CN117783410A - Method for simultaneously identifying ephedra, liquorice and bitter apricot kernel in Maxingshi Ganmi oral liquid - Google Patents
Method for simultaneously identifying ephedra, liquorice and bitter apricot kernel in Maxingshi Ganmi oral liquid Download PDFInfo
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- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 57
- 239000013558 reference substance Substances 0.000 claims description 39
- 238000001704 evaporation Methods 0.000 claims description 36
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- 238000010438 heat treatment Methods 0.000 claims description 34
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 20
- 238000010992 reflux Methods 0.000 claims description 20
- 239000000706 filtrate Substances 0.000 claims description 19
- 238000001914 filtration Methods 0.000 claims description 19
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims description 18
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- Medicines Containing Plant Substances (AREA)
Abstract
The invention belongs to the technical field of a test method for qualitatively determining ephedra, liquorice and bitter apricot seeds in a traditional Chinese medicine compound preparation, and discloses a method for simultaneously identifying ephedra, liquorice and bitter apricot seeds in a ephedra, apricot stone and licorice oral liquid. Placing the sample into Soxhlet extractor, treating with reagents of different properties, extracting in grades to obtain sample solution, treating herba Ephedrae control medicinal material and Glycyrrhrizae radix control medicinal material to obtain control medicinal material solution, adding amygdalin control, and adding methanol to obtain control solution; the sample solution, the control medicinal material solution and the control solution are simultaneously identified by adopting a set of thin layer chromatography unfolding system. The results show that the chromatographic spots are well separated, clear and the negative control is not interfered. The method has the advantages of simple pretreatment, environmental friendliness, high sensitivity, repeatability and durability meeting the requirements of Chinese animal pharmacopoeia, thereby better controlling the quality of the Maxingshigan oral liquid.
Description
Technical Field
The invention relates to the technical field of a test method for qualitatively determining ephedra, liquorice and bitter apricot kernel in a traditional Chinese medicine compound preparation, in particular to a method for simultaneously identifying ephedra, liquorice and bitter apricot kernel in a ephedra, liquorice and bitter apricot kernel oral liquid.
Background
The ephedra, licorice and amygdalin oral liquid is a Chinese veterinary medicine prescription preparation, and is loaded in the (two parts) 2020 edition of the animal pharmacopoeia of the people's republic of China, the original standard has three thin-layer identification, and ephedra (ephedra control medicine is used as a control), licorice (licorice control medicine is used as a control) and amygdalin are respectively identified, and three pretreatment is carried out to prepare a test solution, wherein the identification pretreatment of licorice and amygdalin is complicated, and the whole test can be completed through three different unfolding systems. The existing method for identifying ephedra, liquorice and bitter apricot seed in the ephedra, apricot, lycopus and licorice oral liquid has the problems of complex process, low sensitivity, poor accuracy, poor repeatability and low specificity, and the existing method for identifying ephedra, liquorice and bitter apricot seed in the ephedra, apricot, lycopus and licorice oral liquid needs a large amount of reagents, so that the cost is high, the identification time is long, and the improvement of the identification efficiency is not facilitated.
Therefore, there is a need in the art to develop a method for identifying ephedra, licorice and bitter apricot kernel in Maxingshi Ganmu oral liquid with the advantages of rapidness, sensitivity, accuracy, good repeatability and strong specificity.
Disclosure of Invention
The invention aims to provide a method for simultaneously identifying ephedra, liquorice and bitter apricot seed in a ephedra, apricot, shigan oral liquid, which aims to solve the problems of complicated process, low sensitivity, poor accuracy, poor repeatability and low specificity of the existing method for identifying ephedra, liquorice and bitter apricot seed in the ephedra, apricot, shigan oral liquid; the method also solves the problems that the existing method for identifying ephedra, liquorice and bitter apricot seed in the ephedra, apricot kernel, gypsum and licorice oral liquid needs to adopt a large amount of reagents, has high cost and long identification time, and is not beneficial to improving the identification efficiency.
