CN112362798A - Detection method of cannabidiol in cosmetics - Google Patents
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Abstract
The invention relates to the technical field of cosmetic detection, in particular to a method for detecting cannabidiol in cosmetics. The detection method comprises the following steps: mixing a sample with an extraction solvent, and performing ultrasonic extraction to obtain an extracting solution; adding the extracting solution into a purifying column for purification, and filtering to obtain a target detection solution; the purifying column is an MPFC-QuEChERS high-fat ultrafiltration purifying column made of a nano composite material; and analyzing and detecting the target detection solution by adopting ultra-high performance liquid chromatography-triple quadrupole tandem mass spectrometry. The detection method realizes detection of cannabidiol in cosmetics, and has short analysis time and stable and reliable qualitative and quantitative detection result.
Description
Technical Field
The invention relates to the technical field of cosmetic detection, in particular to a method for detecting cannabidiol in cosmetics.
Background
Cannabis sativa (Cannabis sativa L., Hemp), also known as Hemp, etc., is an annual plant of Moraceae. According to the proportion of Tetrahydrocannabinol (THC) contained in cannabis, there are generally two categories, namely industrial cannabis and narcotic cannabis. The content of tetrahydrocannabinol in industrial hemp is not more than 0.3% at most, and the content of tetrahydrocannabinol in drug hemp is high. Cannabinoids (CBs) currently isolated from cannabis include Cannabidiol (CBD), tetrahydrocannabinol, Cannabinol (CBN), and cannabichromene (CBC). In recent years, the research on cannabidiol and cannabis extract has been rapidly developed, and a number of reports have been made. Cannabidiol is the main chemical component in industrial cannabis, and the use of industrial cannabis extracts as active ingredients or additives in the preparation of skin care products has created a trend. The skin care product has the effects of relieving pain, resisting inflammation, removing freckles, removing yellow, removing acnes, resisting aging, resisting wrinkles and the like, and can quickly cover the skin care product consumption market, particularly the European skin care product market.
At present, the analysis methods for determining the content of cannabidiol 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 mainly aims at the field of forensic or public security physical evidence identification of medicines, blood or hair and the like and the detection of 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) are listed as cosmetic raw materials which can be used in the catalogue of used cosmetic raw material names (2015 edition), while the technical specification of cosmetic safety (2015 edition) in China does not cover the detection and analysis method and does not show relevant national standards. The detection research of cannabidiol in cosmetics is carried out by fresh research institutions at home and abroad. Therefore, in order to effectively perform quality control and safety evaluation of cosmetics containing cannabis extract, it is necessary to establish a method for measuring the cannabidiol content in cosmetics. However, the cosmetic matrix is various and complex, and if the pretreatment is improper, the accurate detection of the cannabidiol is easily influenced.
Disclosure of Invention
In view of this, the present invention provides a method for detecting cannabidiol in cosmetics. The detection method realizes 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 detection method of cannabidiol in cosmetics, which comprises the following steps:
mixing a sample with an extraction solvent, and performing ultrasonic extraction to obtain an extracting solution;
adding the extracting solution into a purifying column for purification, and filtering to obtain a target detection solution; the purifying column is an MPFC-QuEChERS high-fat ultrafiltration purifying column made of a nano composite material;
and analyzing and detecting the target detection solution by adopting ultra-high performance liquid chromatography-triple quadrupole tandem mass spectrometry.
According to the invention, the complexity of the cosmetic matrix is considered to possibly cause matrix effect in the detection process of the ultra-high performance liquid chromatography-triple quadrupole tandem mass spectrometry, and potential influence is generated on the measurement result of the object to be measured in the sample, so that different purification means are selected for preprocessing the sample, the purification effects of different types of purification means are examined, and a suitable sample preprocessing method is selected. The invention is based on cosmetic samples, and 3 facial masks, creams and water aqua without hemp ingredients are selected as blank cosmetic matrixes due to the large difference of different cosmetic matrixes. The MPFC-QuEChERS ultrafiltration type purification column adopts a nano composite material, has large specific surface area, removes other macromolecular interferents in a matrix better than PSA, C18 and the like, has good extraction effect, and can ensure that the recovery rate of cannabidiol meets the requirement. The method applies the QuEChERS rapid sample pretreatment technology to the detection of cannabidiol in cosmetics for the first time, the pretreatment process is simple and rapid, the sample can be subjected to solvent extraction, and the sample can be subjected to on-machine detection after being rapidly purified by the purification column, so that the extraction and purification efficiency of the sample is improved, and the blank of the cannabidiol detection technology in cosmetics is made up.
