CN113624887A - Method for measuring content of cantharidin - Google Patents
Method for measuring content of cantharidin Download PDFInfo
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- CN113624887A CN113624887A CN202110959774.7A CN202110959774A CN113624887A CN 113624887 A CN113624887 A CN 113624887A CN 202110959774 A CN202110959774 A CN 202110959774A CN 113624887 A CN113624887 A CN 113624887A
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- DHZBEENLJMYSHQ-XCVPVQRUSA-N cantharidin Chemical compound C([C@@H]1O2)C[C@@H]2[C@]2(C)[C@@]1(C)C(=O)OC2=O DHZBEENLJMYSHQ-XCVPVQRUSA-N 0.000 title claims abstract description 59
- 229940095758 cantharidin Drugs 0.000 title claims abstract description 59
- 229930008397 cantharidin Natural products 0.000 title claims abstract description 59
- DHZBEENLJMYSHQ-UHFFFAOYSA-N cantharidine Natural products O1C2CCC1C1(C)C2(C)C(=O)OC1=O DHZBEENLJMYSHQ-UHFFFAOYSA-N 0.000 title claims abstract description 59
- 238000000034 method Methods 0.000 title claims abstract description 18
- 239000000243 solution Substances 0.000 claims abstract description 26
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims abstract description 24
- 241000131283 Cantharis Species 0.000 claims abstract description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000012088 reference solution Substances 0.000 claims abstract description 16
- 239000012085 test solution Substances 0.000 claims abstract description 16
- 239000000843 powder Substances 0.000 claims abstract description 14
- 238000002137 ultrasound extraction Methods 0.000 claims abstract description 13
- 238000002156 mixing Methods 0.000 claims abstract description 12
- 238000004811 liquid chromatography Methods 0.000 claims abstract description 5
- 238000010298 pulverizing process Methods 0.000 claims abstract description 5
- 238000004587 chromatography analysis Methods 0.000 claims abstract description 3
- 238000005259 measurement Methods 0.000 claims abstract description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 48
- 239000007788 liquid Substances 0.000 claims description 22
- 239000000523 sample Substances 0.000 claims description 14
- 239000013558 reference substance Substances 0.000 claims description 12
- 238000005303 weighing Methods 0.000 claims description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 6
- 239000012490 blank solution Substances 0.000 claims description 6
- 238000007813 chromatographic assay Methods 0.000 claims description 6
- 238000007865 diluting Methods 0.000 claims description 6
- 238000010790 dilution Methods 0.000 claims description 6
- 239000012895 dilution Substances 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 6
- 239000012488 sample solution Substances 0.000 claims description 6
- 238000001514 detection method Methods 0.000 claims description 5
- GBMDVOWEEQVZKZ-UHFFFAOYSA-N methanol;hydrate Chemical compound O.OC GBMDVOWEEQVZKZ-UHFFFAOYSA-N 0.000 claims description 4
- 238000002360 preparation method Methods 0.000 claims description 4
- 239000000945 filler Substances 0.000 claims description 3
- 239000000706 filtrate Substances 0.000 claims description 3
- 238000002347 injection Methods 0.000 claims description 3
- 239000007924 injection Substances 0.000 claims description 3
- YTJSFYQNRXLOIC-UHFFFAOYSA-N octadecylsilane Chemical compound CCCCCCCCCCCCCCCCCC[SiH3] YTJSFYQNRXLOIC-UHFFFAOYSA-N 0.000 claims description 3
- 230000010355 oscillation Effects 0.000 claims description 3
- 239000002245 particle Substances 0.000 claims description 3
- 239000000377 silicon dioxide Substances 0.000 claims description 3
- 238000000605 extraction Methods 0.000 abstract description 8
- 241000124079 Mylabris Species 0.000 abstract description 6
- 238000011084 recovery Methods 0.000 abstract description 3
- 239000012535 impurity Substances 0.000 abstract description 2
- 238000011002 quantification Methods 0.000 abstract description 2
- 239000002537 cosmetic Substances 0.000 description 5
- HEMHJVSKTPXQMS-UHFFFAOYSA-M sodium hydroxide Inorganic materials [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- 108091005804 Peptidases Proteins 0.000 description 2
- 239000004365 Protease Substances 0.000 description 2
- 102100037486 Reverse transcriptase/ribonuclease H Human genes 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 206010063409 Acarodermatitis Diseases 0.000 description 1
- 241000238631 Hexapoda Species 0.000 description 1
- 241001572617 Mylabris cichorii Species 0.000 description 1
- 241001572616 Mylabris phalerata Species 0.000 description 1
- 206010028980 Neoplasm Diseases 0.000 description 1
- 241001474977 Palla Species 0.000 description 1
- 208000003251 Pruritus Diseases 0.000 description 1
- 241000447727 Scabies Species 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
- 210000004369 blood Anatomy 0.000 description 1
- 201000011510 cancer Diseases 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000000796 flavoring agent Substances 0.000 description 1
- 235000019634 flavors Nutrition 0.000 description 1
- 230000003779 hair growth Effects 0.000 description 1
- 231100000086 high toxicity Toxicity 0.000 description 1
- 230000007803 itching Effects 0.000 description 1
- 230000003211 malignant effect Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 210000003205 muscle Anatomy 0.000 description 1
- 210000005036 nerve Anatomy 0.000 description 1
- 235000016709 nutrition Nutrition 0.000 description 1