In order to achieve the above purpose, the invention adopts the following technical scheme:
the invention provides a method for simultaneously identifying ephedra, liquorice and bitter apricot seed in a ephedra, apricot kernel, shigan oral liquid, which comprises the following steps:
(1) Preparing a sample solution;
(2) Preparation of a control solution: taking herba Ephedrae control medicinal material, adding methanol, ultrasonic extracting, collecting supernatant, evaporating to dryness, and dissolving residue with methanol to obtain herba Ephedrae control medicinal material solution; reflux extracting Glycyrrhrizae radix with water under heating, filtering, concentrating the filtrate, extracting with water saturated n-butanol, collecting n-butanol solution, washing with water saturated n-butanol, evaporating n-butanol solution to dryness, and dissolving the residue with methanol to obtain Glycyrrhrizae radix control solution; dissolving amygdalin reference substance in methanol to obtain amygdalin reference substance solution;
(3) Thin layer chromatography assay: sample application amount: 3-8 μl, silica gel G lamellar plate, deployment system: a mixed solution of ethyl acetate, methanol, water and formic acid, an upper layer solution left overnight at 10 ℃;
and (3) result judgment: inspecting under ultraviolet lamp, wherein in the sample chromatogram, a fluorescent spot with the same color is displayed at the position corresponding to the herba Ephedrae control chromatogram, which indicates that herba Ephedrae can be detected; inspecting under ultraviolet lamp, wherein in the chromatogram of the sample, two black spots with the same color appear at the corresponding positions of the chromatogram of the reference medicinal material of Glycyrrhrizae radix, which indicates that Glycyrrhrizae radix can be detected; spraying alpha-naphthol test solution, heating until the spot color is clear, inspecting in sunlight, and displaying a pink spot with the same color on the position corresponding to the amygdalin reference substance color spectrum in the sample color spectrum to show that the amygdalin can be detected.
Preferably, the preparation of the test solution comprises the following steps:
s1: extracting the sample with chloroform, collecting chloroform layer, evaporating to dryness, and dissolving the residue with methanol;
s2: placing the solution obtained by dissolving in S1 in Soxhlet extractor, adding ethanol, heating and refluxing, filtering, evaporating filtrate to dryness, dissolving residue in methanol, and concentrating to obtain sample solution.
Preferably, in the preparation process of the sample solution:
s1: extracting 3-10 mL of a sample with chloroform for 3 times, adding 20mL of chloroform each time, mixing chloroform layers, evaporating to dryness, and adding 2-5 mL of methanol into residues to dissolve the residues for later use;
s2: putting the solution obtained by dissolving in the S1 into a Soxhlet extractor, adding 30-50 mL of ethanol with the mass fraction of 50%, heating and refluxing for 30min, cooling at normal temperature, filtering, evaporating filtrate to dryness, adding 2-5 mL of methanol into residues to dissolve, and concentrating to 1-2 mL to obtain a sample solution.
Preferably, in the preparation of the ephedra control medicinal material solution, 0.5-1 g of ephedra control medicinal material is taken, 10-20 mL of methanol is added, ultrasonic extraction is carried out for 10min, supernatant fluid is taken, the supernatant fluid is evaporated to dryness, and 2-4 mL of methanol is added into residues to dissolve the residues to be used as the ephedra control medicinal material solution.
Preferably, in the preparation of the licorice reference medicinal material solution, 0.5-2 g of the licorice reference medicinal material is taken, 30-120 mL of water is added, heating reflux is carried out for 30min, cooling is carried out at room temperature, filtering is carried out, filtrate is concentrated to 20-80 mL, water saturated n-butanol is used for 2 times, each time water saturated n-butanol is used for 20-80 mL, n-butanol solutions are taken and combined, water saturated n-butanol is used for 2 times, each time water saturated n-butanol is used for 10-40 mL, n-butanol solutions are taken and combined, evaporation is carried out, and residues are added with 1-4 mL of methanol to dissolve, thus obtaining the licorice reference medicinal material solution.
Preferably, the amygdalin reference substance is taken in the preparation of the amygdalin reference substance solution, methanol is added to dissolve the amygdalin reference substance, and 1-3 mg of amygdalin reference substance solution is prepared per 1mL of amygdalin reference substance solution to be used as the amygdalin reference substance solution.
Preferably, the wavelength of the ultraviolet lamp is 365nm.
Preferably, in the mixed solution of ethyl acetate, methanol, water and formic acid, the volume ratio of ethyl acetate, methanol, water and formic acid is 18-22:4.5-5.8:5-6:0.2-0.4.
Preferably, the heating temperature for heating to the point at which the spot color is clearly developed is 85 to 95 ℃.