MPFC is the abbreviation of multi-filtration clean-up, translated as a "multiple filtration column".
Preferably, the purification column is a LUMTECH MPFC-QuEChERS purification column. Purchased from Beijing Lvjin technologies, Inc.
Preferably, the extraction solvent is methanol.
Preferably, the ratio of the amount of sample to extraction solvent in g/mL is 1: (5-15).
Preferably, the ratio of sample to extraction solvent in g/mL is 1: 10.
according to some specific embodiments of the invention, the sample and the extraction solvent are mixed and then mixed uniformly for 30-60 seconds.
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 10 min.
Preferably, the filtration is by filtration through a microporous organic filter membrane.
Preferably, the microporous organic filter membrane is a 0.22 μm polytetrafluoroethylene filter membrane.
Preferably, the chromatographic conditions of the ultra-high performance liquid chromatography-triple quadrupole tandem mass spectrometry are as follows:
a chromatographic column: a Cao (3) \ 36921;
mobile phase: 0.05 to 0.15vt percent formic acid aqueous solution and 0.05 to 0.15vt percent 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.
Preferably, the chromatographic conditions of the ultra-high performance liquid chromatography-triple quadrupole tandem mass spectrometry are as follows:
mobile phase: 0.1% aqueous formic acid and 0.1% acetonitrile formic acid;
the column temperature is 40 ℃; flow rate: 0.3 mL/min; the sample size 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 spectrum 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, a multi-reaction monitoring mode signal is collected, the flow rate of atomizing gas is 2.5-3.5L/min, the flow rate of drying gas is 8-12L/min, the flow rate of heating gas 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 as follows: the ionization mode is an electrospray ion source positive ion mode, multi-reaction monitoring mode signal acquisition, the flow rate of atomizing gas is 3L/min, the flow rate of drying gas is 10L/min, the flow rate of heating gas is 10L/min, the interface temperature is 300 ℃, and the interface voltage is 4.0 kV.
The invention provides a method for detecting cannabidiol in cosmetics. The detection method comprises the following steps: mixing a sample with an extraction solvent, and performing ultrasonic extraction to obtain an extracting solution; adding the extracting solution into a purifying column for purification, and filtering to obtain a target detection solution; the purifying column is an MPFC-QuEChERS high-fat ultrafiltration purifying column made of a nano composite material; and analyzing and detecting the target detection solution by adopting ultra-high performance liquid chromatography-triple quadrupole tandem mass spectrometry. The invention has the beneficial effects that:
(1) the method fully considers the characteristics of diversity, complexity and the like of cosmetic matrixes, adopts the ultra-high performance liquid chromatography-triple quadrupole tandem mass spectrometry to detect the cannabidiol in the cosmetics for the first time 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 and screening monitoring of the cannabidiol in the cosmetics, and has wide application prospect. The blank of the detection method of the item is made up to a certain extent, the qualitative and quantitative analysis requirements of cannabidiol in the cosmetics can be met, and scientific basis and technical support are provided for safety supervision of related products of the cosmetics.
(2) The detection method provided by the invention has the advantages that the pretreatment process of the cosmetics is simple and rapid, the MPFC-QuEChERS rapid sample pretreatment technology is used for detecting cannabidiol in the cosmetics for the first time, the sample can be tested on a machine after being extracted by a solvent and rapidly purified by a purification column, the extraction and purification efficiency of the sample is improved, and the requirement on the operation technical level of an inspector is relatively low.
