CN114487252B - Thin-layer chromatography identification method for distinguishing Antrodia camphorata from Antrodia camphorata - Google Patents
Thin-layer chromatography identification method for distinguishing Antrodia camphorata from Antrodia camphorata Download PDFInfo
- Publication number
- CN114487252B CN114487252B CN202111629081.8A CN202111629081A CN114487252B CN 114487252 B CN114487252 B CN 114487252B CN 202111629081 A CN202111629081 A CN 202111629081A CN 114487252 B CN114487252 B CN 114487252B
- Authority
- CN
- China
- Prior art keywords
- thin layer
- antrodia
- antrodia camphorata
- silica gel
- layer plate
- 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.)
- Active
Links
- 241001486992 Taiwanofungus camphoratus Species 0.000 title claims abstract description 109
- 238000000034 method Methods 0.000 title claims abstract description 25
- 238000004809 thin layer chromatography Methods 0.000 title claims abstract description 25
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 85
- 239000002994 raw material Substances 0.000 claims description 65
- 239000003795 chemical substances by application Substances 0.000 claims description 55
- 241000123370 Antrodia Species 0.000 claims description 46
- 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
- 238000003892 spreading Methods 0.000 claims description 35
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims description 30
- 238000007689 inspection Methods 0.000 claims description 26
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 20
- 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 17
- 244000082946 Tarchonanthus camphoratus Species 0.000 claims description 17
- 235000005701 Tarchonanthus camphoratus Nutrition 0.000 claims description 17
- 239000003153 chemical reaction reagent Substances 0.000 claims description 17
- 239000007788 liquid Substances 0.000 claims description 17
- 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 15
- 238000001816 cooling Methods 0.000 claims description 12
- 238000005286 illumination Methods 0.000 claims description 12
- 238000005507 spraying Methods 0.000 claims description 11
- 238000001035 drying Methods 0.000 claims description 10
- 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 9
- 238000010438 heat treatment Methods 0.000 claims description 9
- 239000012528 membrane Substances 0.000 claims description 9
- 238000002137 ultrasound extraction Methods 0.000 claims description 9
- 238000007873 sieving Methods 0.000 claims description 8
- 239000012530 fluid Substances 0.000 claims description 7
- 238000000079 presaturation Methods 0.000 claims description 7
- 238000007789 sealing Methods 0.000 claims description 7
- 239000000047 product Substances 0.000 claims 2
- 238000002156 mixing Methods 0.000 claims 1
- 238000004458 analytical method Methods 0.000 abstract description 4
- 238000001514 detection method Methods 0.000 abstract description 4
- 238000011160 research Methods 0.000 abstract description 4
- 230000000007 visual effect Effects 0.000 abstract description 4
- 238000001228 spectrum Methods 0.000 abstract description 3
- 239000007791 liquid phase Substances 0.000 abstract description 2
- 239000000523 sample Substances 0.000 abstract 1
- 239000012488 sample solution Substances 0.000 abstract 1
- 239000000463 material Substances 0.000 description 8
- 239000003086 colorant Substances 0.000 description 4
- 238000005485 electric heating Methods 0.000 description 4
- 239000003814 drug Substances 0.000 description 2
- 230000000694 effects Effects 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
- KIWBPDUYBMNFTB-UHFFFAOYSA-N Ethyl hydrogen sulfate Chemical compound CCOS(O)(=O)=O KIWBPDUYBMNFTB-UHFFFAOYSA-N 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
- 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
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 from Antrodia camphorata. Solves the technical problems that the existing liquid phase fingerprint identification research method for Antrodia camphorata has single spectrum and complex operation, and can not intuitively distinguish Antrodia camphorata from Antrodia camphorata. 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) color development and identification. The thin-layer chromatography identification method has the advantages of rapidness, low cost, simplicity, high efficiency, strong specificity, visual detection result, easy identification and the like, can rapidly identify and distinguish Antrodia camphorata and Antrodia camphorata, 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 is not performed 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 from Antrodia camphorata.
