CN114942239B - Composition, kit and method for rapidly detecting synthetic cannabinoid in tobacco tar - Google Patents
Composition, kit and method for rapidly detecting synthetic cannabinoid in tobacco tar Download PDFInfo
- Publication number
- CN114942239B CN114942239B CN202210490403.3A CN202210490403A CN114942239B CN 114942239 B CN114942239 B CN 114942239B CN 202210490403 A CN202210490403 A CN 202210490403A CN 114942239 B CN114942239 B CN 114942239B
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- tobacco tar
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- 229930003827 cannabinoid Natural products 0.000 title claims abstract description 75
- 239000003557 cannabinoid Substances 0.000 title claims abstract description 75
- 241000208125 Nicotiana Species 0.000 title claims abstract description 74
- 235000002637 Nicotiana tabacum Nutrition 0.000 title claims abstract description 74
- 238000000034 method Methods 0.000 title claims abstract description 36
- 239000000203 mixture Substances 0.000 title abstract description 19
- 238000001514 detection method Methods 0.000 claims abstract description 48
- 238000001069 Raman spectroscopy Methods 0.000 claims abstract description 40
- 239000000701 coagulant Substances 0.000 claims abstract description 34
- 239000000463 material Substances 0.000 claims abstract description 25
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 13
- 238000002156 mixing Methods 0.000 claims abstract description 8
- NLKNQRATVPKPDG-UHFFFAOYSA-M potassium iodide Chemical compound [K+].[I-] NLKNQRATVPKPDG-UHFFFAOYSA-M 0.000 claims description 66
- 229940065144 cannabinoids Drugs 0.000 claims description 42
- BLQJIBCZHWBKSL-UHFFFAOYSA-L magnesium iodide Chemical compound [Mg+2].[I-].[I-] BLQJIBCZHWBKSL-UHFFFAOYSA-L 0.000 claims description 23
- 229910001641 magnesium iodide Inorganic materials 0.000 claims description 23
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 16
- 239000012498 ultrapure water Substances 0.000 claims description 16
- 239000000084 colloidal system Substances 0.000 claims description 8
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 7
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- -1 5F-ADBINACA Chemical compound 0.000 claims description 4
- GPWADXHYJAZPAX-OAHLLOKOSA-N N-[(2S)-1-amino-3,3-dimethyl-1-oxobutan-2-yl]-1-butylindazole-3-carboxamide Chemical compound NC([C@H](C(C)(C)C)NC(=O)C1=NN(C2=CC=CC=C12)CCCC)=O GPWADXHYJAZPAX-OAHLLOKOSA-N 0.000 claims description 4
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- PALJPGHWDUHUPO-UHFFFAOYSA-N jwh-019 Chemical compound C12=CC=CC=C2N(CCCCCC)C=C1C(=O)C1=CC=CC2=CC=CC=C12 PALJPGHWDUHUPO-UHFFFAOYSA-N 0.000 claims description 4
- CHSUEEBESACQDV-GOSISDBHSA-N methyl (2S)-2-[[1-(5-fluoropentyl)indole-3-carbonyl]amino]-3,3-dimethylbutanoate Chemical compound FCCCCCN1C=C(C2=CC=CC=C12)C(=O)N[C@H](C(=O)OC)C(C)(C)C CHSUEEBESACQDV-GOSISDBHSA-N 0.000 claims description 4
- VCHHHSMPMLNVGS-UHFFFAOYSA-N 1-Butyl-3-(1-naphthoyl)indole Chemical compound C12=CC=CC=C2N(CCCC)C=C1C(=O)C1=CC=CC2=CC=CC=C12 VCHHHSMPMLNVGS-UHFFFAOYSA-N 0.000 claims description 3
- VREQTLWJHFQLEX-UHFFFAOYSA-N [1-[(4-fluorophenyl)methyl]indol-3-yl]-naphthalen-1-ylmethanone Chemical compound FC1=CC=C(CN2C=C(C3=CC=CC=C23)C(=O)C2=CC=CC3=CC=CC=C23)C=C1 VREQTLWJHFQLEX-UHFFFAOYSA-N 0.000 claims description 3
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- LWOCBHBFWNGPGM-QGZVFWFLSA-N methyl (2S)-3,3-dimethyl-2-[(1-pent-4-enylindazole-3-carbonyl)amino]butanoate Chemical compound CC([C@@H](C(=O)OC)NC(=O)C1=NN(C2=CC=CC=C12)CCCC=C)(C)C LWOCBHBFWNGPGM-QGZVFWFLSA-N 0.000 claims description 3
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- ROHVURVXAOMRJY-UHFFFAOYSA-N 1h-indole-3-carboxylic acid, 1-[(4-fluorophenyl)methyl]-, 8-quinolinyl ester Chemical compound C1=CC(F)=CC=C1CN1C2=CC=CC=C2C(C(=O)OC=2C3=NC=CC=C3C=CC=2)=C1 ROHVURVXAOMRJY-UHFFFAOYSA-N 0.000 claims description 2
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- WCBYXIBEPFZUBG-HNNXBMFYSA-N N-[(2S)-1-amino-3-methyl-1-oxobutan-2-yl]-1-(5-fluoropentyl)indazole-3-carboxamide Chemical compound NC([C@H](C(C)C)NC(=O)C1=NN(C2=CC=CC=C12)CCCCCF)=O WCBYXIBEPFZUBG-HNNXBMFYSA-N 0.000 claims description 2
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- PXLDPUUMIHVLEC-UHFFFAOYSA-N [1-(5-fluoropentyl)indol-3-yl]-(2,2,3,3-tetramethylcyclopropyl)methanone Chemical compound CC1(C)C(C)(C)C1C(=O)C1=CN(CCCCCF)C2=CC=CC=C12 PXLDPUUMIHVLEC-UHFFFAOYSA-N 0.000 claims description 2
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Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/65—Raman scattering