(3) The detection method has important significance for accurately identifying the cannabidiol component in the cosmetics. Considering that cannabinoids such as Cannabidiol (CBD), Tetrahydrocannabinol (THC), cannabichromene (CBC) are isomers of each other, interference may occur under different liquid phase separation conditions due to consistent retention times and having the same ion fragments (ion pairs). In the process of the invention, the retention behaviors of the 3 substances in the chromatographic column are researched, under the separation condition adopted by the invention, the 3 substances have different retention times, and the compound peak in the actual cosmetic sample is compared with the 3 compound peaks, so that whether cannabidiol is contained or not is identified, the mutual interference is eliminated, the effective separation is realized, and the false judgment of cannabidiol false positive or false negative is avoided. In addition, as the tetrahydrocannabinol not only belongs to the first class of controlled substances in the catalog of psychiatric and drug products of the people's republic of China (2013 edition), but also belongs to forbidden substances specified in the technical Specification for cosmetic safety (2015 edition), accurate identification of cosmetic samples containing or added with the tetrahydrocannabinol is of great significance for cosmetic quality safety supervision.
Drawings
Figure 1 total ion flow diagrams of Cannabidiol (CBD), Tetrahydrocannabinol (THC) and cannabichromene (CBC);
FIG. 2 shows the recovery of cannabidiol from 3 different base cosmetics measured under different purification unit conditions; wherein, a: shimadzu QuEChERS SPE purification tube; b: filtering with a microporous filter membrane only; c: LUMTECH MPFC-QuEChERS (high lipid) ultrafiltration type purification column; d: waters Prime HLB column; e: waters QuEChERS SPE purification column; m: facial mask; c: cream; a: a water aqua.
Detailed Description
The invention discloses a method for detecting cannabidiol in cosmetics, and a person skilled in the art can appropriately improve process parameters by referring to the content. It is expressly intended that all such similar substitutes and modifications which would be obvious to one skilled in the art are deemed to be included in the invention. While the methods and applications of this invention have been described in terms of preferred embodiments, it will be apparent to those of ordinary skill in the art that variations and modifications in the methods and applications described herein, as well as other suitable variations and combinations, may be made to implement and use the techniques of this invention without departing from the spirit and scope of the invention.
The reagents or instruments used in the method for detecting cannabidiol in cosmetics can be purchased from the market. The instrument used was as follows:
AL 204 analytical balance (mettlerlatolite, switzerland); vortex Genie 2 Vortex mixer (Scientific Industries, USA); KQ-3200DE ultrasonic cleaner (ultrasonic instruments Co., Ltd., Kunshan, Jiangsu).
The invention is further illustrated by the following examples:
example 1 detection of cannabidiol in cosmetic
Firstly, sample extraction
Accurately weighing 1g (accurate to 0.001g) of cosmetic sample, placing in a 10mL colorimetric tube with a plug, adding methanol to 10mL, and oscillating on a vortex mixer at high speed for 30s to fully mix the sample and the extraction solvent. Sealing, ultrasonic extracting for 10min, and standing to room temperature.
Secondly, sample purification
After the sample is kept stand to room temperature, the sample is purified by a LUMTECH MPFC-QuEChERS (high lipid) ultrafiltration type purification column (Beijing Lvyconfo science and technology Co., Ltd.), and is filtered by a 0.22 mu m polytetrafluoroethylene microporous membrane, and a subsequent filtrate is taken as a solution to be detected.
Because the cosmetic matrix is complex and the difference of different cosmetic matrixes is large, the invention selects 3 facial masks, creams and water aqua containing no hemp component as the blank cosmetic matrix and inspects the purifying effect of the sample by a sample adding and recovering method. Respectively adopting Shimadzu QuEChERS SPE purification tube to purify and filter, directly passing through a 0.22 mu m filter membrane without purification, LUMTECH MPFC-QuEChERS (high lipid) ultrafiltration type purification column to purify and filter, Waters Prime HLB column to purify and filter, and Waters QuEChERS SPE purification tube to purify and filter to process sample extract, and carrying out ultra-high performance liquid chromatography-tandem triple four-level rod mass spectrometry under the same conditions to calculate the standard recovery rate and standard deviation. The results show that: the pretreatment mode cannabidiol recovery rates of Shimadzu QuEChERS SPE purification column, LUMTECH MPFC-QuEChERS (high lipid) ultrafiltration type purification column and Waters QuEChERS SPE purification tube for purifying 3 samples all meet the test requirements, but the standard difference of 3 times of determination of the results of Shimadzu QuEChERS SPE purification tube purification and Waters QuEChERS SPE purification tube purification is larger. The LUMTECH MPFC-QuEChERS (high lipid) ultrafiltration type purification column has the best purification effect and meets the requirements on recovery rate and repeatability, and can be used as a preferred method.