- 230000035764 nutrition Effects 0.000 description 1
- 238000005220 pharmaceutical analysis Methods 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 239000008213 purified water Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 208000005687 scabies Diseases 0.000 description 1
- 230000004936 stimulating effect Effects 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 239000003440 toxic substance Substances 0.000 description 1
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- 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
- G01N30/02—Column chromatography
-
- 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
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
-
- 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
- G01N30/02—Column chromatography
- G01N30/50—Conditioning of the sorbent material or stationary liquid
- G01N30/52—Physical parameters
- G01N30/54—Temperature
-
- 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
- G01N30/02—Column chromatography
- G01N30/62—Detectors specially adapted therefor
- G01N30/74—Optical detectors
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- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
The invention discloses a cantharidin content determination method, which comprises the following steps: pulverizing Mylabris into 20-70 mesh Mylabris powder, adding water, mixing, performing ultrasonic extraction for several times, performing enzymolysis, adding acetone solution, performing ultrasonic extraction, recovering acetone solution to obtain cantharidin, and determining cantharidin content by liquid chromatography. The invention can greatly shorten the later extraction time after the cantharis is crushed, has high extraction content, is filtered after each extraction, has low impurity content, improves the extraction purity of the cantharidin, designs the mobile phase, the reference solution and the test solution, can accurately measure the content of the cantharidin by matching and carrying out chromatographic analysis and measurement, has simple operation, good repeatability and good recovery rate, and can realize accurate quantification of the cantharidin.
Description
Technical Field
The invention belongs to the technical field of pharmaceutical analysis, and particularly relates to a cantharidin content determination method.
Background
Mylabris, also known as Yunqing, Huaban Mao, etc., is a dried insect body of Mylabris phalerata Pallas or Mylabris cichorii Linnaeus of the family Genkwaceae, is cold in nature and pungent in flavor, and is a highly toxic traditional Chinese medicinal material. Mylabris can erode muscle, and is applied for scabies and malignant boil, and has the effects of counteracting toxic substances, removing blood stasis, resolving hard mass, and resisting tumor. Modern medical research proves that the medicinal component of the cantharis is mainly cantharidin, and is a natural active substance with special effect.
The cantharidin can be added into hair-growing cosmetics besides important clinical application such as resisting malignant tumor, and has the effects of relieving itching of skin, improving local nerve nutrition, stimulating hair root, and promoting hair growth, but due to high toxicity, the content of cantharidin in the hair-growing cosmetics is not allowed to exceed 1% and other cosmetics cannot be contained in the hair-growing cosmetics, which is specified in the requirements of cosmetic hygiene standards on raw materials. Therefore, the content of cantharidin must be strictly controlled. However, the existing cantharidin content determination method is complicated in steps and time-consuming, and the detection accuracy needs to be further improved.
Disclosure of Invention
In order to solve the technical problems in the prior art, the invention aims to provide a cantharidin content measuring method.
In order to achieve the purpose and achieve the technical effect, the invention adopts the technical scheme that:
a cantharidin content determination method comprises the following steps:
step 1), pulverizing the cantharis into 20-70 meshes of cantharis powder, adding water, uniformly mixing, carrying out ultrasonic extraction for 2-5 times, filtering, and combining filter residues;
step 2), carrying out enzymolysis, carrying out ultrasonic oscillation for not less than 6h, then adding an acetone solution, carrying out ultrasonic extraction for 30-50min, filtering, and combining filtrates;
step 3), recovering the acetone solution to obtain cantharidin;
step 4), adopting liquid chromatography to measure the cantharidin content
Step 41) mobile phase preparation
Mixing methanol and water according to the weight ratio of 20-30: mixing at 75-80 vol% to obtain mobile phase;
step 42), preparing a reference solution
Taking a certain amount of cantharidin reference substance, placing in a volumetric flask, adding methanol for dilution, and fixing the volume;
step 43), preparing test solution
Taking a certain amount of cantharidin sample obtained in the step 3), placing the cantharidin sample in a volumetric flask, adding methanol for dissolving and diluting, and fixing the volume;
step 44), chromatographic assay
Respectively injecting a certain amount of blank solution, reference solution and test solution into a liquid chromatograph, respectively recording liquid chromatogram, and analyzing and determining cantharidin content according to the liquid chromatogram.
