CN115407000A - Detection method of cannabidiol and tetrahydrocannabinol in industrial cannabis sativa - Google Patents
Detection method of cannabidiol and tetrahydrocannabinol in industrial cannabis sativa Download PDFInfo
- Publication number
- CN115407000A CN115407000A CN202211266876.1A CN202211266876A CN115407000A CN 115407000 A CN115407000 A CN 115407000A CN 202211266876 A CN202211266876 A CN 202211266876A CN 115407000 A CN115407000 A CN 115407000A
- Authority
- CN
- China
- Prior art keywords
- tetrahydrocannabinol
- cannabidiol
- sample
- hemp
- detecting
- 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.)
- Pending
Links
- 244000025254 Cannabis sativa Species 0.000 title claims abstract description 56
- CYQFCXCEBYINGO-UHFFFAOYSA-N THC Natural products C1=C(C)CCC2C(C)(C)OC3=CC(CCCCC)=CC(O)=C3C21 CYQFCXCEBYINGO-UHFFFAOYSA-N 0.000 title claims abstract description 33
- CYQFCXCEBYINGO-IAGOWNOFSA-N delta1-THC Chemical compound C1=C(C)CC[C@H]2C(C)(C)OC3=CC(CCCCC)=CC(O)=C3[C@@H]21 CYQFCXCEBYINGO-IAGOWNOFSA-N 0.000 title claims abstract description 33
- 229960004242 dronabinol Drugs 0.000 title claims abstract description 33
- QHMBSVQNZZTUGM-UHFFFAOYSA-N Trans-Cannabidiol Natural products OC1=CC(CCCCC)=CC(O)=C1C1C(C(C)=C)CCC(C)=C1 QHMBSVQNZZTUGM-UHFFFAOYSA-N 0.000 title claims abstract description 32
- QHMBSVQNZZTUGM-ZWKOTPCHSA-N cannabidiol Chemical compound OC1=CC(CCCCC)=CC(O)=C1[C@H]1[C@H](C(C)=C)CCC(C)=C1 QHMBSVQNZZTUGM-ZWKOTPCHSA-N 0.000 title claims abstract description 32
- 229950011318 cannabidiol Drugs 0.000 title claims abstract description 32
- ZTGXAWYVTLUPDT-UHFFFAOYSA-N cannabidiol Natural products OC1=CC(CCCCC)=CC(O)=C1C1C(C(C)=C)CC=C(C)C1 ZTGXAWYVTLUPDT-UHFFFAOYSA-N 0.000 title claims abstract description 32
- PCXRACLQFPRCBB-ZWKOTPCHSA-N dihydrocannabidiol Natural products OC1=CC(CCCCC)=CC(O)=C1[C@H]1[C@H](C(C)C)CCC(C)=C1 PCXRACLQFPRCBB-ZWKOTPCHSA-N 0.000 title claims abstract description 32
- 238000001514 detection method Methods 0.000 title claims abstract description 14
- 235000008697 Cannabis sativa Nutrition 0.000 title claims description 10
- 235000012766 Cannabis sativa ssp. sativa var. sativa Nutrition 0.000 claims abstract description 46
- 235000012765 Cannabis sativa ssp. sativa var. spontanea Nutrition 0.000 claims abstract description 46
- 235000009120 camo Nutrition 0.000 claims abstract description 46
- 235000005607 chanvre indien Nutrition 0.000 claims abstract description 46
- 239000011487 hemp Substances 0.000 claims abstract description 46
- 238000000034 method Methods 0.000 claims abstract description 18
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 22
- 238000001035 drying Methods 0.000 claims description 22
- 239000003960 organic solvent Substances 0.000 claims description 16
- 241000218236 Cannabis Species 0.000 claims description 13
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 12
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 11
- 239000001569 carbon dioxide Substances 0.000 claims description 11
- 239000012141 concentrate Substances 0.000 claims description 11
- 239000000126 substance Substances 0.000 claims description 11
- 238000000194 supercritical-fluid extraction Methods 0.000 claims description 11
- 239000006228 supernatant Substances 0.000 claims description 11
- 238000002137 ultrasound extraction Methods 0.000 claims description 11
- 239000007788 liquid Substances 0.000 claims description 10
- 239000000463 material Substances 0.000 claims description 10
- 239000012088 reference solution Substances 0.000 claims description 10
- 239000013558 reference substance Substances 0.000 claims description 8
- VZGDMQKNWNREIO-UHFFFAOYSA-N tetrachloromethane Chemical compound ClC(Cl)(Cl)Cl VZGDMQKNWNREIO-UHFFFAOYSA-N 0.000 claims description 8
- 238000007873 sieving Methods 0.000 claims description 6
- 238000005119 centrifugation Methods 0.000 claims description 5
- GBMDVOWEEQVZKZ-UHFFFAOYSA-N methanol;hydrate Chemical compound O.OC GBMDVOWEEQVZKZ-UHFFFAOYSA-N 0.000 claims description 5