Third, sample detection
The purified sample was subjected to ultra high performance liquid chromatography-triple quadrupole tandem mass spectrometry using LCMS-8060 ultra high performance liquid chromatography-tandem triple quadrupole mass spectrometer (shimadzu corporation, japan).
Chromatographic conditions are as follows:
a chromatographic column: cao (r) \ 36921: performing gradient elution on 0.1% formic acid water solution and 0.1% formic acid acetonitrile solution; flow rate 0.3mL/min, sample size 5. mu.L, column temperature: at 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% aqueous formic acid/%) | 0.1% formic acid acetonitrile solution/%) |
| 0 | 50 | 50 |
| 5 | 10 | 90 |
| 7 | 10 | 90 |
| 7.1 | 50 | 50 |
| 9 | 50 | 50 |
Mass spectrum conditions: an ion source: electrospray ion source positive ion mode (ESI)+) (ii) a Detection mode: and in a multi-reaction monitoring (MRM) mode, the flow rate of atomizing air is 3L/min, the flow rate of drying air is 10L/min, the flow rate of heating air is 10L/min, the interface temperature is 300 ℃, and the interface voltage is 4.0 kV. Mass spectrum parameters of cannabidiol and parent ion and daughter ion are shown in Table 2.
TABLE 2 Mass Spectrometry parameters and qualitative, quantitative ion pairs for Cannabidiol (CBD)
The liquid mass analysis of cannabinoid can adopt positive ion mode or negative ion mode, and adopts formic acid water solution-formic acid acetonitrile (methanol) solution as mobile phase in positive ion mode; when the anion mode is adopted, an ammonium formate aqueous solution (or ammonia water diluted by water directly) -acetonitrile solution without formic acid is used as a mobile phase. According to the invention, a water (containing 0.1% formic acid) solution-acetonitrile (containing 0.1% formic acid) solution is used as a mobile phase, the positive ion mode response is good, and the detection sensitivity can meet the requirement, so that the analysis is performed in the positive ion mode. Performing first-order mass spectrum full scan 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 to the optimum under a multi-reaction monitoring mode (MRM) to obtain the optimum mass spectrum condition.
Example 2
With reference to the detection method of example 1, a cosmetic sample containing 3 kinds of substances such as Cannabidiol (CBD), Tetrahydrocannabinol (THC), and cannabichromene (CBC) was detected. The total ion flow diagram (TIC) of Cannabidiol (CBD), Tetrahydrocannabinol (THC) and cannabichromene (CBC) is shown in figure 1. The mass spectral parameters and parent and daughter ions of Cannabidiol (CBD), Tetrahydrocannabinol (THC) and cannabichromene (CBC) are shown in table 3.
TABLE 3 Mass Spectrometry parameters and qualitative, quantitative ion-pairs for Cannabidiol (CBD), Tetrahydrocannabinol (THC) and cannabichromene (CBC)
Comparative example 1
Due to the fact that the cosmetic matrix is complex, matrix effect can be generated when the liquid chromatograph-mass spectrometer is used for detection, and potential influence is generated on the determination result of the object to be detected in the sample, different purification means are selected for preprocessing the sample, the purification effect of the different purification means is considered, and a proper sample preprocessing method is selected. 3 facial masks, creams and aqueous solutions without hemp are selected as blank cosmetic matrixes. Weighing 3 parts of each blank substrate sample in parallel, placing the blank substrate sample in a 10mL colorimetric tube with a plug, adding 0.5mL cannabidiol standard solution with the concentration of 1 mu g/mL, metering the volume to 10mL by using methanol, oscillating the mixture on a vortex mixer at high speed for 30s to fully mix the sample and the extraction solvent, performing ultrasonic extraction for 10min, and standing the mixture to room temperature. Then respectively adopting Shimadzu QuEChERS SPE purification tube to purify and filter, directly passing through a 0.22 mu m filter membrane without purification, LUMTECH MPFC-QuEChERS (high lipid) ultrafiltration type purification column to purify and filter, Waters Prime HLB column to purify and filter, and Waters QuEChERS SPE purification tube to purify and filter to process the sample extract, carrying out detection and analysis according to the following liquid quality conditions, calculating the standard recovery rate and standard deviation, and detailing the result is shown in figure 2.
