CN108627606B - Thin layer identification method of pogostemon cablin - Google Patents

Thin layer identification method of pogostemon cablin Download PDF

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CN108627606B
CN108627606B CN201810954152.3A CN201810954152A CN108627606B CN 108627606 B CN108627606 B CN 108627606B CN 201810954152 A CN201810954152 A CN 201810954152A CN 108627606 B CN108627606 B CN 108627606B
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patchouli
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CN108627606A (en
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倪艳
程玉钏
王玉娥
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Shanxi Traditional Chinese Medicine Institute (shanxi Provincial Hospital Of Traditional Chinese Medicine)
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    • G01MEASURING; TESTING
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    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/90Plate chromatography, e.g. thin layer or paper chromatography
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
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Abstract

The invention discloses a thin-layer identification method of patchouli, which comprises the steps of firstly preparing a sample to be tested, developing a spectrum by taking petroleum ether-ethyl acetate-methanol-formic acid as a developing agent according to a thin-layer chromatography test method, finally identifying the spectrum obtained by different developing agents by adopting a double identification method, checking whether the spectrum to be tested has a first characteristic spot and/or a second characteristic spot, and identifying the sample to be tested as a patchouli genuine product, a similar product or a fake product. The novel detection method and the detection program provided by the invention have the characteristics of high precision, wide application range and comprehensive detection results.

Description

Thin layer identification method of pogostemon cablin
Technical Field
The invention relates to the technical field of quality inspection, in particular to a stylized patchouli accurate inspection method based on a thin-layer spectrum.
Background
Patchouli is a common and commonly used traditional Chinese medicinal material. In the application of traditional Chinese medicine, some traditional Chinese medicinal materials similar to the cablin potchouli herb in appearance but completely different in plant species and drug property exist, and some medicinal materials similar to the classification of the cablin potchouli herb in species and drug property also exist. Therefore, the method has important practical significance for the precise identification of the pogostemon cablin.
The identification method of herba Agastaches is described as follows.
The pharmacopoeia detection method comprises the following steps: taking appropriate amount of coarse powder, measuring according to volatile oil determination method (Tonghe 2204), collecting volatile oil 0.5ml, and diluting with ethyl acetate to 5ml to obtain sample solution. Adding ethyl acetate into the alcoholic solution of Periplaneta Forrestii to obtain solution containing 2mg per lml as control solution. According to a thin-layer chromatography (general rule 0502) test, sucking 1-2 mu L of each of the two solutions, respectively dropping the two solutions on the same silica gel G thin-layer plate, taking petroleum ether (30-60 ℃), ethyl acetate and glacial acetic acid (95: 5:0.2) as a developing agent, developing, taking out, airing, and spraying a 5% tri-ferroethanol solution. A yellow spot appears in the chromatogram of the test sample; heating until the spots are clear, and displaying the same violet-blue spots on the chromatogram of the sample at the positions corresponding to the chromatogram of the reference.
The literature method, the research on the quality relationship between the patchouli formula granules and the medicinal materials thereof, provides an identification method. Weighing 5.0 g crude powder of raw medicinal material, placing in 30mL triangular flask with plug, adding 20mL petroleum ether, sealing, performing ultrasound for 10min, filtering, discarding petroleum ether solution, adding 10 mL methanol to the residue, sealing, performing ultrasound for 15min, and filtering to obtain methanol solution 1. The intermediate sample is prepared by weighing fluid extract, spraying dry powder about 0.2 g, placing into 30mL triangular flask with plug, adding petroleum ether 20mL, sealing, performing ultrasound for 10min, filtering, discarding petroleum ether solution, adding methanol 10 mL into the residue, sealing, performing ultrasound for 15min, filtering, and collecting methanol solution as sample solution 2. Weighing about 0.2 g of formula granule, placing into 30mL triangular flask with plug, adding 20mL petroleum ether, sealing, performing ultrasonic treatment for 10min, filtering, discarding petroleum ether solution, adding 10 mL methanol into residue, sealing, performing ultrasonic treatment for 15min, filtering, and using methanol solution as sample solution 3. Thin layer chromatography conditions. The thin layer plate is silica gel GF254 precast plate, the sample application amount is 10 muL, the development system is petroleum ether-ethyl acetate-methanol-formic acid (7.5: 1.8: 1: 0.125), and the development mode is secondary development, 9 cm/time. Thin layer behavior and results. Spreading the samples on the same thin layer plate by the same method, taking out, air drying, developing with 5% AlCl3 ethanol solution, and observing at 365 nm. The results show that the patchouli formulation (test 3), intermediate (test 2) and drug (test 10) behave in a thin layer, showing the same fluorescent spot.
