CN114487252A - Thin-layer chromatography identification method for distinguishing antrodia camphorata and antrodia camphorata wood - Google Patents
Thin-layer chromatography identification method for distinguishing antrodia camphorata and antrodia camphorata wood Download PDFInfo
- Publication number
- CN114487252A CN114487252A CN202111629081.8A CN202111629081A CN114487252A CN 114487252 A CN114487252 A CN 114487252A CN 202111629081 A CN202111629081 A CN 202111629081A CN 114487252 A CN114487252 A CN 114487252A
- Authority
- CN
- China
- Prior art keywords
- antrodia camphorata
- thin
- silica gel
- layer plate
- raw material
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 241001486992 Taiwanofungus camphoratus Species 0.000 title claims abstract description 158
- 239000002023 wood Substances 0.000 title claims abstract description 46
- 238000000034 method Methods 0.000 title claims abstract description 26
- 238000004809 thin layer chromatography Methods 0.000 title claims abstract description 25
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 54
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 77
- 239000002994 raw material Substances 0.000 claims description 66
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 45
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 45
- 239000007788 liquid Substances 0.000 claims description 33
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims description 30
- 238000007689 inspection Methods 0.000 claims description 21
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 20
- 238000005286 illumination Methods 0.000 claims description 19
- 238000005507 spraying 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 15
- 235000019253 formic acid Nutrition 0.000 claims description 15
- 238000002360 preparation method Methods 0.000 claims description 14
- 239000003153 chemical reaction reagent Substances 0.000 claims description 13
- ROAYSRAUMPWBQX-UHFFFAOYSA-N ethanol;sulfuric acid Chemical compound CCO.OS(O)(=O)=O ROAYSRAUMPWBQX-UHFFFAOYSA-N 0.000 claims description 10
- 239000000706 filtrate Substances 0.000 claims description 10
- 238000001914 filtration Methods 0.000 claims description 10
- 239000012528 membrane Substances 0.000 claims description 9
- 238000002137 ultrasound extraction Methods 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 8
- 238000007873 sieving Methods 0.000 claims description 8
- DSSYKIVIOFKYAU-XCBNKYQSSA-N (R)-camphor Chemical compound C1C[C@@]2(C)C(=O)C[C@@H]1C2(C)C DSSYKIVIOFKYAU-XCBNKYQSSA-N 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 7
- 229920006395 saturated elastomer Polymers 0.000 claims description 7
- 238000007789 sealing Methods 0.000 claims description 7
- 241000386927 Cinnamomum micranthum f. kanehirae Species 0.000 claims description 6
- 238000007664 blowing Methods 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 5
- 244000082946 Tarchonanthus camphoratus Species 0.000 claims description 3
- 235000005701 Tarchonanthus camphoratus Nutrition 0.000 claims description 3
- 238000012216 screening Methods 0.000 claims 1
- 238000001228 spectrum Methods 0.000 abstract description 9
- 238000001514 detection method Methods 0.000 abstract description 6
- 238000011160 research Methods 0.000 abstract description 5
- 238000004458 analytical method Methods 0.000 abstract description 4
- 230000000007 visual effect Effects 0.000 abstract description 4
- 239000007791 liquid phase Substances 0.000 abstract description 3
- 239000000523 sample Substances 0.000 abstract 1
- 239000012488 sample solution Substances 0.000 abstract 1
- 239000002904 solvent Substances 0.000 description 12
- 238000001816 cooling Methods 0.000 description 5
- 239000000047 product Substances 0.000 description 5
- 241000723346 Cinnamomum camphora Species 0.000 description 4
- 238000005485 electric heating Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 241000723347 Cinnamomum Species 0.000 description 2
- 239000003086 colorant Substances 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 208000004998 Abdominal Pain Diseases 0.000 description 1
- 206010012735 Diarrhoea Diseases 0.000 description 1
- 206010016952 Food poisoning Diseases 0.000 description 1
- 208000019331 Foodborne disease Diseases 0.000 description 1
- 241000233866 Fungi Species 0.000 description 1
- 206010020772 Hypertension Diseases 0.000 description 1
- 208000003251 Pruritus Diseases 0.000 description 1
- 206010070863 Toxicity to various agents Diseases 0.000 description 1
- 230000003110 anti-inflammatory effect Effects 0.000 description 1
- 230000003064 anti-oxidating effect Effects 0.000 description 1
- 230000000259 anti-tumor effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000004069 differentiation Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 238000003306 harvesting Methods 0.000 description 1
- 238000004128 high performance liquid chromatography Methods 0.000 description 1
- 230000007365 immunoregulation Effects 0.000 description 1
- 210000004185 liver Anatomy 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000000144 pharmacologic effect Effects 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 239000010979 ruby Substances 0.000 description 1
- 229910001750 ruby Inorganic materials 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 238000009210 therapy by ultrasound Methods 0.000 description 1
Images
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/90—Plate chromatography, e.g. thin layer or paper chromatography
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/34—Purifying; Cleaning
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/90—Plate chromatography, e.g. thin layer or paper chromatography
- G01N30/94—Development
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/30—Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change
Landscapes
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Engineering & Computer Science (AREA)
- Biomedical Technology (AREA)
- Molecular Biology (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention relates to a thin-layer chromatography analysis method, in particular to a thin-layer chromatography identification method for distinguishing antrodia camphorata and antrodia camphorata wood. The technical problems that the existing research method for identifying the liquid-phase fingerprint spectrum of the antrodia camphorata is single in spectrum, complex to operate and incapable of visually distinguishing the antrodia camphorata and the antrodia camphorata are solved. The method comprises the following steps: 1) preparing a sample solution; 2) carrying out thin-layer sample application; 3) preparing a developing agent; 4) unfolding; 5) and (5) developing and identifying. The thin-layer chromatography identification method has the advantages of rapidness, low cost, simplicity, high efficiency, strong specificity, visual detection result, easiness in identification and the like, can be used for rapidly identifying and distinguishing the antrodia camphorata and the antrodia camphorata wood, effectively ensures the quality of the antrodia camphorata, and fills the gap that the thin-layer chromatography research on the antrodia camphorata and the antrodia camphorata wood is not carried out at present.