- 239000002245 particle Substances 0.000 claims description 5
- 238000010298 pulverizing process Methods 0.000 claims description 5
- BZLVMXJERCGZMT-UHFFFAOYSA-N Methyl tert-butyl ether Chemical compound COC(C)(C)C BZLVMXJERCGZMT-UHFFFAOYSA-N 0.000 claims description 4
- 238000002474 experimental method Methods 0.000 description 10
- 239000000243 solution Substances 0.000 description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000012224 working solution Substances 0.000 description 2
- 241000196324 Embryophyta Species 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000010812 external standard method Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000004811 liquid chromatography Methods 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000012086 standard solution Substances 0.000 description 1
- 238000006467 substitution reaction 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
- G01N30/02—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
- G01N30/62—Detectors specially adapted therefor
- G01N30/74—Optical detectors
-
- 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
- G01N30/86—Signal analysis
- G01N30/8675—Evaluation, i.e. decoding of the signal into analytical information
-
- 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
- G01N2030/062—Preparation extracting sample from raw material
-
- 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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
Landscapes
- Physics & Mathematics (AREA)
- Biochemistry (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Engineering & Computer Science (AREA)
- Library & Information Science (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention relates to the technical field of hemp detection, in particular to a method for detecting cannabidiol and tetrahydrocannabinol in industrial hemp.
Description
Technical Field
The invention relates to the technical field of hemp detection, in particular to a method for detecting cannabidiol and tetrahydrocannabinol in industrial hemp.
Background
Industrial hemp refers to hemp having a tetrahydrocannabinol content of less than 0.3%, which is called hemp (hemp) in china, is an annual herb plant of Cannabis (Cannabiaceae) in Cannabis, which is classified into industrial hemp and drug hemp, and is widely used at home and abroad. The powder milled by the industrial hemp stalk core, namely the hemp stalk core superfine powder modified coating technology is applied to military uniforms and can exert the characteristics of high strength and high performance of products.
Patent application No. CN202111022160.2, which is described in the specification, standard solutions with different concentrations are prepared by adopting cannabidiol and tetrahydrocannabinol standard substances; extracting the sample with ethanol, separating with C18 chromatographic column, detecting at 220nm wavelength of ultraviolet detector, determining the nature according to retention time of chromatographic peak, and quantifying by external standard method to calculate the content of cannabidiol and tetrahydrocannabinol in the sample. And analyzing the standard working solution of the cannabidiol and the standard working solution of the tetrahydrocannabinol according to the established liquid chromatography conditions, drawing a standard working curve by taking the concentration as a horizontal ordinate and the peak area as a vertical coordinate, and quantifying a sample by using the standard working curve to ensure that the response values of the cannabidiol and the tetrahydrocannabinol are in a measurement linear range. The method is simple and convenient to operate, and the measurement result is accurate and reliable, although the above patent can be used for detecting cannabidiol and tetrahydrocannabinol, the detection can be directly carried out by extraction and filtration, the separation degree is poor, so that the detected result has large error and poor repeatability, and the use requirement cannot be met.