Background
Antrodia camphorata (Antrodiacamphora) is also known as Antrodia camphorata, and is usually rotten in the trunk cavity of an over hundred years Antrodia camphorata tree. Antrodia camphorata is the only host of Antrodia camphorata, and the area suitable for growing is very limited, so that wild Antrodia camphorata resources are scarce. Antrodia camphorata is a very 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 itch and the like. Antrodia camphorate is used as a traditional Chinese medicine in Taiwan for a long time and becomes a hot spot in the last ten years. Therefore, antrodia camphorate is called "King in medicine", "forest ruby". Wild Antrodia camphorata is increasingly rare in number due to the excessive harvest of the Antrodia camphorata, and Taiwan has listed the Antrodia camphorata as a protective tree species. The market price of Antrodia camphorate reaches hundreds of thousands or even hundreds of thousands per kilogram, and the market prospect is huge. Due to the uniqueness, rarity and magic efficacy of Antrodia camphorata, a large amount of inferior and even counterfeit Antrodia camphorata medicinal materials appear on the market. The camphorwood is a host for growing camphorwood, so that the phenomenon of replacing camphorwood by camphorwood also appears in the market, and the quality reputation of camphorwood is seriously affected.
Related researchers use high performance liquid chromatography to study the fingerprint of Antrodia camphorata, but the liquid fingerprint is influenced by factors such as single spectrum, complex operation and the like, so that the quality of Antrodia camphorata cannot be well reflected, and simultaneously, the Antrodia camphorata and the Antrodia camphorata cannot be intuitively distinguished.
Disclosure of Invention
The invention aims to solve the technical problems that the existing liquid phase fingerprint identification research method for Antrodia camphorata has single spectrum and complex operation, can not well reflect the quality of Antrodia camphorata and can not intuitively distinguish Antrodia camphorata from Antrodia camphorata, and provides a thin layer chromatography identification method for distinguishing Antrodia camphorata from Antrodia camphorata. The thin layer chromatography has the advantages of high separation effect, fast identification, high sensitivity, low cost, visual pattern and the like, and is widely applied to the production process of Chinese medicinal materials. However, there is no report of thin layer chromatography for distinguishing Antrodia camphorata from Antrodia camphorata.
The technical scheme of the invention is as follows:
the thin-layer chromatography identification method for distinguishing Antrodia camphorata from Antrodia camphorata is characterized by comprising the following steps of:
1) Preparation of sample fluid
Taking Antrodia raw material and Antrodia raw material, crushing, sieving, respectively placing into a sealable test container, respectively adding 6-10 times of ethanol with the mass concentration of 70% -100% into the Antrodia raw material and the Antrodia raw material, performing ultrasonic extraction for 30-60 minutes, cooling to room temperature, filtering by adopting a microporous filter membrane, and collecting filtrate as sample liquid;
2) Carrying out thin layer sample application
Sequentially spotting 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 spotting origins;
3) Preparation of the developing agent
3.1 Toluene, ethyl acetate and formic acid are uniformly mixed according to the volume ratio of 6-10:4-6:0.6-1.0 to obtain a developing agent;
3.2 Placing the developing agent into a developing cylinder, sealing the developing cylinder, and presaturating for 15-20 minutes;
4) Unfolding
4.1 Opening the spreading cylinder after the presaturation in the step 3), and rapidly placing the silica gel G thin layer plate after the sample application in the step 2) into the spreading cylinder, so that the silica gel G thin layer plate leans against the spreading cylinder and the spreading agent in the spreading cylinder cannot overflow the sample application origin position;
4.2 When the front edge of the developing agent moves up to 6 cm-10 cm away from the spotting origin, taking out the silica gel G thin layer plate;
5) Color development and identification
After the reagent on the unfolded silica gel G thin layer plate in the step 4.2) is dried, inspecting under illumination to obtain an inspection view; the Antrodia camphorata raw material has a plurality of spots which are obviously displayed, and the plurality of spots are not obvious or are not displayed.
Further, the step 5) specifically comprises: drying the reagent on the unfolded silica gel G thin layer plate in the step 4.2), spraying 5-10% sulfuric acid ethanol solution to the silica gel G thin layer plate, heating at 100-110 ℃ for 3-5 minutes, and after the silica gel G thin layer plate is cooled to room temperature, inspecting under 365nm ultraviolet light to obtain an inspection view; the inspection images show that spots are respectively arranged 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 the spots are obvious as Antrodia camphorata raw materials; spots were found at each of rf=0.58 to 0.62 and rf=0.65 to 0.70 and showed no apparent material of camphorwood.
Further, the step 5) specifically comprises: drying the reagent on the unfolded silica gel G thin layer plate in the step 4.2), spraying 5-10% sulfuric acid ethanol solution to the silica gel G thin layer plate, heating at 100-110 ℃ for 3-5 minutes, and after the silica gel G thin layer plate is cooled to room temperature, inspecting the silica gel G thin layer plate under white light illumination to obtain an inspection view; spots are respectively arranged 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 the spots are obvious as Antrodia camphorata raw materials; spots were found at each of rf=0.23 to 0.28 and rf=0.36 to 0.41 and showed no apparent material of camphorwood.