Description
Technical Field
The invention relates to a thin-layer chromatography analysis method, in particular to a thin-layer chromatography identification method for distinguishing antrodia camphorata and antrodia camphorata wood.
Background
Antrodia camphorata (Antrodiacamphora), also known as Antrodia camphorata, Antrodia camphorata grotto, is generally rotted in the trunk cavities of last century Antrodia camphorata trees. The antrodia camphorata tree is the only host of antrodia camphorata, and the suitable growing area is extremely limited, which leads to the shortage of wild antrodia camphorata resources. The antrodia camphorata is a rare medicinal fungus, and researches show that the antrodia camphorata has various pharmacological effects, such as anti-tumor, anti-inflammatory, anti-oxidation, immunoregulation, liver protection and the like, and can also be used for treating food and drug poisoning, diarrhea, abdominal pain, hypertension, skin pruritus and the like. Antrodia camphorata has been used as a traditional Chinese medicine in Taiwan early and has become a hotspot in recent ten years. Therefore, Antrodia camphorata is called "king in medicine" or "ruby in forest". Due to the excessive harvesting of the cinnamomum kanehirae, the wild cinnamomum kanahirae is increasingly rare, and the cinnamomum kanahirae is listed as a protective tree species in taiwan. The market price of the antrodia camphorata reaches hundreds of thousands or even hundreds of thousands per kilogram, and the market prospect is huge. Due to uniqueness, rarity and magical effect of antrodia camphorata, a large amount of inferior even counterfeit antrodia camphorata medicinal materials appear in the market. The antrodia camphorata is a host for the growth of the antrodia camphorata, so that the antrodia camphorata is replaced by the antrodia camphorata in the market, and the quality credit of the antrodia camphorata is seriously influenced.
Relevant researchers do fingerprint spectrum research on the antrodia camphorata by using a high performance liquid chromatography, but the liquid phase fingerprint spectrum is influenced by factors such as single spectrum, complex operation and the like, so that the quality of the antrodia camphorata cannot be well embodied, and meanwhile, the antrodia camphorata and the antrodia camphorata wood cannot be visually distinguished.
Disclosure of Invention
The invention aims to solve the technical problems that the existing research method for identifying the liquid-phase fingerprint spectrum of the antrodia camphorata has single spectrum and complicated operation, can not well reflect the quality of the antrodia camphorata and can not visually distinguish the antrodia camphorata from the antrodia camphorata, and provides a thin-layer chromatography identification method for distinguishing the antrodia camphorata from the antrodia camphorata. The thin-layer chromatography has the advantages of high separation effect, quick identification, high sensitivity, low cost, visual spectrum and the like, and is widely applied to the production process of traditional Chinese medicinal materials. However, no report on the thin-layer chromatography for distinguishing antrodia camphorata from antrodia camphorata wood is found at present.
The technical scheme of the invention is as follows:
a thin-layer chromatography identification method for distinguishing antrodia camphorata and antrodia camphorata wood is characterized by comprising the following steps:
1) preparation of sample liquid
Taking an antrodia camphorata raw material and an antrodia camphorata wood raw material, crushing, sieving, respectively placing into a sealable test container, respectively adding ethanol with the mass concentration of 70% -100% in an amount which is 6-10 times that of the antrodia camphorata raw material and the antrodia camphorata wood raw material, performing ultrasonic extraction for 30-60 minutes, placing to room temperature, then filtering by adopting a microporous filter membrane, and collecting filtrate as sample liquid;
2) performing thin layer sample application
Sequentially dropping the sample liquid prepared in the step 1) on different positions of the same silica gel G thin-layer plate at the same height to form a dropping point origin;
3) preparation of developing agent
3.1) uniformly mixing toluene, ethyl acetate and formic acid in a volume ratio of 6-10: 4-6: 0.6-1.0 to obtain a developing agent;
3.2) placing the developing agent into an expansion cylinder, sealing the expansion cylinder, and presaturating for 15-20 minutes;
4) is unfolded
4.1) opening the developing cylinder pre-saturated in the step 3), and quickly putting the silica gel G thin-layer plate subjected to sample application in the step 2) into the developing cylinder, so that the silica gel G thin-layer plate is obliquely leaned against the developing cylinder and the developing agent in the developing cylinder cannot exceed the original point of sample application;
4.2) when the front edge of the developing agent ascends to the position 6-10 cm away from the origin of the sample application, taking out the silica gel G thin-layer plate;
5) color development and identification
After the reagent on the silica gel G thin-layer plate developed in the step 4.2) is dried, inspecting under illumination to obtain an inspection view; the Antrodia camphorata raw material which has a plurality of spots and shows more obvious, the Antrodia camphorata raw material which does not show a plurality of spots or the Antrodia camphorata raw material which does not show the spots.
Further, the step 5) is specifically as follows: blowing the reagent on the silica gel G thin layer plate unfolded in the step 4.2) dry, spraying a 5-10% sulfuric acid ethanol solution to the silica gel G thin layer plate, heating at the temperature of 100-; the inspection chart shows that the Antrodia camphorata raw material has spots at Rf (0.18-0.21), Rf (0.40-0.42), Rf (0.50-0.53), Rf (0.54-0.60), Rf (0.60-0.64) and Rf (0.65-0.70) and is obvious; the Cinnamomum kanehirae Hayata is characterized in that spots are respectively formed at Rf (0.58-0.62) and Rf (0.65-0.70) positions, and the spots are not obvious and are shown as Cinnamomum kanehirae raw materials.