Literature methods, the study on extraction of Pogostemon cablin formula granules, gave the following test methods. And (4) preparing a test sample. Weighing 5 g of coarse powder of a patchouli sample, placing the coarse powder in a 250 mL beaker, adding 10 times of water, extracting according to the finally determined extraction process (namely decocting for 2 hours and 2 times in total), combining the extracting solutions, filtering, concentrating the filtrate under reduced pressure to obtain an extract, and drying the dregs and the extract in a 60 ℃ oven for later use. Extracting the extract with methanol for 2 times, mixing methanol solutions, and concentrating to 5mL to obtain sample a. The residue remaining after the methanol extraction was dissolved in 5mL of water to prepare a sample b. Extracting the above residue with methanol for 2 times, and concentrating methanol solution to 5mL to obtain sample c. Weighing herba Agastaches 5 g, extracting with methanol for 2 times, and concentrating methanol solution to 5mL as sample d. Weighing herba Agastaches 5 g, extracting with appropriate amount of ethanol for 2 times, and concentrating methanol solution to 5mL as sample f. Thin layer chromatography conditions. The thin layer plate is silica gel GF254 precast plate, the developing system is petroleum ether-ethyl acetate-methanol-formic acid (volume ratio is 7.5: 1.8: 1: 0.125), the developing method and color development are carried out, secondary development is carried out, 9 cm is carried out each time, the thin layer plate is taken out and dried, the thin layer plate is observed under an ultraviolet lamp of 365nm, and AlCl3 ethanol solution with mass fraction of 5% is used for color development, and the thin layer plate is observed under 365 nm. And (5) result and analysis. After each sample is spotted, the sample is developed, and after the sample is developed by AlCl3 ethanol solution, the sample is observed under 365nm, and the components of different extraction processes are greatly different from each other on the aspect of thin-layer chromatography, which indicates that more low-polarity components exist in the medicine residue, and most of water-soluble components can be extracted by the water extract.
Therefore, the detection methods in the prior art are simple, have low accuracy and cannot meet the requirements of the pogostemon cablin medicinal material in wide practical application and detection and identification.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a stylized and highly accurate identification method of a patchouli thin layer.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows.
The thin-layer identification method of the patchouli comprises the steps of firstly preparing a sample to be tested, developing a spectrum by using petroleum ether-ethyl acetate-methanol-formic acid as a developing agent according to a thin-layer chromatography test method, finally identifying the spectrum obtained under different developing agents by adopting a double identification method, checking whether the spectrum to be tested has a first characteristic spot and/or a second characteristic spot, and identifying the sample to be tested as a patchouli genuine product, a similar product or a fake product.
As a preferred technical scheme of the invention, the method comprises the following steps:
A. preparation of test samples: placing 1g herba Agastaches powder in conical flask, adding 30mL ethanol, ultrasonic extracting for 30min, filtering, naturally volatilizing filtrate or steaming below 60 deg.C to near dry, and dissolving residue with 1mL methanol to obtain sample solution;
B. and (3) developing by thin-layer chromatography: according to a thin-layer chromatography test method, absorbing 5 mu L of the test solution obtained in the step A, dropping the sample solution on a silica gel G thin-layer plate, taking out and drying the sample solution by taking petroleum ether, ethyl acetate, methanol and formic acid =7.50:1.80:1.00:0.125 as a developing agent according to the volume ratio, spraying a 5% aluminum trichloride ethanol solution, and heating the sample solution at 110 ℃ until spots are clear;
C. two-fold map identification method:
c-1, carrying out first inspection, namely observing the map obtained in the step B in the sunlight, observing whether the map has a characteristic spot ① at the position of RF =0.77-0.83, identifying the detected sample as a patchouli counterfeit product if the map to be inspected does not have the characteristic spot ①, and entering the step C-2 if the map to be inspected has the characteristic spot ①;
and C-2, performing secondary inspection, namely further inspecting whether the sample map with the characteristic spot ① has the characteristic spot ② at the position of RF =0.26-0.32 under an ultraviolet lamp, if the map to be inspected has the characteristic spot ②, determining that the detected sample is a patchouli genuine product and the identification is finished, and if the map to be inspected does not have the characteristic spot ②, determining that the detected sample is a patchouli approximant product and the identification is finished.