- G01N21/658—Raman scattering enhancement Raman, e.g. surface plasmons
Landscapes
- Health & Medical Sciences (AREA)
- Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
- Physics & Mathematics (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
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Abstract
The application discloses a composition, a kit and a method for rapidly detecting synthetic cannabinoid in tobacco tar. The method for rapidly detecting the synthetic cannabinoid in tobacco tar comprises the following steps: pretreating tobacco tar by using a tobacco tar extracting agent to obtain a sample to be detected; mixing the sample to be detected with a coagulant and a nano reinforced base material to form a mixed system to be detected; detecting the mixed system to be detected by a Raman spectrometer; the nano-reinforced base material includes metal nano-particles and the coagulant includes iodinated salt. By using the composition and the method, the convenient, rapid and accurate identification of the synthesized cannabinoid in the tobacco tar can be realized by the SERS technology, and the minimum detection concentration of the synthesized cannabinoid in the tobacco tar can reach 10 mug/mL.
Description
Technical Field
The application relates to a detection method of synthetic cannabinoid, in particular to a composition, a kit and a method for rapidly detecting the synthetic cannabinoid in tobacco tar, and belongs to the technical field of analytical chemistry.
Background
The synthesized cannabinoid is an artificially synthesized compound with the function of phytotoxicity cannabis, and belongs to one of novel mental active substances. In recent years, the harm and abuse of synthetic cannabinoids have attracted widespread social concern, criminals often blend the synthetic cannabinoids into e-cigarette oils for high price vending, and such common-looking e-cigarettes can create illusions for smokers, and the smokers are generally biased towards teenagers, so that the social harm is extremely great. The methods for detecting and synthesizing cannabinoid commonly used at present are gas chromatography-mass spectrometry, colloidal gold immunochromatography and the like. The gas phase/liquid phase-mass spectrometry cannot be used for on-site rapid screening due to the reasons of heavy equipment, complex operation, long time consumption and the like, and the case breaking time is prolonged. The colloidal gold immunochromatography has the disadvantages of high false positive rate, high single detection price, and incapability of carrying out specificity and more accurate identification because the positive result only indicates that one or more of the synthetic cannabinoids are contained. To date, there is no rapid and effective assay available on the market for the on-site identification of synthetic cannabinoids.
On the other hand, portable spectroscopic techniques such as infrared spectroscopy and raman spectroscopy are currently the first methods of synthesizing cannabinoids for rapid mobile on-site analysis, as they enable non-destructive identification of species through fingerprint spectroscopy. However, due to the interference of substrates such as glycerin, pigment and perfume in tobacco tar and the strong fluorescence interference of samples, the conventional raman spectrum cannot directly detect trace synthetic cannabinoids in the electronic tobacco tar, and needs to be realized by a surface enhanced raman spectrum scattering (SERS) technology. The key realization of the technology is as follows: firstly, establishing a SERS method of a synthetic cannabinoid standard substance, effectively combining a tested sample with a nano enhanced substrate by adding a proper coagulant, and then carrying out Raman detection by using a Raman spectrometer; secondly, the high viscosity property of the electronic cigarette oil prevents the synthetic cannabinoid from being adsorbed on the nano enhanced substrate, and different pigments and spice compounds generate SERS signals, so that the cigarette oil needs to be simply treated to obtain a better detection result. At present, there are some scientific reports about SERS analysis of synthetic cannabinoids abroad, but the types of the synthetic cannabinoids which can be analyzed are limited, and most of the synthetic cannabinoids are named as JWH, so that the defects of low sensitivity, narrow application range and the like exist, and the SERS detection technology of the synthetic cannabinoids cannot be really commercialized.