Further, the step 5) is specifically as follows: blowing the reagent on the silica gel G thin layer plate unfolded in the step 4.2) dry, spraying a 5-10% sulfuric acid ethanol solution to the silica gel G thin layer plate, heating at the temperature of 100-; the Antrodia camphorata raw material has spots at the positions of Rf (0.18-0.21), Rf (0.40-0.42), Rf (0.50-0.53), Rf (0.54-0.60), Rf (0.60-0.64) and Rf (0.65-0.70); the camphor wood raw material has spots at Rf (0.23-0.28) and Rf (0.36-0.41) respectively and is not obvious.
Further, the step 5) is specifically as follows: drying the reagent on the silica gel G thin-layer plate unfolded in the step 4.2), and inspecting under 254nm ultraviolet illumination to obtain an inspection view; the Antrodia camphorata raw material is characterized in that the spots are respectively formed at the positions of Rf (0.18-0.21), Rf (0.40-0.42), Rf (0.50-0.53), Rf (0.54-0.60), Rf (0.60-0.64) and Rf (0.65-0.70); the spots are not shown and are made of the cinnamomum kanehirae raw material.
Further, the step 1) specifically comprises the steps of taking antrodia camphorata raw materials and antrodia camphorata wood raw materials, crushing, sieving with a 80-mesh sieve, respectively placing into triangular flasks with plugs, respectively adding ethanol with mass concentration of 70% which is 8-10 times of the mass of the antrodia camphorata raw materials and the antrodia camphorata wood raw materials, performing ultrasonic extraction for 60 minutes, placing to room temperature, then filtering with a microporous filter membrane, and collecting filtrate as sample liquid.
Further, in the step 2), the distance between the sample application origin position and the lower edge of the silica gel G thin-layer plate is 1.0-1.5 cm.
Further, in step 3.1), the volume ratio of toluene, ethyl acetate and formic acid is 8:5: 0.8.
Further, in step 3.2), the developing cylinder is a double-groove developing cylinder, the size of the double-groove developing cylinder is 10 × 10cm, 20 × 10cm or 10 × 20cm, the developing agent dosage in the double grooves is kept consistent, and the developing agent is presaturated for 15 minutes.
Further, the step 4.2) is specifically that when the front edge of the developing agent ascends to 8-10 cm away from the sample application origin, the silica gel G thin layer plate is taken out.
Further, in the step 5), the concentration of the sulfuric acid ethanol solution is 10% by mass.
The invention has the beneficial effects that:
1. the invention provides a thin-layer identification method which is rapid, low in cost, simple, convenient, efficient, strong in specificity, visual in detection result and easy to identify, and can solve the problem of identification and differentiation of antrodia camphorata and antrodia camphorata wood.
2. The thin-layer identification method provided by the invention has obvious distinction and easy identification, and can obviously distinguish the antrodia camphorata and the antrodia camphorata wood under 254nm, 365nm and sunlight.
3. According to the invention, a proper amount of ethanol is selected to directly carry out ultrasonic treatment and filtration on the raw medicinal materials, the filtrate is used as a detection solution, and the method has the advantages of simple sample pretreatment, low cost and easiness in operation.
4. According to the invention, toluene, ethyl acetate and formic acid are mixed according to the volume ratio of 6-10: 4-6: 0.6-1.0 to obtain the developing solvent, the spot separation effect is good, the characteristic spots of each sample are prominent, the phenomena of spot tailing and spot diffusion are avoided, the results are obviously compared, and the judgment is easy.
Drawings
FIG. 1 is an examination view of a developed silica gel G thin layer plate under 254nm illumination in an embodiment of the present invention;
FIG. 2 is an examination view of a silica gel G thin-layer plate sprayed with a color developing agent under 365nm illumination in the embodiment of the invention;
FIG. 3 is a view of a silica gel G thin layer plate sprayed with a color developing agent under white light illumination in the embodiment of the present invention.
Detailed Description
The invention is described in further detail below with reference to the figures and the specific embodiments.
Example one
1) Preparation of sample liquid
Taking antrodia camphorata raw materials and antrodia camphorata wood raw materials, crushing, sieving with a 80-mesh sieve, respectively placing into triangular bottles with plugs, respectively adding ethanol with the mass concentration of 70% which is 6 times of the mass of the antrodia camphorata raw materials and the antrodia camphorata wood raw materials, performing ultrasonic extraction for 60 minutes, placing to room temperature, filtering by adopting a microporous filter membrane, and collecting filtrate as sample liquid. In order to ensure accurate results, preparing two parts of antrodia camphorata and antrodia camphorata wood sample liquid respectively, and marking the antrodia camphorata and antrodia camphorata wood sample liquid numbers as No. 1 and No. 2 respectively;
2) performing thin layer sample application
Sequentially dropping the sample liquid prepared in the step 1) on different positions of the same silica gel G thin-layer plate at the same height to form four sample dropping origin points; and the distance from the spotting origin to the lower edge of the silica gel G thin-layer plate is 1.0 cm;
3) preparation of developing agent
3.1) uniformly mixing toluene, ethyl acetate and formic acid in a volume ratio of 8:5:0.8 to prepare 20mL of developing agent, wherein the toluene, the ethyl acetate and the formic acid are pure products.