In a preferred technical scheme of the invention, in the step a, the patchouli powder is coarse powder obtained by crushing a patchouli medicinal material or decoction pieces.
As a preferred embodiment of the present invention, in step C-1, the sunlight inspection is a transparent inspection, and the RF = 0.80.
As a preferred technical scheme of the invention, in the step C-1, the characteristic spots ① are similar to circular characteristic spots and have the characteristics of clear spots and good separation degree.
In a preferred embodiment of the present invention, in step C-2, the wavelength of the ultraviolet light is 365nm, and the RF = 0.29.
In a preferred embodiment of the present invention, in step C-2, the characteristic spots ② are feature spots similar to a circle, and have a uniform bluish color tone.
Adopt the produced beneficial effect of above-mentioned technical scheme to lie in: the novel detection method and the detection program provided by the invention have the characteristics of high precision, wide application range and comprehensive detection results, can quickly and conveniently classify and identify the genuine products, the similar products and the fake products of the samples to be detected, and are a novel practical method with obvious improvement in detection effect compared with the existing method.
Drawings
FIG. 1 is a picture of the sample to be tested in example 3 under sunlight.
Fig. 2 is a spectrum appearance of a sample to be detected under ultraviolet light.
In the figure, 1-4 samples of patchouli control medicinal material, 5 samples of patchouli water decoction, 6 samples of patchouli alcohol control, ① and ② respectively indicate characteristic spots ① and ②.
Detailed Description
The following examples illustrate the invention in detail. The raw materials and various devices used in the invention are conventional commercially available products, and can be directly obtained by market purchase.
Example 1, sample preparation.
A-1, preparation of a test sample: placing 1g herba Agastaches powder in conical flask, adding 30mL ethanol, ultrasonic extracting for 30min, filtering, evaporating filtrate to dryness (naturally volatilizing or evaporating below 60 deg.C to near dryness), and dissolving residue with 1mL methanol to obtain sample solution; wherein the herba Agastaches powder is coarse powder obtained by pulverizing herba Agastaches or decoction pieces.
A-2, preparing a patchouli non-volatile part reference substance: taking 1g of patchouli powder, adding 30mL of water for dissolving, extracting twice with 40mL of ethyl acetate, 20mL each time, combining the extract solutions, evaporating to dryness, and adding 1mL of ethanol for dissolving the residue to be used as a reference substance solution of the non-volatile part of the patchouli, wherein the patchouli powder is water-decocted dry extract powder of patchouli medicinal materials or decoction pieces, and the preparation method for the water-decocted dry extract powder comprises the following steps: extracting herba Agastaches with heat (generally at 100 deg.C) under reflux for 3 times (each time for 0.8-1.2 hr), filtering, concentrating the filtrate, evaporating to dry, and grinding into powder.
A-3, preparation of a patchouli alcohol reference substance: adding ethanol into patchouli alcohol reference substance to obtain 2mg/ml patchouli alcohol reference substance solution.
Example 2, thin layer chromatography.
B-1, developing by thin-layer chromatography: according to a thin-layer chromatography test method, sucking 5 muL of the test sample solution obtained in the step A-1, and 10 muL of each of the patchouli non-volatile part reference substance solution and the patchouli alcohol reference substance solution obtained in the steps A-2 and A-3, dropping the solution on the same silica gel G thin layer plate, and developing, taking out and airing the solution by using petroleum ether, ethyl acetate, methanol and formic acid =7.50:1.80:1.00:0.125 as developing agents.