Further, in the step 1), the cantharis is crushed into 20-40 meshes of cantharis powder, the water amount is 12-16 times of the weight of the cantharis powder each time, the cantharis powder and the water are mixed and stood for 15-25min, and then ultrasonic extraction is carried out for 2-5 times.
Further, in step 41), the volume ratio of methanol to water is 23: 77.
further, in step 42), the concentration of the reference solution is 0.6-1.4 mg/ml.
Further, in step 43), the concentration of the sample solution is 0.6-1.4 mg/ml.
Further, in step 44), the chromatographic column used in the liquid chromatograph is an Agilent C18 column, the chromatographic column has a length of 250mm, an inner diameter of 4.6mm and a particle size of 5 μm, and octadecylsilane chemically bonded silica is used as a filler.
Further, in step 44), the conditions of the chromatographic assay are as follows:
the mobile phase in the chromatographic column is methanol-water solution, the flow rate is 1.0ml/min, the detection wavelength is 230nm, the temperature of the chromatographic column is 25 ℃, and the sample injection amount is 5 mul.
Further, in step 44), the cantharidin content is calculated according to the following formula:
wherein:
Afor supplying to: peak area of the test solution;
Ato pair: peak area of the control solution;
Wfor supplying to: weighing the sample, g;
Wto pair: weighing a reference substance, and g;
Vto pair: dilution times of reference solutions;
Vfor supplying to: diluting the sample solution by multiple times;
p: and (5) marking the reference substance.
Compared with the prior art, the invention has the beneficial effects that:
the invention discloses a cantharidin content determination method, which comprises the following steps: pulverizing Mylabris into 20-70 mesh Mylabris powder, adding water, mixing, performing ultrasonic extraction for several times, performing enzymolysis, adding acetone solution, performing ultrasonic extraction, recovering acetone solution to obtain cantharidin, and determining cantharidin content by liquid chromatography. The invention can greatly shorten the later extraction time after the cantharis is crushed, has high extraction content, is filtered after each extraction, has low impurity content, improves the extraction purity of the cantharidin, designs the mobile phase, the reference solution and the test solution, can accurately measure the content of the cantharidin by matching and carrying out chromatographic analysis and measurement, has simple operation, good repeatability and good recovery rate, and can realize accurate quantification of the cantharidin.
Drawings
FIG. 1 is a liquid chromatogram of an empty solution in example 1 of the present invention;
FIG. 2 is a liquid chromatogram of a control solution in example 1 of the present invention;
FIG. 3 is a liquid chromatogram of the test solution in example 1 of the present invention.
Detailed Description
The present invention is described in detail below with reference to the attached drawings so that the advantages and features of the present invention can be more easily understood by those skilled in the art, thereby clearly defining the protection scope of the present invention.
The following presents a simplified summary of one or more aspects in order to provide a basic understanding of such aspects. This summary is not an extensive overview of all contemplated aspects, and is intended to neither identify key or critical elements of all aspects nor delineate the scope of any or all aspects. Its sole purpose is to present some concepts of one or more aspects in a simplified form as a prelude to the more detailed description that is presented later.
A cantharidin content determination method comprises the following steps:
step 1), pulverizing the cantharis into 20-70 meshes of cantharis powder, adding water, uniformly mixing, carrying out ultrasonic extraction for 2-5 times, filtering, and combining filter residues;
step 2), carrying out enzymolysis by adopting protease, carrying out ultrasonic oscillation for not less than 6h, then adding an acetone solution, carrying out ultrasonic extraction for 30-50min, filtering, and combining filtrates;
step 3), adding alkali liquor, and recovering the acetone solution to obtain cantharidin; the addition of the lye is sufficient to ensure complete recovery of the acetone solution;
step 4), adopting liquid chromatography to measure the cantharidin content
Step 41) mobile phase preparation
Mixing methanol and water according to the weight ratio of 20-30: mixing at 75-80 vol% to obtain mobile phase;
step 42), preparing a reference solution
Taking a certain amount of cantharidin reference substance, placing in a volumetric flask, adding methanol for dilution, and fixing the volume;
step 43), preparing test solution
Taking a certain amount of cantharidin sample obtained in the step 3), placing the cantharidin sample in a volumetric flask, adding methanol for dissolving and diluting, and fixing the volume;
step 44), chromatographic assay
Respectively injecting a certain amount of blank solution, reference solution and test solution into a liquid chromatograph, respectively recording liquid chromatogram, and analyzing and determining cantharidin content according to the liquid chromatogram.