3.2) placing the developing solvent into a double-groove developing cylinder with the size of 10 multiplied by 10cm, wherein the amount of the developing solvent in the two grooves is consistent, then sealing the developing cylinder, and presaturating for 15 minutes;
4) is unfolded
4.1) opening the developing cylinder pre-saturated in the step 3), and quickly putting the silica gel G thin-layer plate subjected to sample application in the step 2) into the developing cylinder, so that the silica gel G thin-layer plate is obliquely leaned against the developing cylinder and the developing agent in the developing cylinder cannot exceed the original point of sample application;
4.2) taking out the silica gel G thin-layer plate when the developing agent is developed upwards along the thin-layer plate until the front edge of the developing agent is upwards moved to the position 8cm away from the origin of the sample application;
5) color development and identification
Drying the reagent on the silica gel G thin layer plate unfolded in the step 4) by using a blower, and inspecting under 254nm illumination to obtain an inspection view shown in the figure 1;
and spraying a sulfuric acid ethanol solution with the mass ratio concentration of 10% on the silica gel G thin layer plate, then placing the silica gel G thin layer plate on an electric heating plate, heating for 4 minutes at 105 ℃, cooling to room temperature, and inspecting the silica gel G thin layer plate under 365nm ultraviolet light and white light illumination respectively to obtain the inspection views of the graph 2 and the graph 3 respectively.
As shown in fig. 1, before spraying the color developing agent, under 254nm violet light, there are 1 black fluorescent spots at each of Rf 0.18-0.21, Rf 0.40-0.42, Rf 0.50-0.53, Rf 0.54-0.60, Rf 0.60-0.64 and Rf 0.65-0.70 on the silica gel G thin layer plate corresponding to the two sample application positions numbered 1, and 6 corresponding to the antrodia camphorata raw material. And if spots are not obvious or almost no spots are displayed at the two spot application positions with the corresponding serial number of 2, the corresponding sample is the cinnamomum kanehirae raw material.
As shown in fig. 2, after spraying the color developing agent, under 365nm purple light, at two corresponding sample application positions numbered 1 on the silica gel G thin layer plate, 1 spot is respectively located at positions Rf of 0.18 to 0.21, Rf of 0.40 to 0.42, Rf of 0.50 to 0.53, Rf of 0.54 to 0.60, Rf of 0.60 to 0.64 and Rf of 0.65 to 0.70, and 8 spots with different colors are corresponding to the sample, which is the antrodia camphorata raw material. And two corresponding sample application positions with the serial number of 2 respectively have 1 fuzzy spot at the position of Rf & lt 0.58-0.62 & gt and Rf & lt 0.65-0.70 & gt, and the rest spots are not obvious or almost have no spots, so that the corresponding sample is the cinnamomum camphora raw material.
As shown in fig. 3, after spraying the color developing agent, under white light illumination, the silica gel G thin layer plate has 1 spot at each of two spot sample positions corresponding to number 1, where Rf is 0.18-0.21, Rf is 0.40-0.42, Rf is 0.50-0.53, Rf is 0.54-0.60, Rf is 0.60-0.64, and Rf is 0.65-0.70, and the corresponding sample is antrodia camphorata raw material. And at two sample application positions with the corresponding serial number of 2, 1 faint yellow spot is respectively arranged at the position of Rf (0.23-0.28) and Rf (0.36-0.41), the faint yellow spots are not obvious, and the rest spots are very weak or almost have no spots, so that the corresponding sample is the cinnamomum camphora raw material.
Before spraying color developing agent, the inspection picture obtained by inspection under 254nm purple light illumination and the inspection picture obtained by inspection under 365nm purple light and white light illumination after spraying color developing agent can obviously distinguish the antrodia camphorata raw material and the antrodia camphorata wood raw material, but considering that the results are not accurate enough due to incomplete or fuzzy display when not spraying color developing agent, the results are more accurate due to analysis and comparison by combining the inspection picture after spraying color developing agent. In addition, in order to make the result more accurate and reliable, in this embodiment, after spraying the color developing agent, 365nm violet light and white light color spectrum inspections are performed respectively, and the inspection diagrams are verified mutually to ensure the accuracy and reliability of the result.
Example two
1) Preparation of sample liquid
Taking an antrodia camphorata raw material and an antrodia camphorata wood raw material, crushing, sieving with a 80-mesh sieve, respectively placing into triangular bottles with plugs, respectively adding ethanol with the mass concentration of 100% which is 8 times that of the antrodia camphorata raw material and the antrodia camphorata wood raw material, performing ultrasonic extraction for 60 minutes, placing to room temperature, then filtering by adopting a microporous filter membrane, and collecting filtrate as sample liquid. In order to ensure accurate results, preparing two parts of antrodia camphorata and antrodia camphorata wood sample liquid respectively, and marking the antrodia camphorata and antrodia camphorata wood sample liquid numbers as No. 1 and No. 2 respectively;
2) performing thin layer sample application
Sequentially dropping the sample liquid prepared in the step 1) on different positions of the same silica gel G thin-layer plate at the same height to form four sample dropping origin points; and the distance from the sample application origin to the lower edge of the silica gel G thin-layer plate is 1.3 cm;
3) preparation of developing solvent
3.1) uniformly mixing toluene, ethyl acetate and formic acid in a volume ratio of 10:6:1.0 to prepare 20mL of developing agent, wherein the toluene, the ethyl acetate and the formic acid are pure products.
3.2) placing the developing solvent into a double-groove developing cylinder with the size of 10 multiplied by 10cm, wherein the amount of the developing solvent in the two grooves is consistent, then sealing the developing cylinder, and presaturating for 20 minutes;
4) is unfolded
4.1) opening the developing cylinder pre-saturated in the step 3), and quickly putting the silica gel G thin-layer plate subjected to sample application in the step 2) into the developing cylinder, so that the silica gel G thin-layer plate is obliquely leaned against the developing cylinder and the developing agent in the developing cylinder cannot exceed the original point of sample application;
4.2) taking out the silica gel G thin-layer plate when the developing agent is developed upwards along the thin-layer plate until the front edge of the developing agent is upwards moved to the position 6cm away from the origin of the sample application;
5) color development and identification
And (3) drying the reagent on the silica gel G thin layer plate unfolded in the step 4) by using a blower, and inspecting under 254nm illumination to obtain an inspection view similar to that in the figure 1.