Disclosure of Invention
The main object of the present application is to provide a composition, a kit and a method for rapid detection of synthetic cannabinoids in tobacco tar, which overcomes the deficiencies of the prior art.
In order to achieve the above purpose, the present application provides the following technical solutions.
One aspect of the present application provides a composition for rapid detection of synthetic cannabinoids in tobacco tar, comprising metal nanoparticles, iodinated salts, and the like, and may further comprise a tobacco tar extractant.
In another aspect, the present application also provides a kit comprising the composition for rapid detection of synthetic cannabinoids in tobacco tar
Yet another aspect of the present application provides a method for rapid detection of synthetic cannabinoids in tobacco tar comprising:
pretreating tobacco tar by using a tobacco tar extracting agent to obtain a sample to be detected;
mixing the sample to be detected with a coagulant and a nano reinforced base material to form a mixed system to be detected; and
detecting the mixed system to be detected by a Raman spectrometer;
wherein the nano-reinforced base material comprises metal nano-particles and the coagulant comprises iodinated salt.
Compared with the prior art, the composition disclosed by the application is matched with a portable Raman spectrometer, so that the convenient, rapid and accurate identification of the synthesized cannabinoid in the tobacco tar can be realized through the SERS technology, and the minimum detection concentration of the synthesized cannabinoid in the tobacco tar can reach 10 mug/mL.
Drawings
Fig. 1 is a flow chart of a method for rapid detection of synthetic cannabinoids in tobacco tar in an exemplary embodiment of the present application.
FIG. 2 shows SERS spectra of examples 1 to 3 and comparative examples 1 to 2 of the present invention.
FIG. 3A shows SERS spectra of a 5F-ADBICA standard solution at a concentration of 10 μg/mL with two iodinated salts and a single iodinated salt in an embodiment of the invention.
FIG. 3B shows a SERS spectrum of a 5F-ADBICA standard solution at a concentration of 1 μg/mL with two iodinated salts and a single iodinated salt in an embodiment of the invention.
FIGS. 4A-4G show SERS spectra of 35 synthetic cannabinoid standard samples, respectively.
Detailed Description
In view of the shortcomings of the prior art, the applicant has provided the technical scheme of the application through long-term research and practice, which mainly uses common gold or silver nano colloid as a reinforced substrate and uses iodized salt solution as a coagulant to realize the rapid detection of various micro-synthetic cannabinoids in tobacco tar by combining with simple tobacco tar pretreatment. The technical scheme of the present application will be described in detail as follows.
In the present application, the term "comprising" as referred to herein means open, but does not exclude closed forms, if not specified. For example, the term "comprising" may mean that other components not listed may also be included, or that only listed components may be included.
Some embodiments of the present application provide a composition for rapid detection of synthetic cannabinoids in tobacco tar comprising a nanoreinforced substrate material and a coagulant; the nano-reinforced base material includes metal nano-particles and the coagulant includes iodinated salt.
In one embodiment, the composition further comprises a tobacco tar extractant. Wherein the tobacco tar extractant includes ultrapure water, ethanol aqueous solution, methanol aqueous solution, etc., and is not limited thereto.
In one embodiment, the iodinated salt includes one or more of sodium iodide, potassium iodide, magnesium iodide, and combinations thereof, and is not limited thereto.
More preferably, the iodinated salt includes potassium iodide and magnesium iodide.
More preferably, the molar ratio of the potassium iodide to the magnesium iodide is 1:5-5:1.
In one embodiment, the metal nanoparticles may be any one or a combination of gold, silver, and copper, for example, gold nanoparticles, silver nanoparticles, gold-silver alloy nanoparticles, and the like, and are not limited thereto.
Preferably, the nano reinforced substrate material comprises gold or silver nano colloid with a particle size of 30-100nm. The metal nano-gel can be purchased conveniently from commercial sources or can be synthesized easily by referring to the known process, is storage-resistant and has good adaptability to severe environments, so that the detection method matched with the metal nano-gel has the advantages of convenience and low cost in implementation, and can well meet the requirements of actual operation on site.
Some embodiments of the present application provide a kit comprising the composition.