Compared with the prior art, the invention has the following beneficial effects:
(1) The method is superior to the disclosed technology, three medicinal materials of ephedra, liquorice and bitter apricot kernel are simultaneously identified at one time through a set of thin-layer unfolding system, the method is simple, convenient and quick, the separation effect is good, the identification precision is high, the result reproducibility is good, the observation is easy, the specificity is strong, the spots are clear, the requirements of Chinese veterinary pharmacopoeia are met, and the time and the reagent are saved;
(2) The method has the advantages of simple and convenient sample treatment, reagent saving and time saving; the original standard of the Maxingshigan oral liquid is to respectively identify ephedra, liquorice and bitter apricot seed, and 3 times of sample treatment are needed; the method of the invention only carries out one sample treatment, can reduce the use of 20ml of diethyl ether and 45ml of n-butanol, does not need to pass through the elution treatment of a D101 macroporous adsorption resin column, and greatly saves reagents and operation time;
(3) The developing agent of the method only adopts 3 chemical reagents: ethyl acetate, methanol and formic acid, and the developing agent of the original method adopts 6 chemical reagents: chloroform, n-butanol, ethyl acetate, methanol, glacial acetic acid and concentrated ammonia test solution, and the chloroform belongs to a class of easy-to-poison chemicals, so that the method is more environment-friendly and safer.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings that are required to be used in the embodiments or the description of the prior art will be briefly described below, and it is obvious that the drawings in the following description are only embodiments of the present invention, and that other drawings can be obtained according to the provided drawings without inventive effort for a person skilled in the art.
FIG. 1 is a graph showing the result of comparative example 1 by the method of loading (herba Ephedrae identification) in the "animal pharmacopoeia of the people's republic of China" 2020 edition (section two);
FIG. 2 is a graph showing the results of comparative example 1 using the method of harvesting (licorice identification) of the "animal pharmacopoeia of the people's republic of China" 2020 edition (two parts);
fig. 3 is a graph showing the result of comparative example 1 using the method of harvest (bitter almond identification) of the "animal pharmacopoeia of the people's republic of China" 2020 edition (two parts);
FIG. 4 is a thin layer chromatogram of Maxingshi Gai oral liquid prepared by the method of example 1, wherein the liquid is detected under an ultraviolet lamp (365 nm); 1 is negative for ephedra deficiency; 2 is negative for bitter apricot kernel; 3 is negative for lacking licorice; 4 is herba Ephedrae control material; 5 is amygdalin reference substance; 6 is licorice reference medicine; 7 to 9 are self-made standard samples;
FIG. 5 is a thin layer chromatogram of Maxingshi Gai oral liquid prepared by the method of the invention in example 1, wherein an alpha-naphthol test solution is sprayed, and the mixture is heated at 85 ℃ until spots are clear in color, and is inspected in sunlight; 1 is negative for ephedra deficiency; 2 is negative for bitter apricot kernel; 3 is negative for lacking licorice; 4 is herba Ephedrae control material; 5 is amygdalin reference substance; 6 is licorice reference medicine; 7 to 9 are self-made standard samples.
Detailed Description
The invention provides a method for simultaneously identifying ephedra, liquorice and bitter apricot seed in a ephedra, apricot kernel, shigan oral liquid, which comprises the following steps:
(1) Preparing a sample solution;
(2) Preparation of a control solution: taking herba Ephedrae control medicinal material, adding methanol, ultrasonic extracting, collecting supernatant, evaporating to dryness, and dissolving residue with methanol to obtain herba Ephedrae control medicinal material solution; reflux extracting Glycyrrhrizae radix with water under heating, filtering, concentrating the filtrate, extracting with water saturated n-butanol, collecting n-butanol solution, washing with water saturated n-butanol, evaporating n-butanol solution to dryness, and dissolving the residue with methanol to obtain Glycyrrhrizae radix control solution; dissolving amygdalin reference substance in methanol to obtain amygdalin reference substance solution;
(3) Thin layer chromatography assay: sample application amount: 3-8 μl, silica gel G lamellar plate, deployment system: a mixed solution of ethyl acetate, methanol, water and formic acid, an upper layer solution left overnight at 10 ℃;
and (3) result judgment: inspecting under ultraviolet lamp, wherein in the sample chromatogram, a fluorescent spot with the same color is displayed at the position corresponding to the herba Ephedrae control chromatogram, which indicates that herba Ephedrae can be detected; inspecting under ultraviolet lamp, wherein in the chromatogram of the sample, two black spots with the same color appear at the corresponding positions of the chromatogram of the reference medicinal material of Glycyrrhrizae radix, which indicates that Glycyrrhrizae radix can be detected; spraying alpha-naphthol test solution, heating until the spot color is clear, inspecting in sunlight, and displaying a pink spot with the same color on the position corresponding to the amygdalin reference substance color spectrum in the sample color spectrum to show that the amygdalin can be detected.
The invention prepares the sample solution at one time by classifying and extracting with reagents with different properties through a Soxhlet extractor, thereby identifying ephedra, liquorice and bitter apricot seed simultaneously; the three medicinal materials are identified by a set of thin-layer chromatography unfolding system through one-time sample pretreatment in the Ma xing Shigan oral liquid.