EXAMPLE III
1) Preparation of sample liquid
Taking an antrodia camphorata raw material and an antrodia camphorata wood raw material, crushing, sieving with a 80-mesh sieve, respectively placing into triangular bottles with plugs, respectively adding ethanol with the mass concentration of 90% and 6 times of the mass of the antrodia camphorata raw material and the antrodia camphorata wood raw material, performing ultrasonic extraction for 30 minutes, placing to room temperature, then filtering by adopting a microporous filter membrane, and collecting filtrate as sample liquid. In order to ensure accurate results, preparing two parts of antrodia camphorata and antrodia camphorata wood sample liquid respectively, and marking the antrodia camphorata and antrodia camphorata wood sample liquid numbers as No. 1 and No. 2 respectively;
2) performing thin layer sample application
Sequentially dropping the sample liquid prepared in the step 1) on different positions of the same silica gel G thin-layer plate at the same height to form four sample dropping origin points; and the distance from the sample application origin to the lower edge of the silica gel G thin-layer plate is 1.5 cm;
3) preparation of developing agent
3.1) uniformly mixing toluene, ethyl acetate and formic acid in a volume ratio of 8:4:0.7 to prepare 20mL of developing agent, wherein the toluene, ethyl acetate and formic acid are all pure products.
3.2) placing the developing solvent into a double-groove developing cylinder with the size of 10 multiplied by 10cm, wherein the amount of the developing solvent in the two grooves is consistent, then sealing the developing cylinder, and presaturating for 17 minutes;
4) is unfolded
4.1) opening the developing cylinder pre-saturated in the step 3), and quickly putting the silica gel G thin-layer plate subjected to sample application in the step 2) into the developing cylinder, so that the silica gel G thin-layer plate is obliquely leaned against the developing cylinder and the developing agent in the developing cylinder cannot exceed the original point of sample application;
4.2) taking out the silica gel G thin-layer plate when the developing agent spreads upwards along the thin-layer plate until the front edge of the developing agent moves upwards to be 10cm away from the origin of the spotting;
5) color development and identification
And (3) blowing a reagent on the silica gel G thin layer plate unfolded in the step 4) by using a blower, spraying a 5% sulfuric acid ethanol solution in mass ratio to the silica gel G thin layer plate, then placing the silica gel G thin layer plate on an electric heating plate, heating the silica gel G thin layer plate for 5 minutes at 100 ℃, cooling the silica gel G thin layer plate to room temperature, and inspecting the silica gel G thin layer plate under 365nm ultraviolet light illumination to obtain an inspection view consistent with that of the figure 2.
Example four
1) Preparation of sample liquid
Taking the antrodia camphorata raw material and the antrodia camphorata wood raw material, crushing, sieving with a 80-mesh sieve, respectively placing into triangular bottles with plugs, respectively adding ethanol with the mass concentration of 70% which is 10 times of the mass of the antrodia camphorata raw material and the antrodia camphorata wood raw material, performing ultrasonic extraction for 50 minutes, cooling to room temperature, filtering by adopting a microporous filter membrane, and collecting filtrate as sample liquid. In order to ensure accurate results, preparing two parts of antrodia camphorata and antrodia camphorata wood sample liquid respectively, and marking the antrodia camphorata and antrodia camphorata wood sample liquid numbers as No. 1 and No. 2 respectively;
2) performing thin layer sample application
Sequentially dropping the sample liquid prepared in the step 1) on different positions of the same silica gel G thin-layer plate at the same height to form four sample dropping origin points; and the distance from the sample application origin to the lower edge of the silica gel G thin-layer plate is 1.0 cm;
3) preparation of developing agent
3.1) uniformly mixing toluene, ethyl acetate and formic acid in a volume ratio of 6:5:0.6 to prepare 20mL of developing agent, wherein the toluene, the ethyl acetate and the formic acid are pure products.
3.2) placing the developing solvent into a double-groove developing cylinder with the size of 10 multiplied by 10cm, wherein the amount of the developing solvent in the two grooves is consistent, then sealing the developing cylinder, and presaturating for 15 minutes;
4) is unfolded
4.1) opening the developing cylinder pre-saturated in the step 3), and quickly putting the silica gel G thin-layer plate subjected to sample application in the step 2) into the developing cylinder, so that the silica gel G thin-layer plate is obliquely leaned against the developing cylinder and the developing agent in the developing cylinder cannot exceed the original point of sample application;
4.2) taking out the silica gel G thin-layer plate when the developing agent is developed upwards along the thin-layer plate until the front edge of the developing agent is upwards moved to the position 8cm away from the origin of the sample application;
5) color development and identification
And (3) blowing a reagent on the silica gel G thin layer plate unfolded in the step 4) by using a blower, spraying a sulfuric acid ethanol solution with the mass ratio concentration of 7% on the silica gel G thin layer plate, then placing the silica gel G thin layer plate on an electric heating plate, heating at 110 ℃ for 3 minutes, cooling to room temperature, and inspecting the silica gel G thin layer plate under white light illumination to obtain an inspection view consistent with that of the figure 3.
EXAMPLE five
1) Preparation of sample liquid
Taking an antrodia camphorata raw material and an antrodia camphorata wood raw material, crushing, sieving with a 80-mesh sieve, respectively placing into triangular bottles with plugs, respectively adding ethanol with the mass concentration of 70% which is 6 times that of the antrodia camphorata raw material and the antrodia camphorata wood raw material, performing ultrasonic extraction for 30 minutes, placing to room temperature, then filtering by adopting a microporous filter membrane, and collecting filtrate as sample liquid. In order to ensure accurate results, preparing two parts of antrodia camphorata and antrodia camphorata wood sample liquid respectively, and marking the serial numbers of the antrodia camphorata and antrodia camphorata wood sample liquid as No. 1 and No. 2 respectively;
2) carrying out thin layer sample application
Sequentially dropping the sample liquid prepared in the step 1) on different positions of the same silica gel G thin-layer plate at the same height to form four sample dropping origin points; and the distance from the sample application origin to the lower edge of the silica gel G thin-layer plate is 1.5 cm;
3) preparation of developing agent
3.1) uniformly mixing toluene, ethyl acetate and formic acid in a volume ratio of 6:4:0.6 to prepare 20mL of developing agent, wherein the toluene, the ethyl acetate and the formic acid are pure products.