Further, the step 5) specifically comprises: drying the reagent on the unfolded silica gel G thin layer plate in the step 4.2), and then inspecting under 254nm ultraviolet irradiation to obtain an inspection view; spots on 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 are Antrodia raw materials; the spots are not shown as raw materials of the camphor wood.
Further, the step 1) is specifically that Antrodia raw materials and Antrodia raw materials are taken, crushed and then are sieved by a 80-mesh sieve, and are respectively placed in triangular flasks with plugs, ethanol with the mass of 8-10 times and the mass concentration of 70% of the Antrodia raw materials and the Antrodia raw materials is respectively added, ultrasonic extraction is carried out for 60 minutes, the temperature is lowered to the room temperature, then microporous filter membranes are adopted for filtration, and filtrate is collected as sample liquid.
Further, in the step 2), the distance between the point origin position of the sample 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-tank developing cylinder having a size of 10×10cm, 20×10cm or 10×20cm, and the amount of developing agent in the double tank is kept uniform and presaturated for 15 minutes.
Further, step 4.2) is specifically to take out the silica gel G thin layer plate when the front edge of the developing agent is up to 8 cm-10 cm from the spotting origin.
Further, in the step 5), the mass ratio concentration of the sulfuric acid ethanol solution is 10%.
The invention has the beneficial effects that:
1. the invention provides a thin layer identification method which is quick, low in cost, simple, convenient, efficient, strong in specificity, visual in detection result and easy to identify, and can solve the identification and distinguishing problems of Antrodia camphorata and Antrodia camphorata.
2. The thin layer identification method provided by the invention has obvious distinction and easy identification, and can be used for distinguishing Antrodia camphorata from Antrodia camphorata under 254nm, 365nm and sunlight.
3. The invention selects proper amount of ethanol to directly carry out ultrasonic treatment on the raw medicinal materials, filters the raw medicinal materials, takes filtrate as detection solution, has simple sample pretreatment, low cost and easy 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, so that the developing agent is obtained, the spot separation effect is good, the characteristic spots of each sample are outstanding, the spot tailing and the spot diffusion phenomenon are avoided, the result comparison is obvious, and the judgment is easy.
Drawings
FIG. 1 is a view of a silica gel G thin layer plate under 254nm light after being developed in an embodiment of the present invention;
FIG. 2 is a view of a silica gel G thin layer plate after spraying a developer in the embodiment of the invention under 365nm light;
FIG. 3 is a view of a silica gel G thin layer plate after the color developer is sprayed in the embodiment of the invention under the illumination of white light.
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings and specific embodiments.
Example 1
1) Preparation of sample fluid
Taking Antrodia raw material and Antrodia raw material, crushing, sieving with an 80-mesh sieve, respectively placing into triangular flasks with plugs, respectively adding ethanol with the mass of 6 times and the mass concentration of 70% into the Antrodia raw material and the Antrodia raw material, carrying out ultrasonic extraction for 60 minutes, cooling to room temperature, filtering by adopting a microporous filter membrane, and collecting filtrate as a sample liquid. In order to ensure accurate results, two samples of Antrodia camphorata and Antrodia camphorata are prepared respectively, and the numbers of the samples of Antrodia camphorata and Antrodia camphorata are marked as number 1 and number 2 respectively;
2) Carrying out thin layer sample application
Sequentially spotting 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 spotting origins; the distance between the sample application origin and the lower edge of the silica gel G thin layer plate is 1.0cm;
3) Preparation of the developing agent
3.1 Toluene, ethyl acetate and formic acid were mixed uniformly in a volume ratio of 8:5:0.8 to prepare 20mL of developing agent, where toluene, ethyl acetate and formic acid were all pure.