In the step 1), the cantharis is crushed into 20-40 meshes of cantharis powder, the water amount is 12-16 times of the weight of the cantharis powder each time, the cantharis powder and the water are mixed and stood for 15-25min, and then ultrasonic extraction is carried out for 2-5 times.
In step 41), the volume ratio of methanol to water is 23: 77.
in step 42), the concentration of the reference solution is 0.6-1.4 mg/ml.
In step 43), the concentration of the sample solution is 0.6-1.4 mg/ml.
And step 44), the chromatographic column adopted by the liquid chromatograph is an Agilent C18 column, the specifications of the chromatographic column are that the length is 250mm, the inner diameter is 4.6mm, the particle size is 5 mu m, and octadecylsilane chemically bonded silica is adopted as a filling agent.
In step 44), the conditions of the chromatographic assay are:
the mobile phase in the chromatographic column is methanol-water solution, the flow rate is 1.0ml/min, the detection wavelength is 230nm, the temperature of the chromatographic column is 25 ℃, and the sample injection amount is 5 mul.
Example 1
Reagents and materials:
methanol (analytical grade or higher);
purified water (ChP grade);
acetone solution;
a protease;
a base solution, preferably sodium hydroxide;
cantharidin reference substance;
cantharidin samples.
The instrument equipment comprises:
a liquid chromatograph;
a chromatographic column: agilent C18, 4.6X 250mm, 5 μm or equivalent performance column;
a pure water preparation instrument;
an analytical balance;
10ml volumetric flask.
Chromatographic conditions are as follows:
a chromatographic column: agilent C18, 250mm × 4.6mm, 5 μm or equivalent performance column
Column temperature: 25 deg.C
Mobile phase: methanol-water (23:77)
Flow rate: 1.0ml/min
Detection wavelength: 230nm
Sample introduction volume: 5 μ l.
Preparing a solution:
preparing a mobile phase:
mixing methanol and water at a ratio of (23:77) (v/v) to obtain the final product.
Preparing a reference substance solution:
weighing cantharidin reference substance 0.01g, precisely weighing with analytical balance, placing in 10ml volumetric flask, adding methanol to dilute to scale, and making into solution containing 1mg cantharidin per 1 ml.
Preparing a test solution:
taking 0.01g of the cantharis sample obtained in the step 3), precisely weighing by using an analytical balance, placing in a 10ml volumetric flask, adding methanol to dissolve and dilute to a scale, and preparing into a solution containing 1mg of cantharidin per 1 ml.
Chromatographic assay
And (4) taking appropriate amounts of the blank solution, the reference solution and the test solution, respectively injecting into a liquid chromatograph, and respectively recording liquid chromatogram maps.
FIGS. 1 to 3 are liquid chromatograms of a blank solution, a reference solution and a test solution, respectively. FIG. 1 is a liquid chromatogram of a blank solution; FIG. 2 is a liquid chromatogram of a control solution, wherein the average value of the cantharidin peak area is 281.736; FIG. 3 is a liquid chromatogram of the test solution, wherein the average value of the cantharidin peak area is 282.915.
The cantharidin content calculation formula is as follows:
in the formula:
Afor supplying to: peak area of the test solution;
Ato pair: peak area of the control solution;
Wfor supplying to: weighing the sample, g;
Wto pair: weighing a reference substance, and g;
Vto pair: dilution times of reference solutions;
Vfor supplying to: diluting the sample solution by multiple times;
p: and (5) marking the reference substance.
According to the above formula and the results of each chromatogram, the following is calculated:
the parts of the invention not specifically described can be realized by adopting the prior art, and the details are not described herein.
The above description is only an embodiment of the present invention, and not intended to limit the scope of the present invention, and all modifications of equivalent structures and equivalent processes, which are made by the present specification, or directly or indirectly applied to other related technical fields, are included in the scope of the present invention.