In one embodiment, in the kit, the nano-enhancing base material, the coalescing agent and the tobacco tar extraction agent are packaged independently of one another.
In one embodiment, the tobacco tar extracting agent is 1-10 milliliters of aqueous solution, and the dilution multiple of the tobacco tar is ensured to be 10-1000 times only by changing the amount of the added tobacco tar.
In one embodiment, the coagulant is preferably a mixed iodinated salt of potassium iodide and magnesium iodide, pre-formulated as a mixed aqueous solution, the two iodinated salts preferably having 1: 5-5: 1, wherein the concentration of any one of the above compounds is 0.1mol/L to 1mol/L. The nano reinforced substrate material is in the form of a hydrocolloid, and can be directly used after self-made or purchased.
The kit is very simple and convenient when using, the pretreatment and surface enhancement processes of the tobacco tar sample can be completed only by very simple and convenient mixing and manual vibration steps, the accurate detection of the cannabinoid synthesized in the tobacco tar can be completed in one minute through Raman spectrum testing, and the on-site rapid detection can be realized by matching with a portable Raman spectrometer.
Some embodiments of the present application provide a method for rapid detection of synthetic cannabinoids in tobacco tar comprising:
pretreating tobacco tar by using a tobacco tar extracting agent to obtain a sample to be detected;
mixing the sample to be detected with a coagulant and a nano reinforced base material to form a mixed system to be detected; and
detecting the mixed system to be detected by a Raman spectrometer;
wherein the nano-reinforced base material comprises metal nano-particles and the coagulant comprises iodinated salt.
In one embodiment, the tobacco tar may be pre-treated by mixing a tobacco tar extractant with the tobacco tar to obtain a sample to be tested. The main components of the electronic cigarette oil are additives such as glycerol, propylene glycol, nicotine, essence, pigment and the like, and the components can generate interference Raman signals and even generate strong fluorescent background. Normally, the SERS method can directly detect low-content synthetic cannabinoids, but trace amounts of synthetic cannabinoids in tobacco tar cannot directly obtain SERS signals through the nano-enhanced substrate, and because the oiliness and high viscosity of electronic tobacco tar prevent the adsorption and aggregation of synthetic cannabinoid molecules and the nano-enhanced substrate material, pretreatment of tobacco tar is needed first. In the application, the methanol aqueous solution, the ethanol aqueous solution, the ultrapure water and the like are selected as the extracting agents, so that good extraction effects can be obtained. For the purpose of convenient use by law enforcement personnel on site, a nontoxic, nonflammable, portable solvent is preferably employed, so that the tobacco tar extractant is optimally selected from ultrapure water. The adoption of water as the extractant means that the electronic cigarette oil is greatly diluted, so that the oiliness and high viscosity of a cigarette oil matrix are eliminated, and the concentration of additives such as pigments and the like which cannot detect signals is reduced. In the pretreatment step in the present application, the dilution factor of the tobacco tar extraction agent to the tobacco tar may be set to 10 to 1000 times, and optimally, the dilution factor is 100 times.
In one embodiment, the method for rapid detection of synthetic cannabinoids in tobacco tar specifically comprises: and sequentially adding a coagulant and a nano reinforced base material into the sample to be detected, and uniformly mixing to form the mixed system to be detected.
With such a material mixing sequence, optimal SERS sensitivity can be obtained, for example, with the method of the present application having a minimum detection concentration of 100ng/mL for a standard solution of synthetic cannabinoid and a minimum detection concentration of 10 μg/mL for synthetic cannabinoid in tobacco tar.
In one embodiment, the volume ratio of the sample to be detected and the coagulant in the mixed system to be detected is 1:1-10:1.
In one embodiment, the volume ratio of the sample to be detected and the nano reinforced substrate material in the mixed system to be detected is 1:1-10:1.
In one embodiment, the tobacco tar extractant includes ultrapure water, an aqueous ethanol solution, an aqueous methanol solution, or the like, and is not limited thereto.