B-2, color development: and B-1, spraying a 5% aluminum trichloride ethanol solution on the sample, and heating at 110 ℃ until spots are clear.
Example 3, dual map identification.
C-1, performing first inspection, namely referring to the attached figure 1, observing the patchouli alcohol reference substance and the atlas of the sample to be detected obtained in the step B under the sunlight, wherein the patchouli alcohol reference substance has a characteristic spot ① at the position F =0.80, and the characteristic spot ① is a quasi-circular characteristic spot, and the color tone is light blue, in contrast, observing whether the sample to be detected has a characteristic spot ① near the position RF =0.80, if the atlas to be detected does not have the characteristic spot ①, identifying the sample to be detected as a patchouli counterfeit product, finishing the identification, and if the atlas to be detected has the characteristic spot ①, entering the step C-2;
and C-2, a second inspection, referring to the attached figure 2, further observing the sample spectrum with characteristic spots ① and the herba pogostemonis non-volatile part reference substance spectrum under an ultraviolet lamp, and observing the herba pogostemonis non-volatile part reference substance spectrum with characteristic spots ② at the position of RF =0.29 and characteristic spots ② as similar round characteristic spots with the characteristics of clear spots and good separation degree, in contrast, observing whether the to-be-detected sample has the characteristic spots ② near the position of RF =0.29, if the to-be-detected spectrum has the characteristic spots ②, determining that the detected sample is a herba pogostemonis genuine product and the identification is finished, and if the to-be-detected spectrum does not have the characteristic spots ②, determining that the detected sample is a herba pogostemonis similar product and the identification is finished.
Example 4, thin layer chromatography assay methods.
The specific procedures for the thin layer chromatography test in example 2 are as follows.
4.1 instruments and materials
(1) The thin-layer plate is divided into a glass plate, a plastic plate or an aluminum plate and the like according to the material of the support; according to the stationary phase, the composite material is divided into a silica gel thin layer plate, a bonded silica gel plate, a microcrystalline cellulose thin layer plate, a polyamide thin layer plate, an alumina thin layer plate and the like. The fixing phase can be added with adhesive and fluorescent agent. Silicone thin layer plates are commonly used with silicone G, silicone GF254, silicone H, silicone HF254, G, H indicating the presence or absence of paste binders. F254 is fluorescent agent which shows green background under 254nm wavelength of ultraviolet light. The thin layer plate can be specially treated and chemically modified to meet the separation requirement on the premise of ensuring the chromatographic quality by being divided into a common thin layer plate (10-40 mu m) and a high-efficiency thin layer plate (5-10 mu m) according to the particle size of the stationary phase, and the thin layer plate can be self-made in a laboratory. The particle size of the stationary phase is generally required to be 10-40 μm. The glass plate should be smooth and flat, and no water drops are attached after cleaning.
(2) The sample applicator generally adopts a microliter capillary or a manual, semi-automatic or full-automatic sample applicator material.
(3) The upward expansion of the expansion container can be realized by a special flat bottom or a double-groove expansion cylinder which is suitable for the size of a thin-layer plate, and the expansion container needs to be closed when being expanded. The horizontal expansion is realized by a special horizontal expansion groove.
(4) The color developing device should use glass spray bottle or special sprayer to spray color developing agent in uniform fine mist shape with compressed gas; the dipping and color development can be replaced by a special glass apparatus or a proper developing cylinder; the steam fumigation developing can be replaced by a double-groove developing cylinder or a dryer with proper size.
(5) The inspection device is a dark box provided with visible light, 254nm and 365nm ultraviolet light sources and corresponding filters, and can be additionally provided with camera equipment for shooting images. The light source in the dark box should have sufficient illuminance.
4.2 method of operation
(1) Thin layer plate preparation
Commercially available laminae should typically be activated for 30 minutes at 110 ℃ just prior to use. The polyamide film does not require activation. The aluminum substrate thin-layer plate and the plastic thin-layer plate can be cut according to the needs, but the fixed phase layer at the bottom edge of the cut thin-layer plate is not damaged. If the product is polluted by impurities in the air during storage, the product can be developed and pre-washed on a developing cylinder by chloroform, methanol or a mixed solvent of the chloroform and the methanol before use, dried, activated at 110 ℃, and placed in a dryer for later use.