The invention carries out result judgment twice: firstly, placing under ultraviolet lamp (365 nm) to inspect fluorescent spots of herba Ephedrae and Glycyrrhrizae radix, spraying color-developing agent, heating until the spots are clear, and placing under sunlight to inspect pink spots of amygdalin.
In the present invention, the preparation of the test solution includes the steps of:
s1: extracting the sample with chloroform, collecting chloroform layer, evaporating to dryness, and dissolving the residue with methanol;
s2: placing the solution obtained by dissolving in S1 in Soxhlet extractor, adding ethanol, heating and refluxing, filtering, evaporating filtrate to dryness, dissolving residue in methanol, and concentrating to obtain sample solution.
In the invention, in the preparation process of the sample solution, the following steps are adopted:
s1: extracting 3-10 mL of a sample with chloroform for 3 times, adding 20mL of chloroform each time, mixing chloroform layers, evaporating to dryness, and adding 2-5 mL of methanol into residues to dissolve the residues for later use;
s2: putting the solution obtained by dissolving in the S1 into a Soxhlet extractor, adding 30-50 mL of ethanol with the mass fraction of 50%, heating and refluxing for 30min, cooling at normal temperature, filtering, evaporating filtrate to dryness, adding 2-5 mL of methanol into residues to dissolve, and concentrating to 1-2 mL to obtain a sample solution.
In the preparation of the ephedra control medicinal material solution, 0.5-1 g of ephedra control medicinal material is taken, 10-20 mL of methanol is added, ultrasonic extraction is carried out for 10min, supernatant fluid is taken, the supernatant fluid is evaporated to dryness, and 2-4 mL of methanol is added into residues to dissolve the residues to be used as the ephedra control medicinal material solution.
In the preparation of the licorice reference medicinal material solution, 0.5-2 g of the licorice reference medicinal material is taken, 30-120 mL of water is added, heating reflux is carried out for 30min, cooling is carried out at room temperature, filtering is carried out, filtrate is concentrated to 20-80 mL, water saturated n-butanol is used for extraction for 2 times, each time, water saturated n-butanol is used for 20-80 mL, n-butanol solutions are taken and combined, water saturated with n-butanol is used for washing for 2 times, each time, water saturated with n-butanol is used for 10-40 mL, n-butanol solutions are taken and combined, evaporated to dryness, and residues are added with 1-4 mL of methanol to dissolve, thus obtaining the licorice reference medicinal material solution.
In the invention, the amygdalin reference substance is taken in the preparation of the amygdalin reference substance solution, methanol is added to dissolve the amygdalin reference substance, and 1-3 mg of amygdalin reference substance solution is prepared per 1mL of amygdalin reference substance solution to be used as the amygdalin reference substance solution.
In the invention, the wavelength of the ultraviolet lamp is 365nm.
In the invention, the volume ratio of the ethyl acetate, the methanol, the water and the formic acid in the mixed solution of the ethyl acetate, the methanol, the water and the formic acid is preferably 18-22:4.5-5.8:5-6:0.2-0.4, and more preferably 20-21:5.1-5.5:5.5-5.8:0.3.
In the present invention, the heating temperature for heating to the clear spot color development is preferably 85 to 95 ℃, more preferably 88 to 92 ℃.
The technical solutions provided by the present invention are described in detail below with reference to examples, but they should not be construed as limiting the scope of the present invention.
The reagents and apparatus used in the following examples:
reagents and reagents: licorice root is used as a reference medicine, and Chinese food and drug verification institute, batch No. 120904-202021;
ephedra herb reference medicine, chinese food and drug verification institute, lot 121051-201606;
amygdalin reference, chinese food and drug assay institute, lot number 110820-202109.
Other experiments Liu Jun were analytically pure.
Wherein the apparatus used is: BP211D analytical balance (saidolis, germany); automatic sample applicator for CAMAG thin layer (specification model LINOMAT 5) and full-automatic thin layer chromatography imaging system for CAMAG VISUALIZER.