Chromatographic conditions are as follows:
a chromatographic column: cao (r) \ 36921: performing gradient elution on 0.1% formic acid water solution and 0.1% formic acid acetonitrile solution; flow rate 0.3mL/min, sample size 5. mu.L, column temperature: at 40 ℃. The mobile phase and gradient elution procedure are shown in table 1.
Mass spectrum conditions:
an ion source: electrospray ion source positive ion mode (ESI)+) (ii) a Detection mode: multiple Reaction Monitoring (MRM) mode, atomizing air flow 3L/min, drying air flow 10L/min, heating air flow 10L/min, interface temperature 300 deg.C, interface voltage4.0 kV. Mass spectrum parameters of cannabidiol and parent ion and daughter ion are shown in Table 2.
As can be seen from FIG. 2, the recovery rates of the three sample pretreatment modes of Shimadzu QuEChERS SPE purification, LUMTECH MPFC-QuEChERS (high lipid) ultrafiltration purification and Waters QuEChERS SPE purification meet the test requirements, but the standard deviation of 3 times of determination of the results of Shimadzu QuEChERS SPE purification and Waters QuEChERS SPE purification is larger. The analysis reason may be that the two purification methods need to adopt an operation of adding the sample solution into the purification tube and shaking with force, and the shaking force and time affect the result, so that the standard deviation is larger. The comprehensive analysis experiment result shows that the LUMTECH MPFC-QuEChERS (high lipid) ultrafiltration type purification column has the best purification effect, meets the requirements on recovery rate and repeatability, and can be used as a preferred method.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. A detection method of cannabidiol in cosmetics is characterized by comprising the following steps:
mixing a sample with an extraction solvent, and performing ultrasonic extraction to obtain an extracting solution;
adding the extracting solution into a purifying column for purification, and filtering to obtain a target detection solution; the purification column is an MPFC-QuEChERS high-fat ultrafiltration type purification column;
and analyzing and detecting the target detection solution by adopting ultra-high performance liquid chromatography-triple quadrupole tandem mass spectrometry.
2. The assay of claim 1, wherein the purification column is a LUMTECH MPFC-queeches purification column.
3. The detection method according to claim 1, wherein the extraction solvent is methanol.
4. The detection method according to claim 3, wherein the amount ratio of the sample to the extraction solvent is 1: (5-15).
5. The detection method according to claim 1, wherein the temperature of the ultrasonic extraction is 20-30 ℃, the power of the ultrasonic extraction is 500-700W, and the time of the ultrasonic extraction is 10-30 min.
6. The detection method according to claim 1, wherein the filtration is a filtration through a microporous organic filtration membrane.
7. The detection method according to claim 1, wherein the chromatographic conditions of the ultra high performance liquid chromatography-triple quadrupole tandem mass spectrometry are as follows:
a chromatographic column: a Cao (3) \ 36921;
mobile phase: 0.05 to 0.15vt percent formic acid aqueous solution and 0.05 to 0.15vt percent 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.
8. The detection method according to claim 7, wherein the chromatographic conditions of the ultra high performance liquid chromatography-triple quadrupole tandem mass spectrometry are as follows:
mobile phase: 0.1% aqueous formic acid and 0.1% acetonitrile formic acid;
the column temperature is 40 ℃; flow rate: 0.3 mL/min; the sample size was 5. mu.L.
9. The detection method according to claim 7, wherein the gradient elution procedure of the mobile phase is:
。
10. The detection method according to any one of claims 1 to 9, wherein 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, a multi-reaction monitoring mode signal is collected, the flow rate of atomizing gas is 2.5-3.5L/min, the flow rate of drying gas is 8-12L/min, the flow rate of heating gas is 8-12L/min, the interface temperature is 250-350 ℃, and the interface voltage is 3.0-5.0 kV.
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