoma.
Detailed Description
The present invention is described in detail below by way of examples, which should not be construed as limiting the invention.
Example 1
The thin-layer identification method of the kernel technique stomach-invigorating granules comprises the following steps:
(1) identification of zedoary turmeric
Taking 5g of curcuma zedoary powder, adding 30ml of petroleum ether, carrying out ultrasonic treatment for 20 minutes, filtering, and concentrating the filtrate to 1ml to be used as a curcuma zedoary test solution; preparing Curcumae rhizoma control medicinal material solution by the same method with 1g of Curcumae rhizoma control medicinal material powder; performing thin layer chromatography test, sucking the two solutions, respectively dropping on the same silica gel G thin layer plate, developing with petroleum ether-ethyl acetate as developing agent at volume ratio of 10:1, taking out, air drying, and spraying 5% vanillin sulfuric acid ethanol solution; spots of the same color appear in the chromatogram of the test sample and the reference material; as shown in fig. 1.
(2) Coix seed medicinal material identification
Taking 5g of semen Coicis powder, adding 30ml of petroleum ether, performing ultrasonic treatment for 30 min, filtering, collecting filtrate as semen Coicis sample solution, taking 1g of semen Coicis control material, and preparing semen Coicis control material solution by the same method; according to the thin layer chromatography test, 5 mul of each solution is sucked up and respectively spotted on the same silica gel G thin layer plate, and the volume ratio of the solution to the solution is 83: 17: 1, developing, taking out, airing, spraying a 5% vanillin 10% sulfuric acid ethanol solution, heating at 105 ℃ until the color development of spots is clear, and displaying spots with the same pigment color at the positions corresponding to the color spectrum of the control extract in the color spectrum of a test sample; as shown in fig. 2.
(3) Identification of baicalin
Collecting Scutellariae radix powder 5g, adding methanol 50ml, heating under reflux for 1 hr, filtering, evaporating filtrate to dryness, dissolving residue with water 20ml, adjusting pH to about 2 with dilute hydrochloric acid, extracting with ethyl acetate under shaking for 2 times (20 ml each time), mixing extractive solutions, evaporating to dryness, dissolving residue with methanol 5ml to obtain Scutellariae radix sample solution; adding methanol into baicalin control to obtain 1mg solution per 1ml as baicalin control solution; performing thin layer chromatography test, sucking the above two solutions 5 μ l each, dropping on the same silica gel G thin layer plate respectively, developing with ethyl acetate-butanone-formic acid-water as developing agent at volume ratio of 5:3:1:1, taking out, air drying, and spraying with 2% ferric trichloride ethanol solution; spots with the same color appear on the chromatogram of the test solution at the positions corresponding to the chromatograms of the reference solution; as shown in fig. 3.
(4) Identification of rhizoma Atractylodis Macrocephalae
Taking 5g of rhizoma atractylodis macrocephalae, adding 20ml of ethanol, carrying out ultrasonic treatment for 30 minutes, filtering, evaporating filtrate to dryness, and adding 2ml of ethanol into residues to dissolve the residues to obtain a rhizoma atractylodis macrocephalae test sample solution; preparing 1g of rhizoma Atractylodis Macrocephalae control medicinal material into rhizoma Atractylodis control medicinal material solution by the same method; and (3) performing thin-layer chromatography test, sucking 5 mu l of each of the two solutions, respectively dropping the two solutions on the same silica gel G thin-layer plate, and mixing the two solutions in a volume ratio of 5:1 petroleum ether: developing with ethyl acetate as developing agent, taking out, air drying, and inspecting under 365nm ultraviolet lamp; in the chromatogram of the test solution, fluorescent spots with the same color appear at the corresponding positions of the chromatogram of the reference solution; as shown in fig. 4.