Example 1
The method for simultaneously identifying ephedra, liquorice and bitter apricot seed in the ephedra, apricot kernel, gypsum and licorice oral liquid comprises the following steps:
s1: extracting 5mL of the sample with chloroform for 3 times by shaking, each time with 20mL of chloroform, mixing the chloroform solutions, evaporating to dryness, and dissolving the residue with 4mL of methanol;
s2: placing the water solution in the step S1 into a Soxhlet extractor, adding 30mL of ethanol with the mass fraction of 50%, heating and refluxing for 30min, cooling at room temperature, filtering, evaporating filtrate to dryness, adding 4mL of methanol into residues to dissolve, and concentrating to 2mL to obtain a sample solution;
s3: taking herba Ephedrae control medicinal material 0.5g, adding methanol 10mL, performing ultrasonic treatment for 10min, centrifuging, collecting supernatant, evaporating to dryness, and dissolving residue with methanol 2mL to obtain herba Ephedrae control medicinal material solution; taking 0.5g of licorice reference medicine, adding 30mL of water, heating and refluxing for 30min, taking out, cooling at room temperature, filtering, concentrating the filtrate to 20mL, extracting with water-saturated n-butanol for 2 times, each time with water-saturated n-butanol for 20mL, combining n-butanol solutions, washing with water-saturated n-butanol for 2 times, each time with water-saturated n-butanol for 10mL, discarding the water solution, taking the n-butanol solution, evaporating to dryness, and adding 1mL of methanol into the residue to dissolve the residue to obtain licorice reference medicine solution; adding methanol into amygdalin reference substance to obtain 2 mg/1 mL amygdalin reference substance solution as amygdalin reference substance solution;
s4: thin layer chromatography:
sample application amount: 5. Mu.L;
silica gel G thin layer plate (10 cm. Times.20 cm), (lot number: 20230329, available from Qingdao ocean chemical Co., ltd.);
deployment system: a mixed solution of ethyl acetate, methanol, water and formic acid (volume ratio of ethyl acetate, methanol, water and formic acid is 20:5.1:5.8:0.4) was left at 10 ℃ overnight as an upper layer solution;
and (3) result judgment:
4.1: the sample was inspected under an ultraviolet lamp (365 nm). In the chromatogram of the sample, a fluorescence spot with the same color is displayed at the position corresponding to the chromatogram of the herba Ephedrae control medicine, which indicates that herba Ephedrae is detected; two black spots with the same color appear on the corresponding positions of the liquorice control medicine chromatogram, which indicates that liquorice can be detected. The negative sample of ephedra lack and the negative sample of liquorice lack have no spots with the same color on the positions corresponding to the chromatograms of ephedra control medicinal material and liquorice control medicinal material, namely the negative has no interference, which indicates that the method is special and feasible, and the chromatographic spots are well separated, clear and have no interference on the background, and the result is shown in figure 3.
4.2: then spraying alpha-naphthol test solution, heating at 85deg.C until the color of the spot is clear, inspecting in sunlight, and displaying a pink spot with the same color on the position corresponding to the amygdalin reference substance chromatogram in the sample chromatogram to show that amygdalin can be detected. The chromatographic spots are well separated and clear, the background is free from interference, the chromatographic spots are free from interference by no bitter almond negative sample control, and the result is shown in figure 4.
Example 2
S1: extracting 3mL of sample with chloroform for 3 times under shaking, each time with 20mL of chloroform, mixing chloroform solutions, evaporating to dryness, and dissolving the residue with 2mL of methanol;
s2: placing the water solution in the step S1 into a Soxhlet extractor, adding 40mL of ethanol with the mass fraction of 50%, heating and refluxing for 30min, cooling at room temperature, filtering, evaporating filtrate to dryness, adding 2mL of methanol into residues to dissolve, and concentrating to 1mL to obtain a sample solution;
s3: taking 1g of ephedra control medicinal material, adding 20mL of methanol, carrying out ultrasonic treatment for 10min, centrifuging, taking supernatant, evaporating to dryness, and adding 4mL of methanol into residues to dissolve the residues to obtain ephedra control medicinal material solution; taking 1g of licorice reference medicine, adding 60mL of water, heating and refluxing for 30min, taking out, cooling at room temperature, filtering, concentrating filtrate to 40mL, extracting with water-saturated n-butanol for 2 times, each time with water-saturated n-butanol to 40mL, combining n-butanol solutions, washing with water-saturated n-butanol for 2 times, each time with water-saturated n-butanol to 20mL, discarding water solution, taking n-butanol solution, evaporating to dryness, and adding methanol to 3mL of residues to dissolve, thereby obtaining licorice reference medicine solution; adding methanol into amygdalin reference substance to obtain 1 mg/1 mL amygdalin reference substance solution as amygdalin reference substance solution;
s4: thin layer chromatography:
sample application amount: 7. Mu.L;
silica gel G thin layer plate (10 cm. Times.20 cm), (lot number: 20230329, available from Qingdao ocean chemical Co., ltd.);
deployment system: a mixed solution of ethyl acetate, methanol, water and formic acid (volume ratio of ethyl acetate, methanol, water and formic acid is 18:5.0:5.5:0.3) was left at 10 ℃ overnight as an upper layer solution;
and (3) result judgment:
4.1 inspection under an ultraviolet lamp (365 nm). In the chromatogram of the sample, a fluorescence spot with the same color is displayed at the position corresponding to the chromatogram of the herba Ephedrae control medicine, which indicates that herba Ephedrae is detected; two black spots with the same color appear on the corresponding positions of the liquorice control medicine chromatogram, which indicates that liquorice can be detected, and the chromatographic spots are well separated, clear and have no interference on the background.