3.2 Placing the developing agent into a 10X 10cm double-groove developing cylinder, enabling the quantity of the developing agent in the two grooves to be consistent, then sealing the developing cylinder, and presaturating for 15 minutes;
4) Unfolding
4.1 Opening the spreading cylinder after the presaturation in the step 3), and rapidly placing the silica gel G thin layer plate after the sample application in the step 2) into the spreading cylinder, so that the silica gel G thin layer plate leans against the spreading cylinder and the spreading agent in the spreading cylinder cannot overflow the sample application origin position;
4.2 When the developing agent is developed along the upper line of the thin-layer plate and the front edge of the developing agent is up to 8cm away from the point of origin of the sample application, the silica gel G thin-layer plate is taken out;
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 firstly inspecting under 254nm illumination to obtain an inspection view of FIG. 1;
spraying 10% sulfuric acid ethanol solution on the silica gel G thin layer plate, placing the silica gel G thin layer plate on an electric heating plate, heating at 105 ℃ for 4 minutes, and after the silica gel G thin layer plate is cooled to room temperature, respectively inspecting the silica gel G thin layer plate under 365nm ultraviolet light and white light illumination to respectively obtain the inspection views of fig. 2 and 3.
As shown in fig. 1, before the developer is sprayed, under 254nm violet light, there are 1 black fluorescent spots on each of 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, corresponding to the positions of the two spots numbered 1 on the silica gel G thin layer plate, and 6 spots are the raw materials of antrodia camphorata. And at the two sample points with the corresponding number of 2, the spots are not obvious or almost no spots are displayed, and the corresponding sample is the raw material of the camphorwood.
As shown in fig. 2, after the color-developing agent is sprayed, under 365nm violet light, 1 spot is formed on each spot 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 8 spots with different colors are formed on the silica gel G thin layer plate, so that the corresponding sample is the antrodia raw material. And at two spotting points with the corresponding number of 2, 1 blurred spot is respectively arranged at Rf=0.58-0.62 and Rf=0.65-0.70, and the rest spots are not obvious or almost have no spots, so that the corresponding sample is the raw material of the camphorwood.
As shown in fig. 3, after the color developer is sprayed, at two spots corresponding to the number 1 on the silica gel G thin layer plate under white light illumination, 1 spot is respectively formed at the positions 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 spots are spots with brown colors of 6 different shades, and the corresponding sample is Antrodia camphorata raw material. At two spots corresponding to the number 2, 1 yellowish spot is respectively arranged at Rf=0.23-0.28 and Rf=0.36-0.41, and the spots are not obvious, and the rest spots are weak or almost no spots, so that the corresponding sample is the raw material of the camphorwood.
Before the color development agent is sprayed, the obtained inspection image is inspected under 254nm purple light illumination, and after the color development agent is sprayed, the obtained inspection image is inspected under 365nm purple light and white light illumination, and the Antrodia raw material can be distinguished obviously, but the situation that the color development agent is not sprayed possibly has incomplete display or fuzzy display so that the result is inaccurate is considered, so that the analysis and comparison are carried out by combining the inspection image after the color development agent is sprayed so that the result is more accurate. In addition, in order to make the result more accurate and reliable, in this embodiment, after spraying the developer, the chromatograph inspection of 365nm violet light and white light is performed respectively, and the inspection images are mutually verified, so as to ensure the accuracy and reliability of the result.
Example two
1) Preparation of sample fluid
Taking Antrodia raw material and Antrodia raw material, crushing, sieving with an 80-mesh sieve, respectively placing into triangular flasks with plugs, respectively adding ethanol with the mass of 8 times and the mass concentration of 100% into the Antrodia raw material and the Antrodia raw material, performing ultrasonic extraction for 60 minutes, cooling to room temperature, filtering with a microporous filter membrane, and collecting filtrate as sample liquid. In order to ensure accurate results, two samples of Antrodia camphorata and Antrodia camphorata are prepared respectively, and the numbers of the samples of Antrodia camphorata and Antrodia camphorata are marked as number 1 and number 2 respectively;
2) Carrying out thin layer sample application
Sequentially spotting 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 spotting origins; the distance between the sample application origin and the lower edge of the silica gel G thin layer plate is 1.3cm;
3) Preparation of the developing agent
3.1 Toluene, ethyl acetate and formic acid were mixed uniformly in a volume ratio of 10:6:1.0 to prepare 20mL of developing agent, where toluene, ethyl acetate and formic acid were all pure.
3.2 Placing the developing agent into a 10X 10cm double-groove developing cylinder, enabling the quantity of the developing agent in the two grooves to be consistent, then sealing the developing cylinder, and presaturating for 20 minutes;
4) Unfolding
4.1 Opening the spreading cylinder after the presaturation in the step 3), and rapidly placing the silica gel G thin layer plate after the sample application in the step 2) into the spreading cylinder, so that the silica gel G thin layer plate leans against the spreading cylinder and the spreading agent in the spreading cylinder cannot overflow the sample application origin position;
4.2 When the developing agent is developed up along the thin-layer plate and the front edge of the developing agent is up to 6cm away from the spotting origin, the silica gel G thin-layer plate is taken out;
5) Color development and identification
After the reagent on the silica gel G thin layer plate developed in the step 4) is dried by a blower, the reagent is inspected under 254nm light, and the inspection view is similar to that of FIG. 1.