(5) Identification of spreading hedyotis herb
Taking 5g of spreading hedyotis herb powder, adding 20ml of normal hexane, carrying out ultrasonic treatment for 15 minutes, filtering, and taking filtrate as spreading hedyotis herb test solution; preparing herba Hedyotidis Diffusae control solution with 0.5g Atractylodis rhizoma control; according to the thin layer chromatography test, 5 mul of each solution is sucked up and respectively spotted on the same silica gel G thin layer plate, and the volume ratio is 50: 1, developing by using petroleum ether-ethyl acetate as a developing agent, taking out, airing, spraying a 5% vanillin sulfuric acid ethanol solution, and heating until spots are clearly developed; spots of the same color appear in the chromatogram of the test solution at the positions corresponding to those in the chromatogram of the reference solution;
(6) agrimonia pilosa ledeb identification
Taking 5g of hairyvein agrimony powder, adding 40ml of petroleum ether, carrying out ultrasonic treatment for 30 minutes, filtering, and evaporating filtrate to dryness; dissolving residues with 10ml of trichloromethane, extracting with 10ml of 5% sodium oxide solution, discarding three peaches of methylene liquid, adjusting the pH value to 1-2 with dilute hydrochloric acid, shaking with three-hydrogen methane to extract for 2 times, combining the three peaches of methane, adding 10ml of water for washing, discarding water liquid, concentrating the three peaches of methylene liquid to 1ml, and using the three peaches of methylene liquid as a hairyvein agrimony test solution; preparing herba et Gemma Agrimoniae control solution by the same method, except that 2g herba et Gemma Agrimoniae control solution is prepared; taking a hairyvein agrimony phenol B reference substance, and adding three methane to prepare a hairyvein agrimony phenol B solution containing 0.5mg per 1ml, wherein the hairyvein agrimony phenol B solution is used as the hairyvein agrimony phenol B reference substance solution; according to the thin and thick chromatography test, respectively dropping 10 microliters of each of the three solutions on silica gel G thin layer plates, taking the upper layer solution of petroleum ether-acetic acid ethyl acetate-acetic acid as a developing agent in a volume ratio of 100:9:5, developing, taking out, airing, spraying with 10% sulfuric acid ethanol solution, and performing the following steps at 105 ℃: heating until the spots are clearly developed; spots of the same color appear in the chromatogram of the test solution at the positions corresponding to the chromatograms of the reference medicinal material and the reference solution;
(7) identification of Chinese Lobelia
Taking 5g of Chinese lobelia powder, adding 50ml of methanol, carrying out ultrasonic treatment for 30 minutes, cooling and filtering, evaporating filtrate to dryness, and dissolving 2ml of residue methanol to obtain a Chinese lobelia sample solution; preparing herba Lobeliae chinensis reference medicinal material lg, and preparing reference medicinal material solution by the same method; performing thin layer chromatography test, sucking the above two solutions 5 μ l each, respectively dropping on the same silica gel G thin layer plate, developing with chloroform-methanol at volume ratio of 9:1 as developing agent, taking out, air drying, spraying 10% ethanol sulfate solution, heating at 105 deg.C until the color development of spots is clear, respectively placing under sunlight and ultraviolet lamp 365nm for inspection, and displaying spots or fluorescent spots of the same color in the chromatogram of the test product at the position corresponding to the chromatogram of the control medicinal material.
The thin-layer identification method is adopted, so that the medicinal materials can be quickly and accurately identified, and the thin-layer identification method has important application value for ensuring the quality and the clinical curative effect.
Claims (3)
1. A thin-layer identification method for renshu stomach-invigorating granules is characterized by comprising the following steps:
(1) identification of zedoary turmeric
(2) Coix seed medicinal material identification
(3) Identification of baicalin
(4) Identification of rhizoma Atractylodis Macrocephalae
(5) Identification of spreading hedyotis herb
(6) Agrimonia pilosa ledeb identification
(7) And identifying the Chinese lobelia.