Claims (8)
1. The cantharidin content measuring method is characterized by comprising the following steps of:
step 1), pulverizing the cantharis into 20-70 meshes of cantharis powder, adding water, uniformly mixing, carrying out ultrasonic extraction for 2-5 times, filtering, and combining filter residues;
step 2), carrying out enzymolysis, carrying out ultrasonic oscillation for not less than 6h, then adding an acetone solution, carrying out ultrasonic extraction for 30-50min, filtering, and combining filtrates;
step 3), recovering the acetone solution to obtain cantharidin;
step 4), adopting liquid chromatography to measure the cantharidin content
Step 41) mobile phase preparation
Mixing methanol and water according to the weight ratio of 20-30: mixing at 75-80 vol% to obtain mobile phase;
step 42), preparing a reference solution
Taking a certain amount of cantharidin reference substance, placing in a volumetric flask, adding methanol for dilution, and fixing the volume;
step 43), preparing test solution
Taking a certain amount of cantharidin sample obtained in the step 3), placing the cantharidin sample in a volumetric flask, adding methanol for dissolving and diluting, and fixing the volume;
step 44), chromatographic assay
Respectively injecting a certain amount of blank solution, reference solution and test solution into a liquid chromatograph, respectively recording liquid chromatogram, and analyzing and determining cantharidin content according to the liquid chromatogram.
2. The method for measuring the content of cantharidin according to claim 1, wherein in step 1), the cantharis is pulverized into 20-40 mesh cantharis powder, the amount of water added each time is 12-16 times of the weight of the cantharis powder, the cantharis powder and the water are mixed and stood for 15-25min, and then ultrasonic extraction is carried out for 2-5 times.
3. The method for measuring the content of cantharidin according to claim 1, wherein in step 41), the volume ratio of methanol to water is 23: 77.
4. the method for measuring the content of cantharidin according to claim 1, wherein in step 42), the concentration of the reference solution is 0.6-1.4 mg/ml.
5. The method for measuring the content of cantharidin according to claim 1, wherein in step 43), the concentration of the sample solution is 0.6-1.4 mg/ml.
6. The method for measuring cantharidin content according to claim 1, wherein in step 44), the chromatographic column used in the liquid chromatograph is an Agilent C18 column, the chromatographic column has a length of 250mm, an inner diameter of 4.6mm and a particle size of 5 μm, and octadecylsilane chemically bonded silica is used as a filler.
7. The method for measuring the cantharidin content according to claim 1, wherein in step 44), the conditions of chromatographic analysis and measurement are as follows:
the mobile phase in the chromatographic column is methanol-water solution, the flow rate is 1.0ml/min, the detection wavelength is 230nm, the temperature of the chromatographic column is 25 ℃, and the sample injection amount is 5 mul.
8. The method for measuring the content of cantharidin according to claim 1, wherein in step 44), the content of cantharidin is calculated according to the following formula:
wherein:
Afor supplying to: peak area of the test solution;
Ato pair: peak area of the control solution;
Wfor supplying to: weighing the sample, g;
Wto pair: weighing a reference substance, and g;
Vto pair: dilution times of reference solutions;
Vfor supplying to: diluting the sample solution by multiple times;
p: and (5) marking the reference substance.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114113386A (en) * | 2021-11-23 | 2022-03-01 | 海南回元堂药业有限公司 | Detection method of cantharidin in cantharidin cream |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102268006A (en) * | 2011-06-15 | 2011-12-07 | 北京联合大学生物化学工程学院 | Method for extracting cantharidin from compound enzyme |
| CN107915741A (en) * | 2018-01-08 | 2018-04-17 | 佛山市聚成生化技术研发有限公司 | A kind of extracting method of cantharidin and its application |
-
2021
- 2021-08-20 CN CN202110959774.7A patent/CN113624887A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102268006A (en) * | 2011-06-15 | 2011-12-07 | 北京联合大学生物化学工程学院 | Method for extracting cantharidin from compound enzyme |
| CN107915741A (en) * | 2018-01-08 | 2018-04-17 | 佛山市聚成生化技术研发有限公司 | A kind of extracting method of cantharidin and its application |
Non-Patent Citations (2)
| Title |
|---|
| 廖秀英等: "斑蝥素与斑蝥多肽抗肿瘤活性比较", 《中药材》 * |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114113386A (en) * | 2021-11-23 | 2022-03-01 | 海南回元堂药业有限公司 | Detection method of cantharidin in cantharidin cream |
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Application publication date: 20211109 |