CN112362798B - Method for detecting cannabidiol in cosmetics - Google Patents
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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
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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
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
- G01N2030/8809—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample
- G01N2030/884—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample organic compounds
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- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
Abstract
The invention relates to the technical field of cosmetic detection, in particular to a detection method of cannabidiol in cosmetics. The detection method comprises the following steps: mixing the sample with an extraction solvent, and performing ultrasonic extraction to obtain an extraction solution; adding the extracting solution into a purifying column for purifying and filtering to obtain target detection solution; the purifying column is an MPFC-QuEChERS high-lipid ultrafiltration purifying column made of nano composite materials; and analyzing and detecting the target detection liquid by adopting an ultra-high performance liquid chromatography-triple quaternary tandem mass spectrometry. The detection method realizes the detection of cannabidiol in cosmetics, and has short analysis time and stable and reliable qualitative and quantitative detection results.
Description
Technical Field
The invention relates to the technical field of cosmetic detection, in particular to a detection method of cannabidiol in cosmetics.
Background
Cannabis sativa l., hemp), also known as line Hemp, cannabis sativa, etc., is an annual Moraceae plant. Tetrahydrocannabinol (THC) is generally classified into industrial cannabis and drug cannabis according to the proportion of cannabis. The content of tetrahydrocannabinol in industrial cannabis is up to 0.3%, while the content of tetrahydrocannabinol in drug cannabis is higher. The Cannabinoids (CBs) currently isolated from cannabis include mainly Cannabidiol (CBD), tetrahydrocannabinol, cannabinol (CBN), and cannabidene (CBC). In recent years, research and development of cannabidiol and cannabis extracts have been rapidly progressed, and there have been reports on the same. Cannabidiol is a major chemical component in industrial cannabis, and there has been a trend to use industrial cannabis extracts as an active ingredient or additive in the preparation of skin care products. Because the skin care product has various effects of relieving pain, resisting inflammation, removing freckles, removing jaundice, removing acnes, resisting aging, resisting wrinkles and the like, the skin care product can be rapidly covered in the skin care product consumer market, especially in the European skin care product market.
The existing analysis methods for measuring cannabidiol content mainly comprise Gas Chromatography (GC), gas chromatography-tandem mass spectrometry (GC-MS/MS), liquid chromatography-tandem mass spectrometry (LC-MS/MS), liquid chromatography (HPLC) and the like. The cannabidiol detection method reported in the literature is mainly aimed at the detection of drugs, blood or hair and the like based on forensic or public security material evidence identification fields, plants, plant edible oil, fructus cannabis and fructus cannabis oil. In the field of cosmetic detection, CANNABIS sativa leaf EXTRACT (CANNABIS SATIVA LEAF EXTRACT), CANNABIS sativa fruit (CANNABIS SATIVA FRUIT) and CANNABIS sativa seed OIL (CANNABIS SATIVA SEED OIL) have been listed as cosmetic raw materials which can be used in the catalog of names of used cosmetic raw materials (2015 edition), but the detection and analysis methods thereof are not covered in the national "cosmetic safety technical Specification (2015 edition)", nor are related national standards. Research institutions at home and abroad are developing detection research on cannabidiol in cosmetics. Therefore, in order to effectively perform quality control and safety assessment of cosmetics containing cannabis extract, it is necessary to establish a method for measuring cannabidiol content in cosmetics. However, the cosmetic matrix is various and complex, and if the pretreatment is improper, the accurate detection of cannabidiol is easily affected.
Disclosure of Invention
In view of the above, the present invention provides a method for detecting cannabidiol in cosmetics. The detection method realizes the detection of cannabidiol in cosmetics, and has the characteristics of short analysis time, stable and reliable qualitative and quantitative detection results, and the like.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a method for detecting cannabidiol in cosmetics, which comprises the following steps:
mixing the sample with an extraction solvent, and performing ultrasonic extraction to obtain an extraction solution;
adding the extracting solution into a purifying column for purifying and filtering to obtain target detection solution; the purifying column is an MPFC-QuEChERS high-lipid ultrafiltration purifying column made of nano composite materials;
and analyzing and detecting the target detection liquid by adopting an ultra-high performance liquid chromatography-triple quaternary tandem mass spectrometry.