2. The method for identifying the lamina of the renzhu stomach-invigorating granule as claimed in claim 1, comprising the steps of:
(1) identification of zedoary turmeric
Adding petroleum ether into Curcumae rhizoma powder, ultrasonic treating, filtering, and concentrating the filtrate to obtain sample solution; preparing Curcumae rhizoma reference medicinal material powder, and preparing reference medicinal material solution by the same method; performing thin layer chromatography test, sucking the sample solution and the reference solution, respectively dropping on the same silica gel G thin layer plate, developing with petroleum ether-ethyl acetate as developing agent, taking out, air drying, and spraying vanillin sulfuric acid ethanol solution; spots of the same color appear in the chromatogram of the test solution at the positions corresponding to those in the chromatogram of the reference solution;
(2) coix seed medicinal material identification
Adding petroleum ether into Coicis semen powder, ultrasonic treating, filtering, and collecting filtrate as sample solution; preparing a reference medicinal material of semen Coicis, and preparing a reference medicinal solution by the same method; performing thin-layer chromatography test, sucking Coicis semen sample solution and control medicinal material solution, respectively dropping on the same silica gel G thin-layer plate, developing with petroleum ether-diethyl ether-glacial acetic acid as developing agent, taking out, air drying, spraying vanillin sulphuric acid ethanol solution, heating until the color development of spots is clear, and in the sample chromatogram, spots with the same pigment color appear at the position corresponding to the control extract chromatogram;
(3) identification of baicalin
Taking scutellaria baicalensis powder, adding methanol, heating and refluxing, filtering, evaporating filtrate to dryness, dissolving residues in water, adjusting the pH value to about 2-3 by using dilute hydrochloric acid, shaking and extracting by using ethyl acetate, combining extracting solutions, evaporating to dryness, and dissolving residues in methanol to obtain a test solution; adding methanol into baicalin reference substance to obtain baicalin reference substance solution; absorbing the above two solutions, respectively dropping on the same silica gel G thin layer plate, developing with ethyl acetate-butanone-formic acid-water as developing agent, taking out, air drying, spraying ferric trichloride ethanol solution, and allowing spots of the same color to appear in the chromatogram of the test solution at the positions corresponding to those of the chromatogram of the control solution;
(4) identification of rhizoma Atractylodis Macrocephalae
Taking rhizoma Atractylodis Macrocephalae, adding ethanol, performing ultrasonic treatment, filtering, evaporating filtrate to dryness, and dissolving residue with ethanol to obtain rhizoma Atractylodis test solution; preparing Atractylodis rhizoma reference material, and making reference material solution by the same method; sucking rhizoma Atractylodis Macrocephalae sample solution and control solution, and respectively dropping on the same silica gel G thin layer plate by thin layer chromatography, adding petroleum ether: developing with ethyl acetate as developing agent, taking out, air drying, and inspecting under ultraviolet lamp; in the chromatogram of the test solution, fluorescent spots with the same color appear at the corresponding positions of the chromatogram of the reference solution;
(5) identification of spreading hedyotis herb
Taking oldenlandia diffusa powder, adding normal hexane, carrying out ultrasonic treatment and filtering, and taking filtrate as oldenlandia diffusa test solution; taking another Atractylodis rhizoma reference medicinal material, preparing reference medicinal material solution by the same method, subjecting to thin layer chromatography, sucking herba Hedyotidis Diffusae sample solution and reference medicinal material solution, respectively dropping on the same silica gel G thin layer plate, developing with petroleum ether-ethyl acetate as developing agent, taking out, air drying, spraying vanillin-sulfuric acid ethanol solution, and heating until spots appear clearly; spots of the same color appear in the chromatogram of the test solution at the positions corresponding to those in the chromatogram of the reference solution;
(6) agrimonia pilosa ledeb identification