4.2 spraying alpha-naphthol test solution, heating at 85deg.C until the color of the spot is clear, inspecting in sunlight, and displaying a pink spot with the same color on the position corresponding to the amygdalin reference substance chromatogram in the sample chromatogram to indicate that amygdalin can be detected. The chromatographic spots are well separated and clear, and the background is free from interference.
Example 3
S1: extracting 10mL of sample with chloroform for 3 times under shaking, each time with 20mL of chloroform, mixing chloroform solutions, evaporating to dryness, and dissolving the residue with 5mL of methanol;
s2: placing the water solution in the step S1 into a Soxhlet extractor, adding 50mL of ethanol with the mass fraction of 50%, heating and refluxing for 30min, cooling at room temperature, filtering, evaporating filtrate to dryness, adding 5mL of methanol into residues to dissolve, and concentrating to 2mL to obtain a sample solution.
S3: taking herba Ephedrae control medicinal material 0.8g, adding methanol 20mL, performing ultrasonic treatment for 10min, centrifuging, collecting supernatant, evaporating to dryness, and dissolving residue with methanol 3mL to obtain herba Ephedrae control medicinal material solution; taking 2g of licorice reference medicine, adding 120mL of water, heating and refluxing for 30min, taking out, cooling at room temperature, filtering, concentrating the filtrate to 80mL, extracting with water-saturated n-butanol for 2 times, each time with water-saturated n-butanol for 40mL, combining n-butanol solutions, washing with water-saturated n-butanol for 2 times, each time with water-saturated n-butanol for 40mL, discarding the water solution, evaporating the n-butanol solution to dryness, and adding methanol for 4mL to the residue to dissolve the residue to obtain licorice reference medicine solution; and adding methanol into the amygdalin reference substance to obtain 3 mg/1 mL amygdalin reference substance solution as amygdalin reference substance solution.
S4: thin layer chromatography:
sample application amount: 6. Mu.L;
silica gel G thin layer plate (10 cm. Times.20 cm), (lot number: 20230329, available from Qingdao ocean chemical Co., ltd.);
deployment system: a mixed solution of ethyl acetate, methanol, water and formic acid (volume ratio of ethyl acetate, methanol, water and formic acid is 22:5.8:6:0.4) was left at 10 ℃ overnight as an upper layer solution;
and (3) result judgment:
4.1 inspection under an ultraviolet lamp (365 nm). In the chromatogram of the sample, a fluorescence spot with the same color is displayed at the position corresponding to the chromatogram of the herba Ephedrae control medicine, which indicates that herba Ephedrae is detected; two black spots with the same color appear on the corresponding positions of the liquorice control medicine chromatogram, which indicates that liquorice can be detected, and the chromatographic spots are well separated, clear and have no interference on the background.
4.2 spraying alpha-naphthol test solution, heating at 85deg.C until the color of the spot is clear, inspecting in sunlight, and displaying a pink spot with the same color on the position corresponding to the amygdalin reference substance chromatogram in the sample chromatogram to indicate that amygdalin can be detected. The chromatographic spots are well separated and clear, and the background is free from interference.
Comparative example 1
The method for loading and unloading the animal pharmacopoeia 2020 edition (two parts) of the people's republic of China comprises the following specific steps:
(1) 10mL of a sample is taken, 1mL of concentrated ammonia solution is added, chloroform is used for shaking and extracting for 3 times, 20mL of chloroform is used each time, the chloroform solution is combined and evaporated to dryness, and 2mL of methanol is added to residues to dissolve the residues to obtain a sample solution. And adding methanol (10 mL) into herba Ephedrae reference material (0.5 g), performing ultrasonic treatment for 10min, centrifuging, collecting supernatant, evaporating to dryness, and dissolving residue with methanol (2 mL) to obtain reference material solution. According to a thin layer chromatography (appendix 0502) test, 5 mu L of each of the two solutions is sucked and respectively spotted on the same silica gel G thin layer plate, a mixed solution test solution of chloroform, methanol and concentrated ammonia (the volume ratio of the chloroform to the methanol to the concentrated ammonia is 20:5:0.5) is used as a developing agent, and the developing agent is developed, taken out, dried, sprayed with ninhydrin test solution and heated at 105 ℃ until the spot color development is clear. The same mauve main spots appear on the chromatogram of the test sample at the positions corresponding to the chromatograms of the control medicinal materials.