According to the method, the complexity of the cosmetic matrix is considered to possibly cause matrix effect in the ultra-high performance liquid chromatography-triple quaternary rod tandem mass spectrometry detection process, and potential influence is generated on the measurement result of the to-be-measured object in the sample, so that different purification means are selected to perform pretreatment on the sample, the purification effects of different types of purification means are studied in the future, and a proper sample pretreatment method is selected. The invention is based on cosmetic samples, and 3 kinds of masks, creams and aquas without hemp components are selected as blank matrixes of cosmetics due to large differences of different cosmetic matrixes. The MPFC-QuEChERS ultrafiltration purification column adopts a nanocomposite material, has large specific surface area, is superior to PSA, C18 and the like in removing other macromolecular interferents in a matrix, has good extraction effect, and can ensure that the recovery rate of cannabidiol meets the requirement. According to the invention, the QuEChERS rapid sample pretreatment technology is used for detecting cannabidiol in cosmetics for the first time, the pretreatment process is simple and rapid, the samples can be detected on machine after being subjected to solvent extraction and rapid purification by the purification column, the extraction and purification efficiency of the samples is improved, and the blank of the cannabidiol detection technology in cosmetics is filled.
MPFC is a short name of multiplug filtration clean-up and is translated into a 'multiple filtration type purification column'.
Preferably, the purification column is a LUMTECH MPFC-QuEChERS purification column. Purchased from beijing green cotton technologies limited.
Preferably, the extraction solvent is methanol.
Preferably, the ratio of sample to extraction solvent is 1 in g/mL: (5-15).
Preferably, the ratio of sample to extraction solvent is 1 in g/mL: 10.
in some embodiments of the invention, the sample is vortexed after mixing with the extraction solvent for 30-60 s.
Preferably, the temperature of ultrasonic extraction is 20-30 ℃, the power of ultrasonic extraction is 500-700W, and the time of ultrasonic extraction is 10-30 min.
Preferably, the temperature of ultrasonic extraction is room temperature, the power of ultrasonic extraction is 600W, and the time of ultrasonic extraction is 10min.
Preferably, the filtration is by a microporous organic filter membrane.
Preferably, the microporous organic filter membrane is a polytetrafluoroethylene filter membrane of 0.22 μm.
Preferably, the chromatographic conditions of the ultra performance liquid chromatography-triple quadrupole tandem mass spectrometry are as follows:
chromatographic column: cao CAPCELL CORE ADME column, length 100mm, inner diameter 2.1mm, particle size 2.7 μm;
mobile phase: 0.05vt% -0.15 vt% formic acid aqueous solution and 0.05vt% -0.15 vt% formic acid acetonitrile solution;
column temperature is 35-45 ℃; flow rate: 0.2-0.4 mL/min; the sample injection amount is 2-8 mu L.
Preferably, the chromatographic conditions of ultra performance liquid chromatography-triple quadrupole tandem mass spectrometry are:
mobile phase: 0.1% formic acid aqueous solution and 0.1% formic acid acetonitrile solution;
column temperature 40 ℃; flow rate: 0.3mL/min; the sample injection amount was 5. Mu.L.
Preferably, the gradient elution procedure for the mobile phase is:
| time/min | Aqueous formic acid solution/% | Acetonitrile formate solution/% |
| 0 | 50 | 50 |
| 5 | 10 | 90 |
| 7 | 10 | 90 |
| 7.1 | 50 | 50 |
| 9 | 50 | 50 |
。
Preferably, the mass spectrometry conditions of the ultra performance liquid chromatography-triple quadrupole tandem mass spectrometry are as follows: the ionization mode is an electrospray ion source positive ion mode, the multi-reaction monitoring mode signal acquisition is carried out, the atomization air flow is 2.5-3.5L/min, the drying air flow is 8-12L/min, the heating air flow is 8-12L/min, the interface temperature is 250-350 ℃, and the interface voltage is 3.0-5.0 kV.