Taking hairyvein agrimony powder, adding petroleum ether, carrying out ultrasonic treatment, filtering, evaporating filtrate to dryness, dissolving residues by adding trichloromethane, extracting by using an oxygen sodium oxide solution, discarding three-peaches liquid, adjusting the pH value to 1-2 by using dilute hydrochloric acid, shaking and extracting by using three-hydrogen methane, combining the three-peaches liquid, adding water for washing, discarding water liquid, concentrating the three-peaches liquid, and taking the three-peaches liquid as a hairyvein agrimony test solution; preparing herba et Gemma Agrimoniae control medicinal material by the same method; taking a hairyvein agrimony phenol B reference substance, and adding three peaches to prepare a hairyvein agrimony phenol B reference substance solution; according to thin and thick chromatography, sucking the three agrimony test solution, agrimony reference medicinal material solution and agrimophol B reference solution, respectively dropping on -silica gel G thin layer plate, developing with petroleum ether-acetic acid ethyl alcohol-acetic acid upper layer solution as developing agent, taking out, air drying, spraying sulfuric acid ethanol solution, and heating until the spots are clearly developed; spots of the same color appear in the chromatogram of the test solution at the positions corresponding to the chromatograms of the reference medicinal material and the reference solution;
(7) identification of Chinese Lobelia
Taking the Chinese lobelia powder, adding methanol for ultrasonic treatment, cooling and filtering, evaporating the filtrate to dryness and dissolving the residue methanol to obtain a Chinese lobelia test solution; preparing herba Lobeliae chinensis control medicinal material, and making into herba Lobeliae chinensis control medicinal material solution by the same method; according to thin-layer chromatography, sucking the herba Lobeliae chinensis sample solution and herba Lobeliae chinensis control solution, respectively dropping on the same silica gel G thin-layer plate, developing with trimethyl-methanol as developing agent, taking out, air drying, and heating with ethanol sulfate solution until the color spot is clearly developed, and respectively inspecting under sunlight and ultraviolet lamp; in the chromatogram of the test solution, spots or fluorescent spots of the same color appear at the corresponding positions of the chromatogram of the reference solution.
3. The method of thin-layer identification of renzhu stomach invigorating granules according to claim 2, comprising the steps of:
(1) identification of zedoary turmeric
Taking 5g of curcuma zedoary powder, adding 30ml of petroleum ether, carrying out ultrasonic treatment for 20 minutes, filtering, and concentrating the filtrate to 1ml to be used as a curcuma zedoary test solution; preparing Curcumae rhizoma control medicinal material solution by the same method with 1g of Curcumae rhizoma control medicinal material powder; performing thin layer chromatography test, sucking the two solutions, respectively dropping on the same silica gel G thin layer plate, developing with petroleum ether-ethyl acetate as developing agent at volume ratio of 10:1, taking out, air drying, and spraying 5% vanillin sulfuric acid ethanol solution; spots of the same color appear in the chromatogram of the test sample and the reference material;
(2) coix seed medicinal material identification
Taking 5g of semen Coicis powder, adding 30ml of petroleum ether, performing ultrasonic treatment for 30 min, filtering, collecting filtrate as semen Coicis sample solution, taking 1g of semen Coicis control material, and preparing semen Coicis control material solution by the same method; according to the thin layer chromatography test, 5 mul of each solution is sucked up and respectively spotted on the same silica gel G thin layer plate, and the volume ratio of the solution to the solution is 83: 17: 1, developing, taking out, airing, spraying a 5% vanillin 10% sulfuric acid ethanol solution, heating at 105 ℃ until the color development of spots is clear, and displaying spots with the same pigment color at the positions corresponding to the color spectrum of the control extract in the color spectrum of a test sample;
(3) identification of baicalin
Collecting Scutellariae radix powder 5g, adding methanol 50ml, heating under reflux for 1 hr, filtering, evaporating filtrate to dryness, dissolving residue with water 20ml, adjusting pH to about 2 with dilute hydrochloric acid, extracting with ethyl acetate under shaking for 2 times (20 ml each time), mixing extractive solutions, evaporating to dryness, dissolving residue with methanol 5ml to obtain Scutellariae radix sample solution; adding methanol into baicalin control to obtain 1mg solution per 1ml as baicalin control solution; performing thin layer chromatography test, sucking the above two solutions 5 μ l each, dropping on the same silica gel G thin layer plate respectively, developing with ethyl acetate-butanone-formic acid-water as developing agent at volume ratio of 5:3:1:1, taking out, air drying, and spraying with 2% ferric trichloride ethanol solution; spots with the same color appear on the chromatogram of the test solution at the positions corresponding to the chromatograms of the reference solution;