In one embodiment, the iodinated salt includes one or more of sodium iodide, potassium iodide, magnesium iodide, and combinations thereof, and is not limited thereto. In the prior art, in order to obtain the best SERS enhancement effect, a chloride salt is generally added to a metal nanoparticle solution, which has the effect of effectively aggregating metal nanoparticles and a substance to be detected to generate a "hot spot" effect, so that the raman signal method of the substance to be detected is millions times. However, the inventors of the present application found after a lot of experiments that strong raman signals could not be obtained with chloride salts such as sodium chloride, magnesium chloride, potassium chloride, etc. After extensive research and experimentation, the inventors of the present application have found that iodinated salts can act to amplify raman signals. It is particularly surprising that when a mixture of two iodinated salts is used as the coagulant, a further enhancement of the raman signal is found, and the detection result obtained is far better than that obtained when a single iodinated salt is used, and specifically may include any combination of two of sodium iodide, potassium iodide, magnesium iodide. Preferably, the coagulant is a mixture of potassium iodide and magnesium iodide, in particular a mixed solution of the potassium iodide and the magnesium iodide, wherein the molar ratio of the potassium iodide to the magnesium iodide is 1:5-5:1; the concentration of potassium iodide ranges from 0.1 mol/liter to 1 mol/liter. Under such conditions, the method of the present application provides a minimum detection concentration of 100ng/mL for the synthetic cannabinoid standard solution and a minimum detection concentration of 10 μg/mL for the synthetic cannabinoid in tobacco tar.
Further, the nano-reinforced substrate material may be selected from nano-colloids with a valence of 0, such as gold, silver, copper or alloys thereof, or mixtures thereof, and most preferably gold nano-colloids or silver nano-colloids are used. The average particle size of the metal nano colloid is 30-100nm. The synthesis methods of these metal nanocolloids are known in the art, and for example, noble metal nanocolloids can be prepared by performing redox reactions with noble metal salts (e.g., chloroauric acid, silver nitrate, etc.) and reducing agents (e.g., trisodium citrate, ascorbic acid, etc.), and the particle size of the product can be adjusted by controlling the reaction conditions. These noble metal nanocolloids generally have good dispersibility and stability, can be stably stored without contamination, and have a shelf life of over twelve months. The metal nanocomposites can be purchased from commercial sources very conveniently or can be synthesized very easily with reference to known processes, so that the method of the present application has the advantage of being convenient and low cost to implement.
Synthetic cannabinoids are known in a wide variety of forms, but they can be broadly assigned to the following seven structural formulas:
wherein R1 represents a substituted or unsubstituted C 3 -C 8 A hydrocarbon group; a substituted or unsubstituted heterocyclic ring containing 1 to 3 heteroatoms; substituted or unsubstituted heterocyclyl-substituted methyl or ethyl groups containing 1 to 3 heteroatoms. R2 represents hydrogen or methyl or no atom. R3 represents a substituted or unsubstituted C 6 -C 10 Aryl of (a); substituted or unsubstituted C 3 -C 10 Is a hydrocarbon group of (2); a substituted or unsubstituted heterocyclic group containing 1 to 3 hetero atoms; substituted or unsubstituted heterocycle-substituted methyl or ethyl containing 1 to 3 heteroatoms. R4 represents hydrogen; a substituted or unsubstituted phenyl group; substituted or unsubstituted benzyl. R5 represents a substituted or unsubstituted C 3 -C 10 Is a hydrocarbon group of (a). X represents N or C. Y represents N or CH. Z represents O or NH or no atom.
Synthetic cannabinoids conforming to the seven structural formulas above are all the detection objects of the present application.
Further, the detection method of the present application has good detection results for the following 35 kinds of synthetic cannabinoids, such as 4F-MDMB-BUTICA, 5F-MDMB-PICA, 5F-ADBICA, ADB-BUTINACA, MDMB-4en-PINACA, AM-694, FUB-JWH-018, FUB-PB-22, 5F-UR-144, MAM-2201, EAM-2201, 5F-PB-22, JWH-019, UR-144, JWH-122, JWH-081, RCS-4, PB-22, AB-CHMINACA, AB-FUBINACA, 5F-AB-PINACA, STS-135, APINACA, MDMB-CHMICA, MDF-FUBINACA, 5F-AMB, AMB-FUBINACA, JWH-018, JWH-3, JWH-203, JWH-307, JWH-250, etc. Of course, the detection method of the present application is not limited to the 35 kinds of synthetic cannabinoids, and the detection limit for standard solutions of these synthetic cannabinoids can be as low as 100ng/mL (for example, JWH series, JWH-073/JWH-019/JWH-018/JWH-081, etc.), but is usually in the range of 1 to 10. Mu.g/mL.
In one embodiment, the raman spectrometer may be a bench-top raman spectrometer or a portable raman spectrometer or the like. The excitation wavelength of the raman spectrometer may be 532nm, 633nm, 785nm, 1064nm, etc., and is not limited thereto. Generally any raman spectrometer may be used in the detection method of the present application. For the purpose of use in drug sites and the like, the application preferably uses a portable raman spectrometer for raman detection. Such as, but not limited to, portable raman spectrometers produced by sameidie technology (Thermo Fisher Scientific).