Example III
1) Preparation of sample fluid
Taking Antrodia raw material and Antrodia raw material, crushing, sieving with an 80-mesh sieve, respectively placing into triangular flasks with plugs, respectively adding ethanol with the mass of 6 times and the mass concentration of 90% into the Antrodia raw material and the Antrodia raw material, carrying out ultrasonic extraction for 30 minutes, cooling to room temperature, filtering by adopting a microporous filter membrane, and collecting filtrate as sample liquid. In order to ensure accurate results, two samples of Antrodia camphorata and Antrodia camphorata are prepared respectively, and the numbers of the samples of Antrodia camphorata and Antrodia camphorata are marked as number 1 and number 2 respectively;
2) Carrying out thin layer sample application
Sequentially spotting 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 spotting origins; the distance between the sample application origin and the lower edge of the silica gel G thin layer plate is 1.5cm;
3) Preparation of the developing agent
3.1 Toluene, ethyl acetate and formic acid were mixed uniformly in a volume ratio of 8:4:0.7 to prepare 20mL of developing agent, where toluene, ethyl acetate and formic acid were all pure.
3.2 Placing the developing agent into a 10X 10cm double-groove developing cylinder, enabling the quantity of the developing agent in the two grooves to be consistent, then sealing the developing cylinder, and presaturating for 17 minutes;
4) Unfolding
4.1 Opening the spreading cylinder after the presaturation in the step 3), and rapidly placing the silica gel G thin layer plate after the sample application in the step 2) into the spreading cylinder, so that the silica gel G thin layer plate leans against the spreading cylinder and the spreading agent in the spreading cylinder cannot overflow the sample application origin position;
4.2 When the developing agent is developed up along the thin-layer plate and the front edge of the developing agent is up to 10cm away from the spotting origin, the silica gel G thin-layer plate is taken out;
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 5% sulfuric acid ethanol solution with the mass ratio concentration on the silica gel G thin layer plate, placing the silica gel G thin layer plate on an electric heating plate, heating at 100 ℃ for 5 minutes, cooling to room temperature, and inspecting the silica gel G thin layer plate under 365nm ultraviolet light to obtain an inspection view which is consistent with that of FIG. 2.
Example IV
1) Preparation of sample fluid
Taking Antrodia raw material and Antrodia raw material, crushing, sieving with a 80-mesh sieve, respectively placing into triangular bottles with plugs, respectively adding 10 times of ethanol with the mass concentration of the Antrodia raw material and the Antrodia raw material, carrying out 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, two samples of Antrodia camphorata and Antrodia camphorata are prepared respectively, and the numbers of the samples of Antrodia camphorata and Antrodia camphorata are marked as number 1 and number 2 respectively;
2) Carrying out thin layer sample application
Sequentially spotting 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 spotting origins; the distance between the sample application origin and the lower edge of the silica gel G thin layer plate is 1.0cm;
3) Preparation of the developing agent
3.1 Toluene, ethyl acetate and formic acid were mixed uniformly in a volume ratio of 6:5:0.6 to prepare 20mL of developing agent, where toluene, ethyl acetate and formic acid were all pure.
3.2 Placing the developing agent into a 10X 10cm double-groove developing cylinder, enabling the quantity of the developing agent in the two grooves to be consistent, then sealing the developing cylinder, and presaturating for 15 minutes;
4) Unfolding
4.1 Opening the spreading cylinder after the presaturation in the step 3), and rapidly placing the silica gel G thin layer plate after the sample application in the step 2) into the spreading cylinder, so that the silica gel G thin layer plate leans against the spreading cylinder and the spreading agent in the spreading cylinder cannot overflow the sample application origin position;
4.2 When the developing agent is developed along the upper line of the thin-layer plate and the front edge of the developing agent is up to 8cm away from the point of origin of the sample application, the silica gel G thin-layer plate is taken out;
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 an ethanol sulfuric acid solution with the mass ratio concentration of 7% on the silica gel G thin layer plate, 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 which is consistent with that of FIG. 3.