Except for other provisions, the self-made thin-layer plate is prepared by grinding and mixing 1 part of stationary phase and 3 parts of water (or an aqueous solution added with a binder, such as a 0.2-0.5% sodium carboxymethyl cellulose aqueous solution or a modifier solution with a prescribed concentration) in a mortar in the same direction, removing bubbles on the surface, pouring the mixture into a coater, coating the mixture on a glass plate by smoothly moving the coater (the thickness is 0.2-0.3mm), taking down the glass plate coated with a thin layer, airing the glass plate on a horizontal table at room temperature, drying the glass plate at 110 ℃ for 30 minutes, and then placing the glass plate in a drying box with a drying agent for later use. The uniformity of the coating is checked before use, and the coating is inspected under reflected light and perspective light, and the surface is uniform, flat and smooth, and has no pock, bubble, damage or pollution.
(2) The spotting is performed on the thin-layer plate by using a special capillary or matching with a corresponding semi-automatic and automatic spotting apparatus in a clean and dry environment except for other provisions. Generally in the shape of a dot or narrow and thin strip, the dot base line is 10-15mm away from the bottom edge, the high-efficiency plate is generally 8-lO mm away from the bottom edge, the diameter of the dot is generally not more than 4mm, and the high-efficiency plate is generally not more than 2 mm. Care was taken not to damage the surface of the thin layer during contact spotting. The width of the strip is 5-10mm generally, the width of the high-efficiency strip is 4-8mm generally, and the sample can be applied by a special semi-automatic or automatic sample application device through a spraying method. The distance between the points is preferably that the adjacent spots are not interfered with each other due to the visible spot diffusion condition, generally not less than 8mm, and the interval of the high-efficiency board test article is not less than 5 mm.
(3) And (4) spreading, namely putting the thin-layer plate with the sample in a spreading cylinder, immersing the thin-layer plate into a spreading agent to a depth of 5mm from the original thin-layer plate, and sealing. And generally spreading the high-efficiency thin-layer plate upwards for 8-15cm and spreading the high-efficiency thin-layer plate upwards for 5-8cm, except for other provisions. And (4) taking out the thin-layer plate when the front edge of the solvent reaches a specified spreading distance, airing and detecting.
If solvent vapor pre-equilibrium is needed before the development, a proper amount of developing agent can be added into a development cylinder, and the development cylinder is sealed and kept for 15 to 30 minutes generally. After the solvent vapor is pre-balanced, the thin-layer plate carrying the test article is put on the human body quickly, and then the thin-layer plate is closed and unfolded immediately. If the developing cylinder is required to be saturated with the solvent vapor, a piece of filter paper having the same height and width as those of the developing cylinder is attached to the inner wall of the developing cylinder, one end of the filter paper is immersed in the developing agent, the developing cylinder is sealed for a certain time, the solvent vapor is saturated, and then the developing cylinder is developed by the method.
If necessary, the thin-layer plate can be expanded for the second time or expanded in two directions, and the residual expanding agent of the thin-layer plate is completely volatilized before the second expansion.
(4) The color developing and inspecting material can be directly inspected under visible light, and the colorless material can be developed with suitable developer by spraying or soaking method, or developed by heating and inspected under visible light. Fluorescent spots can be observed under an ultraviolet lamp (365 nm or 254nm) by using fluorescent substances or substances capable of exciting to generate fluorescence after development. For the components having absorption under ultraviolet light, spots formed by quenching of fluorescent substances on the surface of a fluorescent plate can be observed under an ultraviolet lamp (254 nm) by using a thin layer plate (such as a silica gel GF254 plate) with the fluorescent agents.
(5) Recording thin layer chromatography images can generally be taken with an image capture device and stored in the form of an optical or electronic image. The corresponding chromatogram can also be recorded by scanning with a thin layer chromatography scanner or other suitable means.