In summary, the development of a method for detecting cannabidiol and tetrahydrocannabinol in industrial cannabis is still a key problem to be solved urgently in the technical field of cannabis detection.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides the method for detecting the cannabidiol and the tetrahydrocannabinol in the industrial cannabis sativa.
In order to achieve the purpose, the invention provides the following technical scheme:
the invention provides a detection method of cannabidiol and tetrahydrocannabinol in industrial cannabis, which comprises the following steps:
(1) Taking a hemp sample, airing the hemp sample, sieving the hemp sample on a vibrating screen, and crushing the hemp sample by using a crusher to obtain a crushed substance;
(2) Drying the crushed material in a drying oven to obtain a dried material with the moisture content not more than 8%;
(3) Performing supercritical extraction on the dried substance by adopting carbon dioxide to obtain an extract;
(4) Adding an organic solvent into the extract, performing ultrasonic extraction again, centrifuging to collect supernatant, and concentrating the supernatant to 1:20-22 to obtain a concentrate;
(5) Preparing a series of reference solutions with cannabidiol and tetrahydrocannabinol standard reference substances, detecting the concentrate and the reference solution by using a high performance liquid chromatograph, drawing a standard working curve by taking the concentration as a horizontal axis and the peak area as a vertical axis, and quantifying the sample by using the standard working curve.
The invention is further provided with: the hemp sample in the step (1) is any one of hemp leaves or hemp stems.
The invention is further arranged as follows: in the step (1), the rotating speed of the pulverizer is 300-320r/min, and the pulverizing time is 12-14min.
The invention is further provided with: in the step (2), the temperature of the drying oven is 95-105 ℃, and the drying time is 20-60min.
The invention is further provided with: in the step (3), the supercritical extraction temperature is 30-60 ℃, the pressure is 10-30MPa, and the flow rate of carbon dioxide is 600-700kg/h.
The invention is further provided with: in the step (4), the organic solvent is any one of n-butanol, tert-butyl methyl ether or carbon tetrachloride.
The invention is further provided with: in the step (4), the mass ratio of the extract to the organic solvent is 1:3-5.
The invention is further provided with: in the step (4), the ultrasonic extraction time is 5-20min, and the power is 400-600W.
The invention is further provided with: in the step (4), the rotating speed of the centrifugation is 8000-12000r/min, and the time is 10-12min.
The invention is further provided with: in the step (5), the chromatographic conditions of the high performance liquid chromatograph are as follows: the chromatographic column is C 18 Column, column height 3.9mm, inner diameter 300mm, particle size 10 μm, mobile phase methanol-water (80 ml/min), flow rate 1ml/min, sample size 20 μ l, wavelength 210nm.
Advantageous effects
Compared with the known public technology, the technical scheme provided by the invention has the following beneficial effects:
the method provided by the invention comprises the steps of taking hemp leaves or hemp stems as samples, airing and sieving hemp samples, crushing, drying in a drying box, performing supercritical extraction by adopting carbon dioxide, adding an organic solvent into an extract, performing ultrasonic extraction, centrifugally collecting supernatant, preparing a series of reference substance solutions by using cannabidiol and tetrahydrocannabinol standard reference substances, detecting a concentrate and the reference substance solutions by adopting a high performance liquid chromatograph, drawing a standard working curve by taking the concentration as a horizontal axis and the peak area as a vertical axis, and quantifying a sample by using the standard working curve.
Drawings
FIG. 1 is a statistical chart of the fluctuation rate in the performance test of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. It is to be understood that the embodiments described are only a few embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The present invention will be further described with reference to the following examples.
Example 1:
the invention provides a detection method of cannabidiol and tetrahydrocannabinol in industrial cannabis, which comprises the following steps:
(1) Taking a hemp sample, airing the hemp sample, sieving the hemp sample on a vibrating screen, and crushing the hemp sample by using a crusher to obtain a crushed substance.