The method can rapidly and qualitatively analyze at least 35 kinds of synthesized cannabinoids in tobacco tar based on a Raman spectrum technology, and overcomes the defect that trace synthesized cannabinoids in tobacco tar cannot be directly detected in the prior art.
For example, referring to fig. 1, a method for detecting synthetic cannabinoids in tobacco tar using SERS technology in the present application may include pretreatment of tobacco tar, SERS treatment, and portable raman spectrometer detection.
In a more specific embodiment, a method for rapid detection of synthetic cannabinoids in tobacco tar specifically comprises the steps of:
(1) And adding a certain amount (for example, 10 mu L) of tobacco tar into a certain amount (for example, 1 mL) of tobacco tar extracting agent, and uniformly shaking to obtain a sample to be detected. Wherein the tobacco tar extracting agent is 18MΩ·cm ultrapure water, ethanol water solution or methanol water solution. The extraction process is simple, but the problems of high viscosity of tobacco tar and interference of other impurities during SERS test can be effectively solved.
(2) And sequentially adding a proper amount of coagulant and nano reinforced base material into the sample to be detected, and vibrating uniformly to obtain a mixed system to be detected. For example, wherein the volume ratio of the sample to be tested and the coagulant is between 1:1 and 10:1, and the volume ratio of the sample to be tested and the nano-reinforced base material is between 1:1 and 10:1.
(3) And placing the mixed system to be detected into a detection chamber of a Raman spectrometer, enabling monochromatic laser (for example, with the wavelength of about 785 nm) to irradiate on a sample, and receiving Raman scattered light of the mixed system to be detected by a detector to obtain a Raman spectrogram with clear synthetic cannabinoid characteristic peaks.
(4) Before the steps (1) - (3), adding SERS spectrograms of a plurality of (for example, the 35 types of) micro-synthetic cannabinoid standard solutions into a portable Raman spectrometer in the form of a spectrum database, automatically comparing and analyzing the Raman spectrum of the mixed system to be detected obtained in the step (3) with a pre-stored spectrum database, and if the Raman frequency shift value of the mixed system to be detected is the same as the Raman frequency shift value of one type of synthetic cannabinoid in the database, identifying that the synthetic cannabinoid exists in the tobacco tar.
By using the method provided by the embodiment, the synthetic cannabinoid in tobacco tar can be rapidly identified in environments such as an anti-drug site and the like, thereby being beneficial to accelerating case detection.
The present application will be described in further detail with reference to specific examples, but the scope of the present application is not limited to these specific examples. Unless otherwise indicated, all materials used in the examples below were available commercially or were self-contained in the literature, and the production equipment, test methods, etc. used may be any equipment or method known in the art.
The method for detecting synthetic cannabinoids provided in examples 1-3 comprises: A5F-ADBICA standard solution (hereinafter simply referred to as "original sample") having a concentration of 10. Mu.g/mL was subjected to a nano-substrate enhancement treatment using a coagulant, and then detected using a portable Raman spectrometer.
The method for detecting synthetic cannabinoids provided in comparative example 1 is substantially the same as in example 2, except that: the coagulant used is potassium chloride solution.
Comparative example 2 was a blank group as example 1, in which the object to be detected was ultrapure water, and the rest was the same as example 1.
The compositions of the coagulants used in examples 1 to 3 and comparative examples 1 to 2 are shown in Table 1.
Specifically, in examples 1 to 3 and comparative example 1, the original sample was obtained by diluting the mother liquor with ultrapure water. The mother liquor is a 5F-ADBICA standard solution with the concentration of 1000 mug/mL, wherein methanol is used as a solvent.
In the method for detecting synthetic cannabinoids provided in examples 1-3 and comparative example 1, 200. Mu.l of the original sample was added to a 4 ml glass bottle used in combination with a portable Raman spectrometer (Siemens technology), then 50. Mu.l of a coagulant and 50. Mu.l of spherical silver nano-colloid (average particle size: about 55 nm) were sequentially added to the glass bottle, and the mixture was mixed by shaking manually for two seconds, and then the glass bottle was put into the portable Raman spectrometer for detection, and the obtained Raman spectra were shown in FIG. 2.
TABLE 1 formulations of coagulants in examples 1-3 and comparative examples 1-2
It can be seen from examples 1-3 and comparative examples 1-2 that the use of different coagulants resulted in different SERS enhancements. As can be seen from the SERS spectra of the sample group (i.e., example 1-example 3) and the blank group (i.e., comparative example 2) in FIG. 2, the Raman characteristic peaks of the 5F-ADBICA standard solution are found to be 770, 1339 and 1535cm- 1 Is a position of (c). The proper coagulant type and concentration can be selected according to the existence and the intensity of the Raman characteristic peakDegree.