(2) Taking 10mL of a test sample, adding 20mL of diethyl ether, heating and refluxing for 30min, discarding diethyl ether solution, adding 20mL of methanol into the water solution, heating and refluxing for 1h, filtering, evaporating the filtrate to dryness, adding 30mL of water into the residue to dissolve, shaking and extracting 3 times with water-saturated n-butanol for 15mL of water-saturated n-butanol each time, combining n-butanol solutions, washing with water-saturated n-butanol for 3 times, adding 15mL of water-saturated n-butanol each time, discarding the water solution, evaporating the n-butanol solution to dryness, and adding 5mL of methanol into the residue to dissolve, thereby obtaining the test sample solution. And 1g of licorice reference medicine is prepared, and a reference medicine solution is prepared by the same method. According to a thin layer chromatography (appendix 0502) test, 5 mu L of each of the two solutions is sucked and respectively spotted on the same silica gel GF254 thin layer plate, and an upper layer solution of a mixed solution of n-butanol, glacial acetic acid and water (the volume ratio of n-butanol, glacial acetic acid and water is 6:1:3) is taken as a developing agent, developed, taken out, dried and inspected under an ultraviolet lamp (254 nm). Spots of the same color appear on the chromatogram of the test sample at positions corresponding to those of the chromatogram of the control drug.
(3) Taking 5mL of a test sample, placing the test sample on a D101 macroporous adsorption resin column (the inner diameter is 1.5cm, the column height is 8cm, water is added for pre-washing until the test sample is clean and alcohol-free), eluting with 30mL of ammonia solution (the elution gradient is 4-100), discarding the ammonia solution, eluting with 20mL of water again, discarding the water solution, eluting with 30mL of ethanol with the mass fraction of 50%, collecting the eluent, evaporating to dryness, and adding 2mL of methanol into residues to dissolve the residues to obtain the test sample solution. And adding methanol into amygdalin reference substance to obtain 2 mg/1 mL amygdalin reference substance solution as reference substance solution. And respectively adding methanol 10mL, ultrasonic treating for 10min, centrifuging, collecting supernatant, evaporating, dissolving in water 5mL, and preparing herba Ephedrae control medicinal material solution and Glycyrrhrizae radix control medicinal material solution by the same method from "D101 macroporous adsorbent resin column". According to a thin layer chromatography (appendix 0502) test, sucking 3 μl of the two licorice control medicinal solutions, respectively injecting the rest 5 μl of the solutions onto the same silica gel G thin layer plate, placing the upper layer solution at 10deg.C overnight with mixed solution of ethyl acetate, methanol, water and formic acid (volume ratio of ethyl acetate, methanol, water and formic acid is 20:5.1:5.8:0.4) as developing agent, spreading, taking out, air drying, and inspecting under ultraviolet lamp (365 nm). In the chromatogram of the sample, a fluorescent spot with the same color is displayed at the position corresponding to the chromatogram of the ephedra control medicine; two black spots with the same color appear on the corresponding position of the liquorice control medicine chromatogram. Then spraying alpha-naphthol test solution, heating at 85deg.C until the color of the spot is clear, inspecting in sunlight, and displaying a pink spot with the same color on the position corresponding to the amygdalin reference substance chromatogram in the sample chromatogram.
The foregoing is merely a preferred embodiment of the present invention and it should be noted that modifications and adaptations to those skilled in the art may be made without departing from the principles of the present invention, which are intended to be comprehended within the scope of the present invention.
Claims (9)
1. A method for simultaneously identifying ephedra, liquorice and bitter apricot seed in Maxingshi Ganma oral liquid is characterized by comprising the following steps:
(1) Preparing a sample solution;
(2) Preparation of a control solution: taking herba Ephedrae control medicinal material, adding methanol, ultrasonic extracting, collecting supernatant, evaporating to dryness, and dissolving residue with methanol to obtain herba Ephedrae control medicinal material solution; reflux extracting Glycyrrhrizae radix with water under heating, filtering, concentrating the filtrate, extracting with water saturated n-butanol, collecting n-butanol solution, washing with water saturated n-butanol, evaporating n-butanol solution to dryness, and dissolving the residue with methanol to obtain Glycyrrhrizae radix control solution; dissolving amygdalin reference substance in methanol to obtain amygdalin reference substance solution;
(3) Thin layer chromatography assay: sample application amount: 3-8 μl, silica gel G lamellar plate, deployment system: a mixed solution of ethyl acetate, methanol, water and formic acid, an upper layer solution left overnight at 10 ℃;
and (3) result judgment: inspecting under ultraviolet lamp, wherein in the sample chromatogram, a fluorescent spot with the same color is displayed at the position corresponding to the herba Ephedrae control chromatogram, which indicates that herba Ephedrae can be detected; inspecting under ultraviolet lamp, wherein in the chromatogram of the sample, two black spots with the same color appear at the corresponding positions of the chromatogram of the reference medicinal material of Glycyrrhrizae radix, which indicates that Glycyrrhrizae radix can be detected; spraying alpha-naphthol test solution, heating until the spot color is clear, inspecting in sunlight, and displaying a pink spot with the same color on the position corresponding to the amygdalin reference substance color spectrum in the sample color spectrum to show that the amygdalin can be detected.