Further, the hemp sample is any one of hemp leaves or hemp stems.
Furthermore, the rotating speed of the pulverizer is 300r/min, and the pulverizing time is 12min.
(2) Drying the pulverized material in a drying oven to obtain dried material with water content of not more than 8%.
Furthermore, the temperature of the drying box is 95 ℃, and the drying time is 20min.
(3) And performing supercritical extraction on the dried substance by using carbon dioxide to obtain an extract.
Furthermore, the supercritical extraction temperature is 30 ℃, the pressure is 10MPa, and the flow of carbon dioxide is 600kg/h.
(4) Adding an organic solvent into the extract, performing ultrasonic extraction again, centrifuging to collect supernatant, and concentrating the supernatant to 1:20, obtaining a concentrate.
Further, the organic solvent is n-butanol.
Further, the mass ratio of the extract to the organic solvent was 1:3.
Further, the ultrasonic extraction time is 5min, and the power is 400W.
Further, the rotating speed of the centrifugation is 8000r/min, and the time is 10min.
(5) Preparing a series of reference solutions with cannabidiol and tetrahydrocannabinol standard reference substances, detecting the concentrate and the reference solution by using a high performance liquid chromatograph, drawing a standard working curve by taking the concentration as a horizontal axis and the peak area as a vertical axis, and quantifying the sample by using the standard working curve.
Further, the chromatographic conditions of the high performance liquid chromatograph are as follows: the chromatographic column is C 18 Column, column height 3.9mm, inner diameter 300mm, particle size 10 μm, mobile phase methanol-water (80 ml/min), flow rate 1ml/min, sample size 20 μ l, wavelength 210nm.
Example 2:
the invention provides a detection method of cannabidiol and tetrahydrocannabinol in industrial cannabis, which comprises the following steps:
(1) Taking a hemp sample, airing the hemp sample, sieving the hemp sample on a vibrating screen, and crushing the hemp sample by using a crusher to obtain a crushed substance.
Further, the hemp sample is any one of hemp stems.
Furthermore, the rotating speed of the pulverizer is 310r/min, and the pulverizing time is 13min.
(2) Drying the pulverized material in a drying oven to obtain dried material with water content of not more than 8%.
Further, the temperature of the drying box is 100 ℃, and the drying time is 40min.
(3) And performing supercritical extraction on the dried substance by using carbon dioxide to obtain an extract.
Furthermore, the supercritical extraction temperature is 45 ℃, the pressure is 20MPa, and the flow of carbon dioxide is 650kg/h.
(4) Adding an organic solvent into the extract, performing ultrasonic extraction again, centrifuging to collect supernatant, and concentrating the supernatant to 1:21, obtaining a concentrate.
Further, the organic solvent is any one of n-butyl alcohol, tert-butyl methyl ether or carbon tetrachloride.
Further, the mass ratio of the extract to the organic solvent was 1:4.
Further, the time of ultrasonic extraction is 12min, and the power is 500W.
Further, the rotation speed of the centrifugation is 10000r/min, and the time is 11min.
(5) Preparing a series of reference solutions with cannabidiol and tetrahydrocannabinol standard reference substances, detecting the concentrate and the reference solution by using a high performance liquid chromatograph, drawing a standard working curve by taking the concentration as a horizontal axis and the peak area as a vertical axis, and quantifying the sample by using the standard working curve.
Further, the chromatographic conditions of the high performance liquid chromatograph are as follows: the chromatographic column is C 18 Column, column height 3.9mm, inner diameter 300mm, particle size 10 μm, mobile phase methanol-water (801ml/min, a sample size of 20. Mu.l, a wavelength of 210nm.