In general, in order to obtain SERS enhancement effect, a chloride salt was added to the metal nanoparticle solution, so in comparative example 1, potassium chloride was attempted to be added, but no raman signal was found, indicating that the chloride salt did not act to aggregate the analyte and the nano-metal particles.
With continued reference to FIG. 2, either potassium iodide or magnesium iodide alone produced a Raman characteristic peak in 5F-ADBICA as compared to potassium chloride, indicating that a single iodide salt may act as a coacervation.
Further, referring to fig. 2 again, it can be seen that the mixed solution of magnesium iodide and potassium iodide is used as the coagulant, and the signal of the corresponding raman characteristic peak is significantly enhanced.
Therefore, in the detection methods of examples 1 to 3, the optimal coagulant is a mixed solution of two iodinated salts, and the concentration of potassium iodide is 0.5mol/L and the concentration of magnesium iodide is 0.2mol/L, so that the strongest Raman peak signal can be obtained.
In particular, referring to FIG. 3A, it can be seen that the SERS signal intensity of 10. Mu.g/mL 5F-ADBICA at the same concentration is compared on the same axis from the strongest characteristic peak (1339 cm- 1 ) In this regard, the peak intensity of the mixed solution of potassium iodide and magnesium iodide (potassium iodide, magnesium iodide concentration: u0.5mol/L, 0.2mol/L, respectively) used as the coagulant was about twice that of the magnesium iodide solution (concentration: 0.2 mol/L), three times that of the potassium iodide solution (concentration: 0.5 mol/L), and therefore the effect of using both of the iodine salts at the same time was significantly superior to that of using one of the iodine salts.
Example 4a method of detecting synthetic cannabinoids comprising: referring to example 1, a 5F-ADBICA standard solution (hereinafter, simply referred to as "original sample") having a concentration of 1. Mu.g/mL was subjected to a nano-substrate enhancement treatment using a coagulant, and then detected using a portable Raman spectrometer. Wherein the coagulant adopted is respectively a mixed solution of potassium iodide and magnesium iodide (the concentration of the potassium iodide and the concentration of the magnesium iodide are respectively 0.5mol/L and 0.2 mol/L), a magnesium iodide solution (the concentration of the magnesium iodide is 0.2 mol/L) and a potassium iodide solution (the concentration of the magnesium iodide is 0.5 mol/L).
Referring to FIG. 3B, SERS signal intensities of 1 μg/mL5F-ADBICA at the same concentration are compared fromThe strongest characteristic peak (1339 cm) 1 ) In this regard, when a mixed solution of potassium iodide and magnesium iodide was used as the coagulant at the same time, there was a distinct characteristic peak, whereas when either magnesium iodide or potassium iodide was used alone, there was no characteristic peak, and a signal was substantially blank, so that the detection limit could not be 1. Mu.g/mL with single iodide salt.
Example 5 this example is a nano-substrate enhancement of a standard solution of 35 synthetic cannabinoids using the method of example 1, followed by testing using a portable raman spectrometer and establishing a spectral database, resulting in SERS spectra as shown in fig. 4A-4G. From SERS maps of different synthetic cannabinoids, it can be seen that although the structures of the partially synthesized cannabinoids are similar, minor differences in their structures can result in differences in the characteristic peak positions. Such as FUB-JWH-018 in which the former substituent is 4-fluorobenzyl and JWH-018 in which the latter substituent is pentyl, resulting in a wave number of 848cm- 1 The characteristic peaks at the positions are different, so that the difference is easy to distinguish. However, some synthetic cannabinoids are indistinguishable because the substituents are alkanes of similar structure, such as JWH-019, JWH-073 and JWH-018, and the substituents are hexyl, butyl and pentyl groups, respectively, so the SERS spectra are nearly identical and indistinguishable. For the drug-taking site, if indistinguishable synthetic cannabinoids are found, the drug-taking site can be further sent to a laboratory for detection, and SERS detection is used as a rapid detection means to rapidly screen which type of synthetic cannabinoids is beneficial to drug-taking work.