(4) identification of rhizoma Atractylodis Macrocephalae
Taking 5g of rhizoma atractylodis macrocephalae, adding 20ml of ethanol, carrying out ultrasonic treatment for 30 minutes, filtering, evaporating filtrate to dryness, and adding 2ml of ethanol into residues to dissolve the residues to obtain a rhizoma atractylodis macrocephalae test sample solution; preparing 1g of rhizoma Atractylodis Macrocephalae control medicinal material into rhizoma Atractylodis control medicinal material solution by the same method; and (3) performing thin-layer chromatography test, sucking 5 mu l of each of the two solutions, respectively dropping the two solutions on the same silica gel G thin-layer plate, and mixing the two solutions in a volume ratio of 5:1 petroleum ether: developing with ethyl acetate as developing agent, taking out, air drying, and inspecting under 365nm ultraviolet lamp; in the chromatogram of the test solution, fluorescent spots with the same color appear at the corresponding positions of the chromatogram of the reference solution;
(5) identification of spreading hedyotis herb
Taking 5g of spreading hedyotis herb powder, adding 20ml of normal hexane, carrying out ultrasonic treatment for 15 minutes, filtering, and taking filtrate as spreading hedyotis herb test solution; preparing herba Hedyotidis Diffusae control solution with 0.5g Atractylodis rhizoma control; according to the thin layer chromatography test, 5 mul of each solution is sucked up and respectively spotted on the same silica gel G thin layer plate, and the volume ratio is 50: 1, developing by using petroleum ether-ethyl acetate as a developing agent, taking out, airing, spraying a 5% vanillin sulfuric acid ethanol solution, and heating until spots are clearly developed; spots of the same color appear in the chromatogram of the test solution at the positions corresponding to those in the chromatogram of the reference solution;
(6) agrimonia pilosa ledeb identification
Taking 5g of hairyvein agrimony powder, adding 40ml of petroleum ether, carrying out ultrasonic treatment for 30 minutes, filtering, and evaporating filtrate to dryness; dissolving residues with 10ml of trichloromethane, extracting with 10ml of 5% sodium oxide solution, discarding three peaches of methylene liquid, adjusting the pH value to 1-2 with dilute hydrochloric acid, shaking with three-hydrogen methane to extract for 2 times, combining the three peaches of methane, adding 10ml of water for washing, discarding water liquid, concentrating the three peaches of methylene liquid to 1ml, and using the three peaches of methylene liquid as a hairyvein agrimony test solution; preparing herba et Gemma Agrimoniae control solution by the same method, except that 2g herba et Gemma Agrimoniae control solution is prepared; taking a hairyvein agrimony phenol B reference substance, and adding three methane to prepare a hairyvein agrimony phenol B solution containing 0.5mg per 1ml, wherein the hairyvein agrimony phenol B solution is used as the hairyvein agrimony phenol B reference substance solution; according to the thin and thick chromatography test, respectively dropping 10 microliters of each of the three solutions on silica gel G thin layer plates, taking the upper layer solution of petroleum ether-acetic acid ethyl acetate-acetic acid as a developing agent in a volume ratio of 100:9:5, developing, taking out, airing, spraying with 10% sulfuric acid ethanol solution, and performing the following steps at 105 ℃: heating until the spots are clearly developed; spots of the same color appear in the chromatogram of the test solution at the positions corresponding to the chromatograms of the reference medicinal material and the reference solution;
(7) identification of Chinese Lobelia
Taking 5g of Chinese lobelia powder, adding 50ml of methanol, carrying out ultrasonic treatment for 30 minutes, cooling and filtering, evaporating filtrate to dryness, and dissolving 2ml of residue methanol to obtain a Chinese lobelia sample solution; preparing herba Lobeliae chinensis reference medicinal material lg, and preparing reference medicinal material solution by the same method; performing thin layer chromatography test, sucking the above two solutions 5 μ l each, respectively dropping on the same silica gel G thin layer plate, developing with chloroform-methanol at volume ratio of 9:1 as developing agent, taking out, air drying, spraying 10% ethanol sulfate solution, heating at 105 deg.C until the color development of spots is clear, respectively placing under sunlight and ultraviolet lamp 365nm for inspection, and displaying spots or fluorescent spots of the same color in the chromatogram of the test product at the position corresponding to the chromatogram of the control medicinal material.
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