Example 3:
the invention provides a detection method of cannabidiol and tetrahydrocannabinol in industrial cannabis sativa, which comprises the following steps:
(1) Taking a hemp sample, airing the hemp sample, sieving the hemp sample on a vibration sieve, and crushing the hemp sample by using a crusher to obtain a crushed substance.
Further, the hemp sample is any one of hemp leaves or hemp stems.
Furthermore, the rotating speed of the pulverizer is 320r/min, and the pulverizing time is 14min.
(2) Drying the pulverized material in a drying oven to obtain dried material with water content of not more than 8%.
Further, the temperature of the drying oven was 105 ℃ and the drying time was 60min.
(3) And performing supercritical extraction on the dried substance by using carbon dioxide to obtain an extract.
Furthermore, the supercritical extraction temperature is 60 ℃, the pressure is 30MPa, and the flow of carbon dioxide is 700kg/h.
(4) Adding an organic solvent into the extract, performing ultrasonic extraction again, centrifuging to collect supernatant, and concentrating the supernatant to 1:22, obtaining a concentrate.
Further, the organic solvent is any one of n-butyl alcohol, tert-butyl methyl ether or carbon tetrachloride.
Further, the mass ratio of the extract to the organic solvent was 1:5.
Further, the time of ultrasonic extraction is 20min, and the power is 600W.
Further, the rotation speed of the centrifugation is 12000r/min, and the time is 12min.
(5) Preparing a series of reference solutions with cannabidiol and tetrahydrocannabinol standard reference substances, detecting the concentrate and the reference solution by using a high performance liquid chromatograph, drawing a standard working curve by taking the concentration as a horizontal axis and the peak area as a vertical axis, and quantifying the sample by using the standard working curve.
Further, of high performance liquid chromatographyThe chromatographic conditions are as follows: the chromatographic column is C 18 Column, column height 3.9mm, inner diameter 300mm, particle size 10 μm, mobile phase methanol-water (80 ml/min), flow rate 1ml/min, sample size 20 μ l, wavelength 210nm.
And (3) performance detection:
cannabis leaves are taken as samples, cannabidiol and tetrahydrocannabinol are detected by the methods of example 1, example 2 and example 3 respectively, cannabidiol and tetrahydrocannabinol are detected by the method of patent application No. CN202111022160.2 respectively, the samples are taken as experiment 1 group, experiment 2 group, experiment 3 group and control group respectively, the repetition is carried out for 10 times, the fluctuation rate of the detection result of 10 repeated experiments of each group is counted, and relevant data are recorded in a table 1.
Table 1: fluctuation ratio of each group of repeated experiments
As can be seen from table 1 and fig. 1, the fluctuation ratios of the complex experiments in the experimental groups (experiment 1 group, experiment 2 group, and experiment 3 group) were significantly lower than those in the control group (p < 0.05), and the fluctuation ratio difference of the complex experiments between the experimental groups was not significant (p > 0.05). The method provided by the invention can improve the purity of the extracted cannabidiol and tetrahydrocannabinol, so that the detection result has small fluctuation and is more reliable.
The above examples are only intended to illustrate the technical solution of the present invention, and not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; such modifications and substitutions do not depart from the spirit and scope of the corresponding technical solutions.
Claims (10)
1. A detection method of cannabidiol and tetrahydrocannabinol in industrial cannabis is characterized by comprising the following steps:
(1) Taking a hemp sample, airing the hemp sample, sieving the hemp sample on a vibrating screen, and crushing the hemp sample by using a crusher to obtain a crushed substance;
(2) Drying the crushed material in a drying oven to obtain a dried material with the moisture content of not more than 8%;
(3) Performing supercritical extraction on the dried substance by adopting carbon dioxide to obtain an extract;
(4) Adding an organic solvent into the extract, performing ultrasonic extraction again, centrifuging to collect supernatant, and concentrating the supernatant to 1:20-22 to obtain a concentrate;
(5) Preparing a series of reference solutions with cannabidiol and tetrahydrocannabinol standard reference substances, detecting the concentrate and the reference solution by using a high performance liquid chromatograph, drawing a standard working curve by taking the concentration as a horizontal axis and the peak area as a vertical axis, and quantifying the sample by using the standard working curve.