2. The method for simultaneously identifying ephedra, licorice and bitter apricot seed in ephedra, apricot kernel, licorice and licorice oral liquid according to claim 1, wherein the preparation of the test solution comprises the following steps:
s1: extracting the sample with chloroform, collecting chloroform layer, evaporating to dryness, and dissolving the residue with methanol;
s2: placing the solution obtained by dissolving in S1 in Soxhlet extractor, adding ethanol, heating and refluxing, filtering, evaporating filtrate to dryness, dissolving residue in methanol, and concentrating to obtain sample solution.
3. The method for simultaneously identifying ephedra, licorice and bitter apricot seed in ephedra, apricot kernel, gypsum and licorice oral liquid according to claim 2, wherein the preparation process of the test solution is characterized in that:
s1: extracting 3-10 mL of a sample with chloroform for 3 times, adding 20mL of chloroform each time, mixing chloroform layers, evaporating to dryness, and adding 2-5 mL of methanol into residues to dissolve the residues for later use;
s2: putting the solution obtained by dissolving in the S1 into a Soxhlet extractor, adding 30-50 mL of ethanol with the mass fraction of 50%, heating and refluxing for 30min, cooling at normal temperature, filtering, evaporating filtrate to dryness, adding 2-5 mL of methanol into residues to dissolve, and concentrating to 1-2 mL to obtain a sample solution.
4. The method for simultaneously identifying ephedra, licorice and bitter apricot kernel in ephedra, apricot kernel and lycopus oral liquid according to claim 1, which is characterized in that in the preparation of ephedra control medicinal material solution, 0.5-1 g of ephedra control medicinal material is taken, 10-20 mL of methanol is added, ultrasonic extraction is carried out for 10min, supernatant is taken, evaporated, and 2-4 mL of methanol is added into residues to dissolve the residues to be used as the ephedra control medicinal material solution.
5. The method for simultaneously identifying ephedra, licorice and bitter apricot kernel in a ephedra, apricot kernel and licorice oral liquid according to claim 4, wherein in the preparation of the licorice control medicinal material solution, 0.5-2 g of licorice control medicinal material is taken, 30-120 mL of water is added, heating reflux is carried out for 30min, cooling is carried out at room temperature, filtration is carried out, filtrate is concentrated to 20-80 mL, water saturated n-butanol is used for extraction for 2 times, each time water saturated n-butanol is used for 20-80 mL, n-butanol solutions are taken and combined, water saturated n-butanol is used for washing for 2 times, each time water saturated with n-butanol is used for 10-40 mL, n-butanol solutions are taken and combined, evaporated to dryness, and 1-4 mL of methanol is added into residues to dissolve the residues to be used as the licorice control medicinal material solution.
6. The method for simultaneously identifying ephedra, licorice and bitter apricot kernel in ephedra, apricot kernel, licorice and licorice oral liquid according to claim 5, characterized in that in the preparation of said bitter apricot kernel reference solution, bitter apricot kernel reference is taken, methanol is added to dissolve, and 1-3 mg of bitter apricot kernel reference solution is prepared per 1mL of bitter apricot kernel reference solution as bitter apricot kernel reference solution.
7. The method for simultaneously identifying ephedra, licorice and bitter apricot seed in ephedra, apricot kernel, lycopodium clavatum oral liquid according to claim 1, wherein the wavelength of the ultraviolet lamp is 365nm.
8. The method for simultaneously identifying ephedra, licorice and bitter apricot seed in ephedra, apricot kernel, licorice and licorice oral liquid according to claim 7, wherein the volume ratio of ethyl acetate, methanol, water and formic acid in the mixed solution of ethyl acetate, methanol, water and formic acid is 18-22:4.5-5.8:5-6:0.2-0.4.
9. The method for simultaneously identifying ephedra, licorice and bitter apricot seed in ephedra, apricot kernel, licorice and licorice oral liquid according to claim 7 or 8, wherein the heating temperature for heating to the point that the color of spots is clear is 85-95 ℃.
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