3.2) placing the developing solvent into a double-groove developing cylinder with the size of 10 multiplied by 10cm, wherein the amount of the developing solvent in the two grooves is consistent, then sealing the developing cylinder, and presaturating for 20 minutes;
4) is unfolded
4.1) opening the developing cylinder pre-saturated in the step 3), and quickly putting the silica gel G thin-layer plate subjected to sample application in the step 2) into the developing cylinder, so that the silica gel G thin-layer plate is obliquely leaned against the developing cylinder and the developing agent in the developing cylinder cannot exceed the original point of sample application;
4.2) taking out the silica gel G thin-layer plate when the developing agent is developed upwards along the thin-layer plate until the front edge of the developing agent is upwards moved to the position 6cm away from the origin of the sample application;
5) color development and identification
Drying the reagent on the silica gel G thin layer plate unfolded in the step 4) by using a blower, spraying a sulfuric acid ethanol solution with the mass ratio concentration of 10% onto the silica gel G thin layer plate, then placing the silica gel G thin layer plate on an electric heating plate, heating at 105 ℃ for 5 minutes, cooling to room temperature, respectively inspecting the silica gel G thin layer plate under 365nm ultraviolet light and white light illumination to respectively obtain inspection views, wherein the obtained inspection views are respectively similar to those in the figures 2 and 3.
The inspection graphs obtained in the second to fifth embodiments correspond to the inspection graph obtained in the first embodiment, and the experimental result analysis shows that before spraying the color developing agent, under 254nm illumination, fluorescence spots of 0.18 to 0.21 Rf, 0.40 to 0.42 Rf, 0.50 to 0.53 Rf, 0.54 to 0.60 Rf, 0.60 to 0.64 Rf and 0.65 to 0.70 Rf are obtained at two sample application positions corresponding to number 1 on the silica gel G thin layer plate. And spots are not obvious or hardly exist at the two spots with the corresponding number of 2. After spraying the color developing agent, under 365nm purple light illumination, spots are respectively arranged at two spot-sample positions with the number of 1 on the silica gel G thin layer plate, wherein the spots are spots with different colors at the positions of Rf (0.18-0.21), Rf (0.40-0.42), Rf (0.50-0.53), Rf (0.54-0.60), Rf (0.60-0.64) and Rf (0.65-0.70), and the Antrodia camphorata raw material is obtained. And two corresponding sample application positions with the number of 2 have fuzzy spots at the positions of Rf & lt 0.58-0.62 & gt and Rf & lt 0.65-0.70 & gt, and the rest spots are not obvious or almost have no spots, so that the cinnamomum camphora raw material is obtained. After spraying the color developing agent, under the illumination of white light, two sample application positions with the number of 1 are correspondingly arranged on the silica gel G thin layer plate, spots are respectively arranged at positions with Rf being 0.18-0.21, Rf being 0.40-0.42, Rf being 0.50-0.53, Rf being 0.54-0.60, Rf being 0.60-0.64 and Rf being 0.65-0.70, and the spots are brown spots with different depths, and the Antrodia camphorata raw material is obtained. And (3) at two sample application positions with the corresponding number of 2, light yellow spots are respectively arranged at positions with Rf of 0.23-0.28 and Rf of 0.36-0.41, the light yellow spots are not obvious, and the rest spots are very weak or almost have no spots, so that the cinnamomum camphora raw material is obtained.
The invention provides a thin-layer chromatography identification method for antrodia camphorata and antrodia camphorata wood, and a thin-layer chromatography detection view of the antrodia camphorata and the antrodia camphorata wood is obtained, and in practical application, a sample needing to be identified or distinguished can be compared with the detection view obtained by the invention, so that the antrodia camphorata and the antrodia camphorata wood can be distinguished, or whether the sample is real antrodia camphorata or real antrodia camphorata wood is distinguished.
The thin-layer chromatography identification method provided by the invention has the advantages of rapidness, low cost, simplicity, high efficiency, strong specificity, visual detection result, obvious comparison and distinction and easy identification, and can obviously distinguish the antrodia camphorata and the antrodia camphorata wood under 254nm, 365nm and white light.
Claims (10)
1. A thin-layer chromatography identification method for distinguishing antrodia camphorata and antrodia camphorata wood is characterized by comprising the following steps:
1) preparation of sample liquid
Taking an antrodia camphorata raw material and an antrodia camphorata wood raw material, crushing, sieving, respectively placing into a sealable test container, respectively adding ethanol with the mass concentration of 70% -100% in an amount of 6-10 times that of the antrodia camphorata raw material and the antrodia camphorata wood raw material, performing ultrasonic extraction for 30-60 minutes, placing to room temperature, filtering by adopting a microporous filter membrane, and collecting filtrate as sample liquid;
2) performing thin layer sample application
Sequentially dropping the sample liquid prepared in the step 1) on different positions of the same silica gel G thin-layer plate at the same height to form a dropping point origin;
3) preparation of developing agent
3.1) uniformly mixing toluene, ethyl acetate and formic acid in a volume ratio of 6-10: 4-6: 0.6-1.0 to obtain a developing agent;
3.2) placing the developing agent into an expansion cylinder, sealing the expansion cylinder, and presaturating for 15-20 minutes;
4) is unfolded
4.1) opening the developing cylinder pre-saturated in the step 3), and quickly putting the silica gel G thin-layer plate subjected to sample application in the step 2) into the developing cylinder, so that the silica gel G thin-layer plate is obliquely leaned against the developing cylinder and the developing agent in the developing cylinder cannot exceed the original point of sample application;
4.2) when the front edge of the developing agent ascends to the position 6-10 cm away from the origin of the sample application, taking out the silica gel G thin-layer plate;
5) color development and identification
After the reagent on the silica gel G thin-layer plate developed in the step 4.2) is dried, inspecting under illumination to obtain an inspection view; the Antrodia camphorata raw material which has a plurality of spots and shows more obvious, the Antrodia camphorata raw material which does not show a plurality of spots or the Antrodia camphorata raw material which does not show the spots.