2. The method of claim 1, wherein the cannabidiol and tetrahydrocannabinol are detected from industrial cannabis sativa, wherein the cannabis sativa sample in step (1) is any one of cannabis sativa leaves or cannabis sativa stems.
3. The method as claimed in claim 1, wherein the rotation speed of the pulverizer is 300-320r/min and the pulverizing time is 12-14min in step (1).
4. The method for detecting cannabidiol and tetrahydrocannabinol in industrial cannabis sativa as claimed in claim 1, wherein in step (2), the temperature of the drying oven is 95-105 ℃ and the drying time is 20-60min.
5. The method for detecting cannabidiol and tetrahydrocannabinol in industrial cannabis as claimed in claim 1, wherein in step (3), the supercritical extraction temperature is 30-60 ℃, the pressure is 10-30MPa, and the flow rate of carbon dioxide is 600-700kg/h.
6. The method for detecting cannabidiol and tetrahydrocannabinol in industrial cannabis, as claimed in claim 1, wherein in step (4), the organic solvent is any one of n-butanol, tert-butyl methyl ether or carbon tetrachloride.
7. The method for detecting cannabidiol and tetrahydrocannabinol in industrial cannabis sativa as claimed in claim 1, wherein in step (4), the mass ratio of the extract to the organic solvent is 1:3-5.
8. The method for detecting cannabidiol and tetrahydrocannabinol in industrial cannabis as claimed in claim 1, wherein in step (4), the ultrasonic extraction time is 5-20min and the power is 400-600W.
9. The method as claimed in claim 1, wherein the centrifugation is performed at 8000-12000r/min for 10-12min in step (4).
10. The method for detecting cannabidiol and tetrahydrocannabinol in industrial cannabis as claimed in claim 1, wherein in step (5), the chromatographic conditions of the hplc are: the chromatographic column is C 18 Column, column height 3.9mm, inner diameter 300mm, particle size 10 μm, mobile phase methanol-water (80 ml/min), flow rate of 1ml/min, sample size of 20 μ l, wavelength 210nm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211266876.1A CN115407000A (en) | 2022-10-17 | 2022-10-17 | Detection method of cannabidiol and tetrahydrocannabinol in industrial cannabis sativa |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211266876.1A CN115407000A (en) | 2022-10-17 | 2022-10-17 | Detection method of cannabidiol and tetrahydrocannabinol in industrial cannabis sativa |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN115407000A true CN115407000A (en) | 2022-11-29 |
Family
ID=84169086
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202211266876.1A Pending CN115407000A (en) | 2022-10-17 | 2022-10-17 | Detection method of cannabidiol and tetrahydrocannabinol in industrial cannabis sativa |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN115407000A (en) |
Citations (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB0222078D0 (en) * | 2002-09-23 | 2002-10-30 | Gw Pharma Ltd | Method of preparing cannabidiol from plant material |
| CN107337586A (en) * | 2017-08-28 | 2017-11-10 | 黑龙江省科学院大庆分院 | A kind of method of extraction purification cannabidiol in fiber crops from the Chinese |
| CN107382672A (en) * | 2017-07-28 | 2017-11-24 | 云南汉木森生物科技有限责任公司 | Utilize the method and its cannabidiol product of supercritical carbon dioxide extracting cannabidiol |
| CN107589203A (en) * | 2017-09-21 | 2018-01-16 | 黑龙江省科学院大庆分院 | A kind of method for detecting three kinds of cannabinol compounds in Chinese fiber crops simultaneously using SPE HPLC |