Example five
1) Preparation of sample fluid
Taking Antrodia raw material and Antrodia raw material, crushing, sieving with an 80-mesh sieve, respectively placing into triangular flasks with plugs, respectively adding ethanol with the mass of 6 times and the mass concentration of 70% into the Antrodia raw material and the Antrodia raw material, carrying out ultrasonic extraction for 30 minutes, cooling to room temperature, filtering by adopting a microporous filter membrane, and collecting filtrate as sample liquid. In order to ensure accurate results, two samples of Antrodia camphorata and Antrodia camphorata are prepared respectively, and the numbers of the samples of Antrodia camphorata and Antrodia camphorata are marked as number 1 and number 2 respectively;
2) Carrying out thin layer sample application
Sequentially spotting 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 spotting origins; the distance between the sample application origin and the lower edge of the silica gel G thin layer plate is 1.5cm;
3) Preparation of the developing agent
3.1 Toluene, ethyl acetate and formic acid were mixed uniformly in a volume ratio of 6:4:0.6 to prepare 20mL of developing agent, where toluene, ethyl acetate and formic acid were all pure.
3.2 Placing the developing agent into a 10X 10cm double-groove developing cylinder, enabling the quantity of the developing agent in the two grooves to be consistent, then sealing the developing cylinder, and presaturating for 20 minutes;
4) Unfolding
4.1 Opening the spreading cylinder after the presaturation in the step 3), and rapidly placing the silica gel G thin layer plate after the sample application in the step 2) into the spreading cylinder, so that the silica gel G thin layer plate leans against the spreading cylinder and the spreading agent in the spreading cylinder cannot overflow the sample application origin position;
4.2 When the developing agent is developed up along the thin-layer plate and the front edge of the developing agent is up to 6cm away from the spotting origin, the silica gel G thin-layer plate is taken out;
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 an ethanol sulfate solution with the mass ratio concentration of 10% on the silica gel G thin layer plate, placing the silica gel G thin layer plate on an electric heating plate, heating at 105 ℃ for 5 minutes, cooling to room temperature, and respectively inspecting the silica gel G thin layer plate under 365nm ultraviolet light and white light to obtain inspection views respectively, wherein the obtained inspection views are similar to those in fig. 2 and 3 respectively.
The inspection images obtained in the second to fifth embodiments correspond to the inspection images obtained in the first reference embodiment, and the experimental result analysis shows that before the developer is sprayed, fluorescent spots on the silica gel G thin layer plate corresponding to the sample points with the number 1 are Antrodia raw materials at the positions of Rf=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 and Rf=0.65 to 0.70 under 254nm illumination. And at two spotting points corresponding to the number 2, spots are not obvious or almost no spots are the raw materials of the camphorwood. After the color reagent is sprayed, spots are respectively formed at 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 on two spots corresponding to the number 1 on the silica gel G thin layer plate under 365nm purple light irradiation, and spots with different colors are formed by Antrodia camphorata raw materials. And at two spots corresponding to the number 2, blurred spots are respectively arranged at Rf=0.58-0.62 and Rf=0.65-0.70, and the rest spots are not obvious or almost no spots, so that the material is the camphor wood raw material. After the color reagent is sprayed, spots are respectively arranged at 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 on two sample points corresponding to the number 1 on the silica gel G thin layer plate under white light illumination, and spots with brown colors with different depths are Antrodia camphorata raw materials. At two spots corresponding to the number 2, there are yellowish spots at the positions rf=0.23-0.28 and rf=0.36-0.41, and the spots are not obvious, and the rest spots are weak or almost no spots, so that the material is the raw material of the camphorwood.
The invention provides a thin-layer chromatography identification method of Antrodia camphorata and Antrodia camphorata, and obtains a thin-layer chromatography inspection view of Antrodia camphorata and Antrodia camphorata, and in practical application, samples to be identified or distinguished can be compared with the inspection view obtained by the method, namely, antrodia camphorata and Antrodia camphorata can be distinguished, or whether the samples are real Antrodia camphorata or real Antrodia camphorata can be identified.
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 easiness in identification, and can be used for obviously distinguishing Antrodia camphorata from Antrodia camphorata under 254nm, 365nm and white light.
Claims (10)
1. A thin layer chromatography identification method for distinguishing antrodia camphorata from antrodia camphorata, which is characterized by comprising the following steps:
1) Preparation of sample fluid
Taking Antrodia raw material and Antrodia raw material, crushing, sieving, respectively placing in a sealable test container, respectively adding 6-10 times of ethanol with the mass concentration of 70% -100% into the Antrodia raw material and the Antrodia raw material, performing ultrasonic extraction for 30-60 minutes, cooling to room temperature, filtering by adopting a microporous filter membrane, and collecting filtrate as sample liquid;
2) Carrying out thin layer sample application
Sequentially spotting 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 spotting origins;
3) Preparation of the 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 a developing cylinder, sealing the developing cylinder, and presaturating for 15-20 minutes;
4) Unfolding
4.1 Opening the spreading cylinder after the presaturation in the step 3), and rapidly placing the silica gel G thin layer plate after the sample application in the step 2) into the spreading cylinder, so that the silica gel G thin layer plate leans against the spreading cylinder and the spreading agent in the spreading cylinder cannot overflow the sample application origin position;
4.2 When the front edge of the developing agent is up to 6 cm-10 cm away from the spotting origin, taking out the silica gel G thin layer plate;
5) Color development and identification
After the reagent on the unfolded silica gel G thin layer plate in the step 4.2) is dried, directly inspecting under 254nm ultraviolet irradiation to obtain an inspection view; or after the reagent on the unfolded silica gel G thin layer plate in the step 4.2) is dried, spraying 5% -10% sulfuric acid ethanol solution with mass ratio concentration to the silica gel G thin layer plate, heating at 100-110 ℃ for 3-5 minutes, and after the silica gel G thin layer plate is cooled to room temperature, inspecting the silica gel G thin layer plate under the illumination of white light or 365nm ultraviolet light to obtain an inspection view;
in the view, a plurality of spots are displayed obviously, namely the Antrodia raw material, and the spots are displayed unobviously or are not displayed.
2. The thin layer chromatography identification method for distinguishing Antrodia camphorata from Antrodia camphorata according to claim 1, wherein the step 5) specifically comprises: drying the reagent on the unfolded silica gel G thin layer plate in the step 4.2), spraying 5-10% sulfuric acid ethanol solution to the silica gel G thin layer plate, heating at 100-110 ℃ for 3-5 minutes, cooling to room temperature, and inspecting the silica gel G thin layer plate under 365nm ultraviolet light to obtain an inspection view; spots are formed 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 the spots are obvious as Antrodia camphorata raw materials; spots are formed at the positions of Rf=0.58-0.62 and Rf=0.65-0.70, and the spots are not obvious to be the raw materials of the camphorwood.
3. The thin layer chromatography identification method for distinguishing Antrodia camphorata from Antrodia camphorata according to claim 1, wherein the step 5) specifically comprises: drying the reagent on the unfolded silica gel G thin layer plate in the step 4.2), spraying 5-10% sulfuric acid ethanol solution to the silica gel G thin layer plate, heating at 100-110 ℃ for 3-5 minutes, and after cooling to room temperature, inspecting the silica gel G thin layer plate under white light to obtain an inspection view; spots are formed 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 the spots are obvious as Antrodia camphorata raw materials; spots are formed at the positions of Rf=0.23-0.28 and Rf=0.36-0.41, and the spots are not obvious to be the raw materials of the camphorwood.
4. The thin layer chromatography identification method for distinguishing Antrodia camphorata from Antrodia camphorata according to claim 1, wherein the step 5) specifically comprises: drying the reagent on the unfolded silica gel G thin layer plate in the step 4.2), and then inspecting under 254nm ultraviolet irradiation to obtain an inspection view; spots are formed 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, respectively, and are Antrodia raw materials; the spots are not shown as raw materials of the camphor wood.
5. A thin layer chromatography identification method for distinguishing antrodia camphorata from antrodia camphorate according to any one of claims 1 to 4, wherein:
the preparation method comprises the steps of 1) taking Antrodia raw materials and Antrodia raw materials, crushing the Antrodia raw materials, sieving the crushed Antrodia raw materials with a 80-mesh sieve, respectively placing the crushed Antrodia raw materials and the Antrodia raw materials into triangular flasks with plugs, respectively adding ethanol with the mass of 8-10 times and the mass concentration of 70% into the Antrodia raw materials and the Antrodia raw materials, carrying out ultrasonic extraction for 60 minutes, standing the obtained products to the room temperature, filtering the obtained products by adopting a microporous filter membrane, and collecting filtrate as sample liquid.
6. The thin layer chromatography identification method for distinguishing Antrodia camphorata from Antrodia camphorata according to claim 5, wherein:
in the step 2), the distance between the point origin position and the lower edge of the silica gel G thin layer plate is 1.0-1.5 cm.