Preferably, the mass spectrometry conditions of the ultra performance liquid chromatography-triple quadrupole tandem mass spectrometry are: the ionization mode is an electrospray ion source positive ion mode, multiple reaction monitoring mode signal acquisition, atomization air flow rate of 3L/min, drying air flow rate of 10L/min, heating air flow rate of 10L/min, interface temperature of 300 ℃ and interface voltage of 4.0kV.
The invention provides a method for detecting cannabidiol in cosmetics. The detection method comprises the following steps: mixing the sample with an extraction solvent, and performing ultrasonic extraction to obtain an extraction solution; adding the extracting solution into a purifying column for purifying and filtering to obtain target detection solution; the purifying column is an MPFC-QuEChERS high-lipid ultrafiltration purifying column made of nano composite materials; and analyzing and detecting the target detection liquid by adopting an ultra-high performance liquid chromatography-triple quaternary tandem mass spectrometry. The beneficial effects of the invention are as follows:
(1) The invention fully considers the characteristics of diversity and complexity of cosmetic matrixes and the like, and detects cannabidiol in cosmetics for the first time by adopting an ultra-high performance liquid chromatography-triple quadrupole tandem mass spectrometry by optimizing and comparing different pretreatment conditions, has short analysis time, high sensitivity, strong selectivity and stable and reliable qualitative and quantitative detection results, can be used for risk assessment, screening and monitoring of cannabidiol in cosmetics, and has wider application prospect. The method for detecting cannabidiol in cosmetics has the advantages that the method fills the blank of the project detection method to a certain extent, can meet the requirements of qualitative and quantitative analysis of cannabidiol in cosmetics, and provides scientific basis and technical support for safety supervision of related products of cosmetics.
(2) The detection method is simple and quick in pretreatment process of cosmetics, the MPFC-QuEChERS rapid sample pretreatment technology is used for detecting cannabidiol in cosmetics for the first time, and the samples can be detected on machine after being subjected to solvent extraction and rapid purification by the purification column, so that the extraction and purification efficiency of the samples is improved, and the requirements on the operation technical level of a tester are relatively low.
(3) The detection method provided by the invention has important significance for accurately identifying cannabidiol components in cosmetics. Considering that cannabinoids such as Cannabidiol (CBD), tetrahydrocannabinol (THC), cannabidene (CBC) are isomers of each other, interference may occur due to uniform retention time and the same ion fragments (ion pairs) under different liquid phase separation conditions. The retention behavior of the 3 substances on the chromatographic column is studied in the process of the invention, the 3 substances have different retention times under the separation condition adopted by the invention, and whether cannabidiol is contained or not is identified by comparing the compound peaks in the actual cosmetic sample with the 3 compound peaks, so that mutual interference is eliminated, effective separation is realized, and false judgment of generating cannabidiol false positive or false negative is avoided. In addition, since tetrahydrocannabinol belongs to not only the first controlled substances in the catalogue of the mental medicine variety of the people's republic of China (2013 edition) but also forbidden substances specified in the technical Specification of cosmetic safety (2015 edition), accurate identification of the cosmetic sample containing or added with tetrahydrocannabinol has important significance for quality safety supervision of cosmetics.
Drawings
FIG. 1 total ion flow diagram of Cannabidiol (CBD), tetrahydrocannabinol (THC) and cannabidene (CBC);
FIG. 2 measurement of the recovery of cannabidiol from 3 different base cosmetics under different purification apparatus conditions; wherein a: shimadzu QuEChERS SPE purge tube; b: filtration was performed using only microporous membranes; c: LUMTECH MPFC-QuEChERS (high lipid) ultrafiltration purification column; d: waters Prime HLB column; e: waters QuEChERS SPE purification column; m: a facial mask; c: cream; a: an aqueous solution.
Detailed Description
The invention discloses a method for detecting cannabidiol in cosmetics, and a person skilled in the art can properly improve the technological parameters by referring to the content of the cannabidiol. It is expressly noted that all such similar substitutions and modifications will be apparent to those skilled in the art, and are deemed to be included in the present invention. While the methods and applications of this invention have been described in terms of preferred embodiments, it will be apparent to those skilled in the relevant art that variations and modifications can be made in the methods and applications described herein, and in the practice and application of the techniques of this invention, without departing from the spirit or scope of the invention.