Example 6 this example is a method according to example 1, in which tobacco tar actually obtained by illegally adding synthetic cannabinoid is detected. The results of the detection of these real samples are shown in Table 2. Because the oiliness and high viscosity of the e-tar can prevent the adsorption and aggregation of the synthesized cannabinoid molecules and the nano-reinforced substrate material, the tar needs to be pretreated first, and in this embodiment, an aqueous methanol solution, an aqueous ethanol solution and ultrapure water are selected as the tar extractant, and all the three extractants are found to have good extraction effects. Ultrapure water is preferred as the tobacco tar extractant for ease of use by law enforcement personnel on site. The electronic cigarette oil can be diluted greatly by adopting water as the cigarette oil extracting agent, so that the oiliness and high viscosity of a cigarette oil matrix are eliminated, and the concentration of additives such as pigment is reduced to be undetectable. The dilution factor may be 10 to 1000 times, with an optimal dilution factor of 100 times.
TABLE 2 tobacco tar pretreatment method and test results in example 5
Sample of | Tobacco tar is short for | Tobacco tar pretreatment method | Detection result |
Real sample 767-1 | MDMB-4en-PINACA | Ultrapure water; diluted 10 times | Detecting; matching |
Real sample 767-2 | MDMB-4en-P1NACA | Ultrapure water; diluted 10 times | Detecting; matching |
True sample (Red) | ADB-BUTINACA | Ultrapure water; diluted 100 times | Detecting; matching |
Real sample (Green) | ADB-BUTINACA | UltrapureWater; diluted 100 times | Detecting; matching |
True sample (Red bean flavor) | 5F-MDMB-PICA | Ultrapure water; diluted 100 times | Detecting; matching |
True sample (mung bean flavor) | 5F-MDMB-PICA | Ultrapure water; diluted 100 times | Detecting; matching |
In summary, the embodiment of the application develops a novel method for detecting the synthetic cannabinoid in the tobacco tar, which comprises the steps of firstly carrying out simple, safe and easy-to-operate tobacco tar pretreatment, and then using the SERS technology based on the enhanced base material and the coagulant to greatly enhance the detection sensitivity of the synthetic cannabinoid, so that the trace synthetic cannabinoid in the tobacco tar is detected within 1 minute, and the minimum detection concentration is 10 mug/mL. The detection method provided by the embodiment of the application is simple and convenient to operate, low in cost, quick and high in accuracy, and can be used for conveniently, quickly and accurately screening the synthetic cannabinoid in the tobacco tar on the drug-killing site.
While the present application has been described with reference to illustrative embodiments, it will be understood by those skilled in the art that various other changes, omissions and/or additions may be made and substantial equivalents may be substituted for those of the embodiments without departing from the spirit and scope of the present application. In addition, many modifications may be made to adapt a particular situation or material to the teachings of the application without departing from the scope thereof. Therefore, it is intended that the present application not be limited to the particular embodiments disclosed for carrying out this application, but that the application will include all embodiments falling within the scope of the appended claims.
Claims (2)
1. A method for rapid detection of synthetic cannabinoids in tobacco tar comprising:
diluting tobacco tar 100-1000 times by using a tobacco tar extracting agent to realize pretreatment of the tobacco tar and obtain a sample to be detected, wherein the tobacco tar extracting agent is ultrapure water;
sequentially adding a coagulant and a nano reinforced base material into the sample to be detected, and uniformly mixing to form a liquid-phase mixed system to be detected, wherein the nano reinforced base material adopts spherical silver nano colloid with the particle size of 30-100nm, the coagulant adopts potassium iodide and magnesium iodide with the molar ratio of 1:5-5:1, and the concentration of any iodized salt in the mixed system to be detected is 0.1 mol/L-1 mol/L;
detecting the mixed system to be detected by a Raman spectrometer;
wherein the synthetic cannabinoid is selected from any one or more of 4F-MDMB-BUTICA, 5F-MDMB-PICA, 5F-ADBINACA, ADB-BUTINACA, MDMB-4en-PINACA, AM-694, FUB-JWH-018, FUB-PB-22, 5F-UR-144, MAM-2201, EAM-2201, 5F-PB-22, JWH-019, UR-144, JWH-122, JWH-081, RCS-4, PB-22, AB-CHMINACA, AB-FUBINACA, 5F-AB-PINACA, STS-135, APINACA, MDMB-CHMICA, MDMB-FUBINACA, 5F-AMB, AMB-FUBINACA, JWH-073, JWH-203, JWH-210, JWH-307, JWH-1220, or combinations thereof.
2. The method for rapid detection of synthetic cannabinoids in tobacco tar as claimed in claim 1, characterized in that: in the mixed system to be detected, the volume ratio of the sample to be detected to the coagulant is 1:1-10:1, and the volume ratio of the sample to be detected to the nano reinforced base material is 1:1-10:1.
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