7. The thin-layer chromatography identification method for distinguishing Antrodia camphorata from Antrodia camphorata according to claim 6, wherein:
in step 3.1), the volume ratio of toluene, ethyl acetate and formic acid was 8:5:0.8.
8. The thin layer chromatography identification method for distinguishing Antrodia camphorata from Antrodia camphorata according to claim 7, wherein:
in step 3.2), the deployment cylinder is a double-tank deployment cylinder, the size of the double-tank deployment cylinder is 10×10cm, 20×10cm or 10×20cm, and the doses of the deployment agent in the double tanks are kept consistent and presaturated for 15 minutes.
9. The thin layer chromatography identification method for distinguishing 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 cm-10 cm away from the spotting origin.
10. A thin layer chromatography identification method for distinguishing antrodia camphorate from antrodia camphorate 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 CN114487252A (en) | 2022-05-13 |
| CN114487252B true 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 |
|---|
| Mushroom extracts and compounds with suppressive action on breast cancer: evidence from studies using cultured cancer cells, tumor-bearing animals, and clinical trials;Wong Jack Ho等;《 Applied microbiology and biotechnology》;20201231;第104卷;第1-29页 * |
| UPLC法同时测定牛樟芝子实体中7个三萜类成分的含量;李沁等;《药物分析杂志》;20210930;第41卷(第09期);第1576-1582页 * |
| 皿培式牛樟芝化学成分及质量控制和活性研究;吴雨;《中国优秀硕士论文电子期刊网》;20190715(第07期);第79-89页 * |
| 薄层色谱-分光光度法测定樟芝菌粉中的总三萜含量;张寅等;《天然产物研究与开发》;20101231;第22卷(第04期);第639-642页 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN114487252A (en) | 2022-05-13 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN108008026B (en) | Method for synchronously detecting 13 colorants in hawthorn pills | |
| CN106198832B (en) | A kind of quality of production control method of intensified loquet distillate | |
| CN114487252B (en) | Thin-layer chromatography identification method for distinguishing Antrodia camphorata from Antrodia camphorata | |
| CN110632236B (en) | Method for rapidly identifying three active ingredients of folium cortex eucommiae and cortex eucommiae by thin-layer chromatography | |
| CN106483210B (en) | A kind of detection method of red ganoderma medicinal material | |
| CN101422596B (en) | Preserved snake gall orange peel oral liquid and quality control method thereof | |
| CN101658546B (en) | TLC identification method for Naoxinqing tablet and persimmon leaf extract | |
| CN108956843A (en) | A kind of quick multi information thin-layer identification method of banxia baizhu tianma decoction freeze-dried powder | |
| CN109085284A (en) | A kind of quick thin-layer identification method of multiple medicine taste of Ershiwuwei zhenzhu wan | |
| CN108627606B (en) | Thin layer identification method of pogostemon cablin | |
| CN114720621B (en) | Thin-layer chromatographic analysis method for distinguishing fermented cordyceps sinensis bacterial powder from fermented cordyceps sinensis bacterial powder | |
| CN112697950A (en) | Thin-layer chromatography identification method of pyrrosia lingua | |
| CN112730724A (en) | Thin-layer identification method for cynanchum glaucescens formula granules | |
| CN111638300B (en) | Thin-layer identification method for 16-oxo-alisol A in alisma orientale | |
| CN117233313A (en) | Thin layer chromatography method for distinguishing semen astragali Complanati medicinal materials and preparations thereof | |
| CN109374698A (en) | A method of based on the 2.5D electrochemistry fingerprint identification fleece-flower root or RADIX POLYGONI MULTIFLORI PREPARATA | |
| CN109444319B (en) | Method for determining astragaloside content in Astragalus membranaceus mushroom | |
| CN110426486A (en) | The discrimination method of Zhejiang Radix Ophiopogonis in Chinese materia medica preparation | |
| CN115586290A (en) | Method for rapidly identifying dioscorea zingiberensis diosgenin and dioscorea mexicana saponin | |
| CN104713979A (en) | Thin-layer identification method for Dendrobium officinale | |
| CN107290473A (en) | A kind of thin-layer identification method of Yam dispensing granule and Rhizoma Dioscoreae (parched with bran) granule | |
| CN108562684A (en) | The identification method of cornu caprae hircus | |
| CN114414723B (en) | Thin-layer full-medicine taste identification method for Xinkeshu tablets | |
| CN113252835B (en) | Thin-layer chromatography identification method of Yanhuweian capsules | |
| CN114217004B (en) | Windproof detection method based on thin-layer chromatography |
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 |