The reagents or instruments used in the method for detecting cannabidiol in the cosmetic of the present invention are commercially available. The instruments used were as follows:
AL 204 analytical balance (mertrehler tolidox, switzerland); vortex Genie 2 Vortex mixer (us Scientific Industries company); KQ-3200DE ultrasonic cleaner (Jiangsu Kunshan ultrasonic instruments Co., ltd.).
The invention is further illustrated by the following examples:
example 1 method for detecting cannabidiol in cosmetics
1. Sample extraction
Accurately weighing 1g (accurate to 0.001 g) of the cosmetic sample, placing the cosmetic sample in a 10mL colorimetric tube with a plug, adding methanol to 10mL, and oscillating at high speed on a vortex mixer for 30s to fully mix the sample with the extraction solvent. Sealing, ultrasonic extracting for 10min, and standing to room temperature.
2. Sample purification
After the sample is kept stand to room temperature, the sample is purified by a LUMTECH MPFC-QuEChERS (high-lipid) ultrafiltration purification column (Beijing green cotton technology Co., ltd.) and filtered by a polytetrafluoroethylene microporous filter membrane with the size of 0.22 mu m, and the subsequent filtrate is taken as a solution to be tested.
Because the cosmetic matrix is complex and the differences between different cosmetic matrixes are large, the invention selects 3 kinds of masks, cream and water agents which do not contain hemp components as blank matrixes of cosmetics, and examines the sample purifying effect by a sample adding recovery method. Purifying and filtering by using Shimadzu QuEChERS SPE purifying tube, directly filtering with 0.22 μm filter membrane without purification, purifying and filtering by using LUMTECH MPFC-QuEChERS ultrafiltration type purifying column, purifying and filtering by using Waters Prime HLB column, purifying and filtering by using Waters QuEChERS SPE purifying tube, treating sample extract, performing ultra-high performance liquid chromatography-tandem triple four-level rod mass spectrometry under the same condition, and calculating standard deviation and standard deviation. The results show that: the recovery rate of cannabidiol in the pretreatment mode of Shimadzu QuEChERS SPE purifying column purifying, LUMTECH MPFC-QuEChERS (high lipid) ultrafiltration purifying column purifying and Waters QuEChERS SPE purifying tube purifying 3 samples meets the test requirement, but the standard deviation of 3 times of measurement of the purifying results of Shimadzu QuEChERS SPE purifying tube purifying and Waters QuEChERS SPE purifying tube purifying is larger. And (3) comprehensively analyzing experimental results, wherein the LUMTECH MPFC-QuEChERS (high lipid) ultrafiltration type purification column has the best purification effect, and the recovery rate and the repeatability meet the requirements and can be used as a preferred method.
3. Sample detection
And performing ultra-high performance liquid chromatography-triple quadrupole tandem mass spectrometry on the purified sample by adopting an LCMS-8060 ultra-high performance liquid chromatography-triple quadrupole mass spectrometer (Shimadzu corporation).
Chromatographic conditions:
chromatographic column: cao CAPCELL CORE ADME column (2.1 mm. Times.100 mm,2.7 μm), mobile phase: 0.1% formic acid in water and 0.1% formic acid in acetonitrile, and performing gradient elution; the flow rate is 0.3mL/min, the sample injection amount is 5 mu L, and the column temperature is as follows: 40 ℃. The mobile phase and gradient elution procedure are shown in table 1.
TABLE 1 mobile phase composition and gradient elution procedure
| Time/min | 0.1% formic acid aqueous solution/% | 0.1% formic acid acetonitrile solution/% |
| 0 | 50 | 50 |
| 5 | 10 | 90 |
| 7 | 10 | 90 |
| 7.1 | 50 | 50 |
| 9 | 50 | 50 |
Mass spectrometry conditions: ion source: electrospray ion source positive ion mode (ESI) + ) The method comprises the steps of carrying out a first treatment on the surface of the Detection mode: multiple Reaction Monitoring (MRM) mode, atomizing air flow rate of 3L/min, drying air flow rate of 10L/min, heating air flow rate of 10L/min, interface temperature of 300 ℃ and interface voltage of 4.0kV. Mass spectrum parameters of cannabidiol and parent and child ions are shown in Table 2.
TABLE 2 Mass Spectrometry parameters and qualitative and quantitative ion pairs for Cannabidiol (CBD)
The liquid quality analysis of cannabinoid can adopt positive ion mode or negative ion mode, and formic acid aqueous solution-formic acid acetonitrile (methanol) solution is used as mobile phase when adopting positive ion mode; when the negative ion mode is adopted, an ammonium formate aqueous solution (or directly adopting ammonia water diluted by water) -acetonitrile solution without formic acid is taken as a mobile phase. The invention adopts water (containing 0.1% formic acid) solution-acetonitrile (containing 0.1% formic acid) solution as mobile phase, has good positive ion mode response, and can meet the detection sensitivity, thus the analysis under the positive ion mode is selected. Performing primary mass spectrum full scanning on the target compound to obtain [ M+H ] of the target compound] + And (3) carrying out secondary scanning on the parent ions, optimizing voltage, selecting 2 sub-ions with strongest response, and optimizing collision energy when the sub-ions respond optimally in a multi-reaction monitoring mode (MRM) to obtain optimal mass spectrum conditions.
Example 2
Cosmetic samples containing 3 substances such as Cannabidiol (CBD), tetrahydrocannabinol (THC) and cannabidene (CBC) were tested by the test method of example 1. The total ion flow diagram (TIC) of Cannabidiol (CBD), tetrahydrocannabinol (THC) and cannabidene (CBC) is shown in fig. 1. Mass spectrum parameters of Cannabidiol (CBD), tetrahydrocannabinol (THC) and cannabidene (CBC) and parent and daughter ions are shown in Table 3.
TABLE 3 Mass Spectrometry parameters and qualitative and quantitative ion pairs for Cannabidiol (CBD), tetrahydrocannabinol (THC) and cannabidene (CBC)
Comparative example 1
Because the cosmetic matrix is complex, matrix effect can be generated when the liquid chromatography-mass spectrometer is used for detection, and potential influence is generated on the detection result of the to-be-detected object in the sample, different purification means are selected to perform pretreatment on the sample, so that the purification effects of different types of purification means are examined and a proper sample pretreatment method is selected. 3 kinds of facial masks, cream and water aqua without hemp component are selected as blank matrix of cosmetics. 3 parts of each blank matrix sample is weighed in parallel, placed in a 10mL colorimetric tube with a plug, added with 0.5mL of cannabidiol standard solution with the concentration of 1 mug/mL, fixed to 10mL by methanol, and subjected to high-speed oscillation on a vortex mixer for 30s to fully and uniformly mix the samples with an extraction solvent, subjected to ultrasonic extraction for 10min, and placed to the room temperature. The sample extracts were then treated by purifying with Shimadzu QuEChERS SPE purification tube and filtering, directly passing through 0.22 μm filter membrane without purification, LUMTECH MPFC-QuEChERS ultrafiltration column purification and filtering, waters Prime HLB column purification and filtering, waters QuEChERS SPE purification tube purification and filtering, and detection analysis was performed according to the following liquid conditions, and standard deviation and standard recovery rate were calculated, with the results shown in fig. 2.
Chromatographic conditions:
chromatographic column: cao CAPCELL CORE ADME column (2.1 mm. Times.100 mm,2.7 μm), mobile phase: 0.1% formic acid in water and 0.1% formic acid in acetonitrile, and performing gradient elution; the flow rate is 0.3mL/min, the sample injection amount is 5 mu L, and the column temperature is as follows: 40 ℃. The mobile phase and gradient elution procedure are shown in table 1.
Mass spectrometry conditions:
ion source: electrospray ion source positive ion mode (ESI) + ) The method comprises the steps of carrying out a first treatment on the surface of the Detection mode: multiple Reaction Monitoring (MRM) mode, atomizing air flow rate of 3L/min, drying air flow rate of 10L/min, heating air flow rate of 10L/min, interface temperature of 300 ℃ and interface voltage of 4.0kV. Mass spectrum parameters of cannabidiol and parent and child ions are shown in Table 2.
As can be seen from FIG. 2, the recovery rates of the pretreatment modes of the three samples, namely Shimadzu QuEChERS SPE purification column purification, LUMTECH MPFC-QuEChERS (high lipid) ultrafiltration purification column purification and Waters QuEChERS SPE purification tube purification, all meet the test requirements, but the standard deviation of the 3-time measurement results of the Shimadzu QuEChERS SPE purification tube purification and Waters QuEChERS SPE purification tube purification is larger. The analysis reasons are probably because the two purification modes need to adopt the operation of adding the sample solution into the purification tube and shaking the sample solution with force, the shaking force and the time influence the result, and the standard deviation is larger. The comprehensive analysis experiment results show that the ultrafiltration purifying column with LUMTECH MPFC-QuEChERS (high lipid) has the best purifying effect, and the recovery rate and repeatability meet the requirements, and can be used as the preferred method.
The foregoing is merely a preferred embodiment of the present invention and it should be noted that modifications and adaptations to those skilled in the art may be made without departing from the principles of the present invention, which are intended to be comprehended within the scope of the present invention.
Claims (4)
1. A method for detecting cannabidiol in cosmetics, which is characterized by comprising the following steps:
mixing the sample with an extraction solvent, and performing ultrasonic extraction to obtain an extraction solution; the extraction solvent is methanol; the ratio of the sample to the extraction solvent was 1 in g/mL: (5-15);
the temperature of ultrasonic extraction is 20-30 ℃, the power of ultrasonic extraction is 500-700W, and the time of ultrasonic extraction is 10-30 min;
adding the extracting solution into a purifying column for purifying and filtering to obtain target detection solution; the purifying column is an MPFC-QuEChERS high-lipid ultrafiltration purifying column;
analyzing and detecting the target detection liquid by adopting an ultra-high performance liquid chromatography-triple quaternary tandem mass spectrometry;
the chromatographic conditions of the ultra-high performance liquid chromatography-triple quaternary tandem mass spectrometry are as follows:
chromatographic column: cao CAPCELL CORE ADME chromatographic column, length 100mm, inner diameter 2.1mm, particle size 2.7 μm;
mobile phase: 0.05vt% -0.15 vt% formic acid aqueous solution and 0.05vt% -0.15 vt% formic acid acetonitrile solution;
the column temperature is 35-45 ℃; flow rate: 0.2-0.4 mL/min; the sample injection amount is 2-8 mu L;
the mass spectrometry conditions of the ultra-high performance liquid chromatography-triple quadrupole tandem mass spectrometry are as follows: the ionization mode is an electrospray ion source positive ion mode, multiple reaction monitoring mode signal acquisition is carried out, the atomization air flow is 2.5-3.5L/min, the drying air flow is 8-12L/min, the heating air flow is 8-12L/min, the interface temperature is 250-350 ℃, and the interface voltage is 3.0-5.0 kV;
the gradient elution procedure of the mobile phase is:
。
2. The method of claim 1, wherein the purification column is a LUMTECH MPFC-QuEChERS purification column.
3. The method of claim 1, wherein the filtering is by a microporous organic filter membrane.
4. The method according to claim 1, wherein the chromatographic conditions of the ultra performance liquid chromatography-triple quadrupole tandem mass spectrometry are:
mobile phase: 0.1% formic acid aqueous solution and 0.1% formic acid acetonitrile solution;
column temperature 40 ℃; flow rate: 0.3mL/min; the sample injection amount was 5. Mu.L.
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| 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 |
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| WO2016153347A1 (en) * | 2015-03-23 | 2016-09-29 | Echo Pharmaceuticals B.V. | Cannabidiol isolate from industrial-hemp and use thereof in pharmaceutical and/or cosmetic preparations |
| 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 |
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