4.3 System suitability test
The system applicability test is carried out on the experimental conditions according to the requirements of variety items, namely, the experimental conditions are tested and adjusted by the test sample and the standard substance, and the requirements are met.
(1) The shift value (Rf) refers to the ratio of the distance from the baseline to the center of the developed spot to the distance from the baseline to the front edge of the developing agent.
(2) When the separation degree (or called separation efficiency) is identified, spots in the chromatogram of the test sample and the standard substance are clearly separated.
4.4 assay
The identification method comprises preparing test solution and reference standard solution, spotting, developing and inspecting on the same thin layer plate, wherein the position and color (or fluorescence) of spots in chromatogram of the test solution are identical to those of standard substance chromatogram.
In summary, the novel detection method and the detection program provided by the invention have the characteristics of high precision, wide application range and comprehensive detection results, can quickly and conveniently classify and identify the genuine products, the similar products and the fake products of the samples to be detected, and are a novel practical method with obviously improved detection effect compared with the existing method.
The above description is only presented as an enabling solution for the present invention and should not be taken as a sole limitation on the solution itself.

Claims (6)

1. The thin-layer identification method of the pogostemon cablin is characterized by comprising the following steps of: firstly, preparing a sample to be tested, developing a spectrum by using petroleum ether-ethyl acetate-methanol-formic acid as a developing agent according to a thin-layer chromatography test method, finally, respectively identifying the spectrum obtained under different developing agents by adopting a double identification method, checking whether the spectrum to be tested has a first characteristic spot and/or a second characteristic spot, and identifying the sample to be tested as a patchouli genuine product, a similar product or a fake product; the method comprises the following steps:
A. preparation of test samples: placing 1g herba Agastaches powder in conical flask, adding 30mL ethanol, ultrasonic extracting for 30min, filtering, naturally volatilizing filtrate or steaming below 60 deg.C to near dry, and dissolving residue with 1mL methanol to obtain sample solution;
B. and (3) developing by thin-layer chromatography: according to a thin-layer chromatography test method, absorbing 5 mu L of the test solution obtained in the step A, dropping the sample solution on a silica gel G thin-layer plate, taking out and drying the sample solution by taking petroleum ether, ethyl acetate, methanol and formic acid =7.50:1.80:1.00:0.125 as a developing agent according to the volume ratio, spraying a 5% aluminum trichloride ethanol solution, and heating the sample solution at 110 ℃ until spots are clear;
C. two-fold map identification method:
c-1, carrying out first inspection, namely observing the map obtained in the step B in the sunlight, observing whether the map has a characteristic spot ① at the position of RF =0.77-0.83, identifying the detected sample as a patchouli counterfeit product if the map to be inspected does not have the characteristic spot ①, and entering the step C-2 if the map to be inspected has the characteristic spot ①;
and C-2, performing secondary inspection, namely further inspecting whether the sample map with the characteristic spot ① has the characteristic spot ② at the position of RF =0.26-0.32 under an ultraviolet lamp, if the map to be inspected has the characteristic spot ②, determining that the detected sample is a patchouli genuine product and the identification is finished, and if the map to be inspected does not have the characteristic spot ②, determining that the detected sample is a patchouli approximant product and the identification is finished.
2. The method for identifying the thin layer of pogostemon cablin according to claim 1, wherein: in the step A, the patchouli powder is coarse powder obtained by crushing a patchouli medicinal material or decoction pieces.
3. The method for identifying the thin layer of pogostemon cablin according to claim 1, wherein: in step C-1, the solar inspection is a transmission inspection, the RF = 0.80.
4. The method for identifying Pogostemon cablin thin layer according to claim 1, wherein in step C-1, said characteristic spots ① are quasi-circular characteristic spots with distinct spots and good resolution.
5. The method for identifying the thin layer of pogostemon cablin according to claim 1, wherein: in step C-2, the wavelength of the ultraviolet light is 365nm, and the RF = 0.29.
6. The method for identifying Pogostemon cablin thin layer according to claim 1, wherein said characteristic spots ② are feature spots similar to a circle and have a uniform pale blue color in step C-2.
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