2. The TLC identification method for differentiating Antrodia camphorata from Antrodia camphorata according to claim 1, wherein the step 5) is specifically as follows: blowing the reagent on the silica gel G thin layer plate unfolded in the step 4.2) dry, spraying a 5-10% sulfuric acid ethanol solution to the silica gel G thin layer plate, heating at the temperature of 100-; the Antrodia camphorata raw material has spots at Rf (0.18-0.21), Rf (0.40-0.42), Rf (0.50-0.53), Rf (0.54-0.60), Rf (0.60-0.64) and Rf (0.65-0.70); the spots are respectively marked at the Rf of 0.58 to 0.62 and the Rf of 0.65 to 0.70, and the spots are not obvious as the raw material of the camphor wood.
3. The TLC identification method for differentiating Antrodia camphorata from Antrodia camphorata according to claim 1, wherein the step 5) is specifically as follows: blowing the reagent on the silica gel G thin layer plate unfolded in the step 4.2) dry, spraying a 5-10% sulfuric acid ethanol solution to the silica gel G thin layer plate, heating at the temperature of 100-; the Antrodia camphorata raw material has spots at the positions of Rf (0.18-0.21), Rf (0.40-0.42), Rf (0.50-0.53), Rf (0.54-0.60), Rf (0.60-0.64) and Rf (0.65-0.70); the camphor wood raw material has spots at Rf (0.23-0.28) and Rf (0.36-0.41) respectively and is not obvious.
4. The TLC identification method for differentiating Antrodia camphorata from Antrodia camphorata according to claim 1, wherein the step 5) is specifically as follows: drying the reagent on the silica gel G thin-layer plate unfolded in the step 4.2), and inspecting under 254nm ultraviolet illumination to obtain an inspection view; the Antrodia camphorata raw material is characterized in that the spots are respectively formed at the positions of Rf (0.18-0.21), Rf (0.40-0.42), Rf (0.50-0.53), Rf (0.54-0.60), Rf (0.60-0.64) and Rf (0.65-0.70); the spots are not shown and are made of the cinnamomum kanehirae raw material.
5. The TLC identification method for differentiating Antrodia camphorata from Antrodia camphorata according to any one of claims 1 to 4, wherein:
specifically, the method comprises the steps of 1), taking antrodia camphorata raw materials and antrodia camphorata wood raw materials, crushing, screening by a 80-mesh sieve, respectively placing in triangular flasks with plugs, respectively adding ethanol with mass concentration of 70% and 8-10 times of the mass of the antrodia camphorata raw materials and the antrodia camphorata wood raw materials, performing ultrasonic extraction for 60 minutes, placing to room temperature, filtering by a microporous filter membrane, and collecting filtrate as sample liquid.
6. The TLC identification method for differentiating Antrodia camphorata from Antrodia camphorata according to claim 5, wherein:
in the step 2), the distance between the spotting origin position and the lower edge of the silica gel G thin-layer plate is 1.0-1.5 cm.
7. The TLC identification method for differentiating Antrodia camphorata from Antrodia camphorata according to claim 6, wherein:
in step 3.1), the volume ratio of toluene, ethyl acetate and formic acid is 8:5: 0.8.
8. The TLC identification method for differentiating Antrodia camphorata from Antrodia camphorata according to claim 7, wherein:
in the step 3.2), the developing cylinder adopts a double-groove developing cylinder, the size of the double-groove developing cylinder is 10 multiplied by 10cm, 20 multiplied by 10cm or 10 multiplied by 20cm, the developing agent dosage in the double grooves is kept consistent, and the developing agent is presaturated for 15 minutes.
9. The TLC identification method for differentiating Antrodia camphorata from Antrodia camphorata according to claim 8, wherein:
and step 4.2) specifically, taking out the silica gel G thin-layer plate when the front edge of the developing agent ascends to 8-10 cm away from the origin of the spotting.