| UY37799A (en) * | 2017-07-07 | 2019-01-02 | Orochem Tech Inc | PROCESS FOR PURIFICATION AND SEPARATION OF CANNABINOID DRY HEMP AND CANNABIS LEAVES |
| CN109232191A (en) * | 2018-08-20 | 2019-01-18 | 润贝（安徽）饮料食品有限公司 | A method of extracting cannabidiol in industrial hemp leaf |
| CN109725080A (en) * | 2019-01-02 | 2019-05-07 | 中国农业科学院麻类研究所 | Cannabidiol, cannabidiolic acid, in tetrahydrocannabinol one or more of substances method for qualitative and quantitative detection |
| CN110780003A (en) * | 2019-11-13 | 2020-02-11 | 云南绿新生物药业有限公司 | Method for measuring content of cannabidiol and tetrahydrocannabinol in industrial cannabis sativa leaves |
| CN111122744A (en) * | 2020-01-20 | 2020-05-08 | 云南绿新生物药业有限公司 | Method for detecting content of one or more cannabinoids in industrial hemp extract by using HPLC |
| CN112034059A (en) * | 2020-08-21 | 2020-12-04 | 滇麻生物科技(曲靖)有限公司 | Method for detecting cannabinoids in industrial hemp flowers and leaves and extract thereof by high performance liquid chromatography |
| CN112730696A (en) * | 2020-09-15 | 2021-04-30 | 中国标准化研究院 | Method for detecting 5 cannabinol compounds in cannabis sativa oil by using HPLC (high performance liquid chromatography) method |
| CN114527201A (en) * | 2021-09-01 | 2022-05-24 | 吉林省农业科学院 | Detection method of cannabidiol and tetrahydrocannabinol in cannabis sativa |
| CN115032287A (en) * | 2021-03-04 | 2022-09-09 | 云南翰谷生物科技有限公司 | Quantitative analysis method of tetrahydrocannabinol and cannabidiol |
-
2022
- 2022-10-17 CN CN202211266876.1A patent/CN115407000A/en active Pending
Patent Citations (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB0222078D0 (en) * | 2002-09-23 | 2002-10-30 | Gw Pharma Ltd | Method of preparing cannabidiol from plant material |
| UY37799A (en) * | 2017-07-07 | 2019-01-02 | Orochem Tech Inc | PROCESS FOR PURIFICATION AND SEPARATION OF CANNABINOID DRY HEMP AND CANNABIS LEAVES |
| US20190010107A1 (en) * | 2017-07-07 | 2019-01-10 | Orochem Technologies, Inc. | Process for purification and separation of cannabinoids, from dried hemp and cannabis leaves |
| CN107382672A (en) * | 2017-07-28 | 2017-11-24 | 云南汉木森生物科技有限责任公司 | Utilize the method and its cannabidiol product of supercritical carbon dioxide extracting cannabidiol |
| CN107337586A (en) * | 2017-08-28 | 2017-11-10 | 黑龙江省科学院大庆分院 | A kind of method of extraction purification cannabidiol in fiber crops from the Chinese |
| CN107589203A (en) * | 2017-09-21 | 2018-01-16 | 黑龙江省科学院大庆分院 | A kind of method for detecting three kinds of cannabinol compounds in Chinese fiber crops simultaneously using SPE HPLC |
| CN109232191A (en) * | 2018-08-20 | 2019-01-18 | 润贝（安徽）饮料食品有限公司 | A method of extracting cannabidiol in industrial hemp leaf |
| CN109725080A (en) * | 2019-01-02 | 2019-05-07 | 中国农业科学院麻类研究所 | Cannabidiol, cannabidiolic acid, in tetrahydrocannabinol one or more of substances method for qualitative and quantitative detection |
| CN110780003A (en) * | 2019-11-13 | 2020-02-11 | 云南绿新生物药业有限公司 | Method for measuring content of cannabidiol and tetrahydrocannabinol in industrial cannabis sativa leaves |
| CN111122744A (en) * | 2020-01-20 | 2020-05-08 | 云南绿新生物药业有限公司 | Method for detecting content of one or more cannabinoids in industrial hemp extract by using HPLC |
| CN112034059A (en) * | 2020-08-21 | 2020-12-04 | 滇麻生物科技(曲靖)有限公司 | Method for detecting cannabinoids in industrial hemp flowers and leaves and extract thereof by high performance liquid chromatography |
| CN112730696A (en) * | 2020-09-15 | 2021-04-30 | 中国标准化研究院 | Method for detecting 5 cannabinol compounds in cannabis sativa oil by using HPLC (high performance liquid chromatography) method |
| CN112730697A (en) * | 2020-09-15 | 2021-04-30 | 中国标准化研究院 | Method for simultaneously detecting 5 cannabinol compounds by using HPLC-MS/MS |
| CN115032287A (en) * | 2021-03-04 | 2022-09-09 | 云南翰谷生物科技有限公司 | Quantitative analysis method of tetrahydrocannabinol and cannabidiol |
| CN114527201A (en) * | 2021-09-01 | 2022-05-24 | 吉林省农业科学院 | Detection method of cannabidiol and tetrahydrocannabinol in cannabis sativa |
Non-Patent Citations (1)
| Title |
|---|
| 刘波: "《药物分析》", 西安交通大学出版社, pages: 69 - 70 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102183611B (en) | Method for detecting pesticide residue in white paeony root crude drug | |
| CN103789094A (en) | Method for extracting agilawood essential oil from agilawood chips | |
| CN107011308B (en) | The method of polymethoxyflavone class compound is isolated and purified from bowl mandarin orange fruit | |
| CN103076411A (en) | Analytical method for determining aromatic constituents in tea | |
| Shen et al. | DART-MS: a new research tool for herbal medicine analysis | |
| CN102980956A (en) | Quick extraction and detection method of 9-oxo-10,11-dehydroagerophorone | |
| CN109134583B (en) | Method for extracting triterpenoids from schefflera octophylla leaves by using ionic liquid | |
| CN101525328B (en) | Method for extracting alpha-mangostin from mangosteen fruit peel | |
| CN104807907A (en) | Determination method for content of buddleoside in dendranthema indicum | |
| CN108627596B (en) | Method for detecting content of multiple flavone compounds in taxus chinensis branches and preparation method thereof | |
| CN115407000A (en) | Detection method of cannabidiol and tetrahydrocannabinol in industrial cannabis sativa | |
| CN106496292A (en) | A kind of method for preparing 6 iridoid glycoside constituents from Fructus Gardeniae simultaneously | |
| CN103710421A (en) | Method for establishing lucid ganoderma sporophore HPLC (High Performance Liquid Chromatography) finger-print spectrum | |
| CN106442805A (en) | Method for extracting milled wood lignin from stone cells in Korla fragrant pear fruit | |
| CN106526056A (en) | Ultra-high performance liquid chromatography and tandem mass spectrometry detection method for AFB1 in beer and raw and auxiliary materials of beer | |
| Huang et al. | The quantification of monacolin K in some red yeast rice from Fujian province and the comparison of the other product | |
| CN105859715A (en) | Critical fluid chromatographic method for separating and purifying evodiamine and rutaecarpine from fructus evodiae | |
| CN108101923A (en) | A kind of process for separation and purification of glabridin monomer | |
| CN105906687B (en) | A kind of method that a variety of tanshinone monomer components are isolated and purified from the red sage root | |
| CN103275054A (en) | Method for preparing bellidifolin | |
| CN105693675A (en) | A method of extracting flavonoid compounds from tagetes erecta | |
| CN114414701A (en) | Preparation method and content determination method of myrobalamin acid in myrobalan meat | |
| CN113063867A (en) | Method for detecting bitter metabolites of wild bitter Chinese wolfberry | |
| Cui et al. | Fingerprint profile of active components for Andrographis paniculata Nees by HPLC-DAD | |
| CN104062389B (en) | A kind of Folium camelliae assamicae GC finger printing test method of Different Extraction Method |
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 | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20221129 |