10. The TLC identification method for differentiating Antrodia camphorata from Antrodia camphorata according to claim 2 or 3, wherein:
in the step 5), the mass ratio concentration of the sulfuric acid ethanol solution is 10%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111629081.8A CN114487252B (en) | 2021-12-28 | 2021-12-28 | Thin-layer chromatography identification method for distinguishing Antrodia camphorata from Antrodia camphorata |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111629081.8A CN114487252B (en) | 2021-12-28 | 2021-12-28 | Thin-layer chromatography identification method for distinguishing Antrodia camphorata from Antrodia camphorata |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN114487252A true CN114487252A (en) | 2022-05-13 |
| CN114487252B CN114487252B (en) | 2024-03-26 |
Family
ID=81495338
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202111629081.8A Active CN114487252B (en) | 2021-12-28 | 2021-12-28 | Thin-layer chromatography identification method for distinguishing Antrodia camphorata from Antrodia camphorata |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN114487252B (en) |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| TW201029658A (en) * | 2009-02-13 | 2010-08-16 | Univ Kaohsiung Medical | Ethanol extract of antrodia camphorata for inducing apoptosis and preparation method thereof |
| TW201623208A (en) * | 2014-12-30 | 2016-07-01 | 合一生技股份有限公司 | Compounds from antrodia camphorata, method for preparing the same and use thereof |
| TW201831436A (en) * | 2017-02-24 | 2018-09-01 | 郭盈妤 | Compound isolated from Antrodia camphorata and applications therefor capable of being used as a pharmaceutical product to inhibit the growth of cancerous cells |
| CN110687243A (en) * | 2019-10-29 | 2020-01-14 | 陕西嘉禾生物科技股份有限公司 | Thin-layer detection method for rapidly identifying honeysuckle and lonicera confusa |
| JP6633717B1 (en) * | 2018-10-30 | 2020-01-22 | 科捷生物科技股▲ふん▼有限公司 | Pharmaceutical composition for prevention and / or treatment of liver fibrosis and application thereof |
-
2021
- 2021-12-28 CN CN202111629081.8A patent/CN114487252B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| TW201029658A (en) * | 2009-02-13 | 2010-08-16 | Univ Kaohsiung Medical | Ethanol extract of antrodia camphorata for inducing apoptosis and preparation method thereof |
| TW201623208A (en) * | 2014-12-30 | 2016-07-01 | 合一生技股份有限公司 | Compounds from antrodia camphorata, method for preparing the same and use thereof |
| TW201831436A (en) * | 2017-02-24 | 2018-09-01 | 郭盈妤 | Compound isolated from Antrodia camphorata and applications therefor capable of being used as a pharmaceutical product to inhibit the growth of cancerous cells |
| JP6633717B1 (en) * | 2018-10-30 | 2020-01-22 | 科捷生物科技股▲ふん▼有限公司 | Pharmaceutical composition for prevention and / or treatment of liver fibrosis and application thereof |
| CN110687243A (en) * | 2019-10-29 | 2020-01-14 | 陕西嘉禾生物科技股份有限公司 | Thin-layer detection method for rapidly identifying honeysuckle and lonicera confusa |
Non-Patent Citations (4)
| Title |
|---|
| WONG JACK HO等: "Mushroom extracts and compounds with suppressive action on breast cancer: evidence from studies using cultured cancer cells, tumor-bearing animals, and clinical trials", 《 APPLIED MICROBIOLOGY AND BIOTECHNOLOGY》, vol. 104, 31 December 2020 (2020-12-31), pages 1 - 29 * |
| 吴雨: "皿培式牛樟芝化学成分及质量控制和活性研究", 《中国优秀硕士论文电子期刊网》, no. 07, 15 July 2019 (2019-07-15), pages 79 - 89 * |
| 张寅等: "薄层色谱-分光光度法测定樟芝菌粉中的总三萜含量", 《天然产物研究与开发》, vol. 22, no. 04, 31 December 2010 (2010-12-31), pages 639 - 642 * |
| 李沁等: "UPLC法同时测定牛樟芝子实体中7个三萜类成分的含量", 《药物分析杂志》, vol. 41, no. 09, 30 September 2021 (2021-09-30), pages 1576 - 1582 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN114487252B (en) | 2024-03-26 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107843677B (en) | Radix paeoniae rubra control extract and preparation method and application thereof | |
| CN109254107A (en) | The general tea Fast Classification discrimination method of mandarin orange | |
| CN108008026B (en) | Method for synchronously detecting 13 colorants in hawthorn pills | |
| CN108088715B (en) | Moutan bark reference extract and preparation method and application thereof | |
| CN111189954A (en) | Method for detecting drugs in hair by TLC-SERS | |
| CN114487252A (en) | Thin-layer chromatography identification method for distinguishing antrodia camphorata and antrodia camphorata wood | |
| CN108956843A (en) | A kind of quick multi information thin-layer identification method of banxia baizhu tianma decoction freeze-dried powder | |
| CN112730724B (en) | Thin-layer identification method for cynanchum glaucescens formula granules | |
| CN112697743A (en) | Method for identifying pterocarpus santalinus pen container based on two-dimensional correlation infrared spectrum | |
| CN108627606B (en) | Thin layer identification method of pogostemon cablin | |
| CN112697950A (en) | Thin-layer chromatography identification method of pyrrosia lingua | |
| CN113341005A (en) | Method for detecting aflatoxin-producing fungal contamination by GC-IMS and fluorescence spectroscopy | |
| CN114720621A (en) | Thin-layer chromatographic analysis method for distinguishing fermented cordyceps sinensis powder from fermented cordyceps sinensis powder | |
| CN109374698A (en) | A method of based on the 2.5D electrochemistry fingerprint identification fleece-flower root or RADIX POLYGONI MULTIFLORI PREPARATA | |
| CN106526059B (en) | A kind of method of thin-layer chromatography coupling infrared technique analysis tobacco pollutant | |
| CN109541116A (en) | A kind of discrimination method of agalloch eaglewood | |
| CN110426486A (en) | The discrimination method of Zhejiang Radix Ophiopogonis in Chinese materia medica preparation | |
| CN116818976A (en) | Thin layer chromatography identification method for identifying and distinguishing cherries and acerola cherries | |
| CN101419189B (en) | HPCE fingerprint identification method for origin ginseng protection | |
| CN117233313A (en) | Thin layer chromatography method for distinguishing semen astragali Complanati medicinal materials and preparations thereof | |
| CN113252835B (en) | Thin-layer chromatography identification method of Yanhuweian capsules | |
| CN117491550A (en) | Method for identifying effective components in Tiantian capsules | |
| CN111024881B (en) | Rapid double-information thin-layer identification method for thesium Chinese medicinal materials, granules and target decoction dry powder | |
| CN115166129A (en) | Thin-layer chromatography detection method for angelica sinensis in Naoan dropping pills | |
| CN112649393A (en) | Infrared spectrum-based method for identifying small ornament of dalbergia odorifera |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |