Method for detecting drugs in atmospheric environment samples

Abstract

The present application belongs to the technical field of drug detection method, and particularly relates to a method for detecting drugs in atmospheric environment samples, comprising the following steps: using the adsorption material of a gas sampling instrument to adsorb the drugs in the gas; after the material adsorbs the drugs, using ultrasonic extraction in an organic solvent or a high-temperature heating method to resolve the drugs; and using high-sensitivity mass spectrometry, molecular immunocolloidal gold or fluorescence method to detect the resolved drugs. The detection method can qualitatively and quantitatively detect the drugs in the atmosphere, and is also suitable for detecting the drugs in the exhaled gas of drug users, and contains new psychoactive drugs such as amphetamines, opioids and synthetic cannabis.

Description

Technical Field

[0001] This invention belongs to the technical field of drug detection methods, and particularly relates to a method for detecting drugs in atmospheric environmental samples. Background Technology

[0002] Atmospheric samples are a crucial component of evidence in criminal cases. Changes in drug concentration in the atmosphere can reveal variations in geographical location and time within specific areas. By monitoring drug use and trafficking activities through atmospheric observation, intelligence can be gathered to uncover potential drug manufacturing plants and drug use sites. However, the concentration of drugs in the ambient atmosphere is very low, and atmospheric samples change constantly across space. This necessitates addressing technical challenges such as developing more effective sampling techniques and achieving higher sensitivity and selectivity in analytical methods.

[0003] Detection and monitoring of drugs in environmental samples can objectively, in real-time, accurately, and effectively reflect drug abuse, understand its spatial distribution and temporal changes, and is an effective means to compensate for the shortcomings of traditional drug monitoring methods and to discover potential drug cases. There are currently no research reports in China on the detection of drugs in atmospheric environmental samples. Conducting related research is highly innovative and has great potential application prospects in assessing drug consumption and abuse, as well as guiding case leads.

[0004] Drug and explosive detection dogs have solved numerous cases based on scent, with gaseous evidence playing a crucial role. While these dogs have achieved significant success through scent tracking, they are susceptible to external interference, have short effective working times, exhibit considerable differences between individual dogs, and their operational methods are subject to certain limitations. Researchers have long conducted extensive work on atmospheric sample collection for "electronic noses," such as the electronic nose for detecting heroin disclosed in patent application (CN99230194.7). However, this electronic nose suffers from drawbacks such as detecting a limited range of drugs, insufficient sensitivity in real-world cases, and an immature technological approach with poor reliability. Patent application (CN200920067426.3) discloses a gas sampling device using functionalized magnetic nanomaterials; however, the materials used in this device are not suitable for many common drugs, resulting in poor technical feasibility.

[0005] Therefore, it is of great significance to develop a method for detecting drugs in atmospheric environmental samples that can perform qualitative and quantitative detection of drugs in the atmosphere. Summary of the Invention

[0006] To address the problems existing in the prior art, this invention provides a method for detecting drugs in atmospheric environmental samples. This method can perform qualitative and quantitative detection of drugs in the atmosphere and is also applicable to the detection of drugs in the exhaled breath of drug users, including but not limited to amphetamines, opioids, synthetic cannabis, and other new psychoactive drugs.

[0007] To achieve the above objectives, the present invention adopts the following technical solution:

[0008] This invention uses a grid-like polysiloxane material and passively adsorbs it under negative pressure, allowing airflow to pass through the material to optimize a tubular, highly efficient adsorption structure. This structure adsorbs molecular-level drugs from the atmosphere and detects them using mass spectrometry or molecular immunoassay.

[0009] A method for detecting drugs in atmospheric environmental samples includes the following steps:

[0010] (1) Adsorbing drugs in atmospheric environmental samples using adsorption materials;

[0011] (2) After the material adsorbs the drug, ultrasonic extraction in an organic solvent or high-temperature heating is used to desorb the drug;

[0012] (3) The extracted drugs are detected by high-sensitivity mass spectrometry, molecular immunoassay, colloidal gold or fluorescence methods.

[0013] The adsorbent material has a tubular structure. Gas flows inside the tube, and atmospheric drug molecules collide with and come into contact with the mesh-like polysiloxane material on the tube wall. The polysiloxane material and drug molecules are adsorbed onto the material due to intermolecular forces. The tubular structure is 20 mm long, has an outer diameter of 2.3 mm, an inner diameter of 1.5 mm, and an enrichment film thickness of 0.1 mm. (See attached image.) Figure 1 .

[0014] The adsorbent material is prepared using a composite process of polysiloxane with a network structure and activated carbon material ACAR.

[0015] The detection method described in this invention can objectively, in real-time, accurately, and effectively reflect drug abuse in environmental samples, monitor drug processing and trafficking activities, and provide intelligence leads for discovering potential drug manufacturing plants and drug use sites. Understanding its spatial distribution and temporal changes is an effective means to compensate for the shortcomings of traditional drug monitoring methods and to discover potential drug cases. It has extremely strong potential application prospects in drug consumption and abuse assessment and case lead guidance.

[0016] This invention also discloses an atmospheric environmental sampler, the structure of which includes, along the gas flow direction, a filter element, an air pump, an electromagnetic proportional valve, a pressure sensor, and a flow restrictor connected sequentially via connecting pipes. The filter element is filled with the aforementioned tubular adsorbent material. Ambient air is controlled to flow through the interior of the tubular adsorbent material at a certain flow rate, thereby completing the adsorption of drugs. The sampler uses a brushless diaphragm pump with an internal battery, enabling an ultra-miniaturized design with advantages such as small size, light weight, and long battery life.

[0017] The atmospheric environmental sampler described in this invention achieves precise control of gas volume. Effective enrichment of the effective volume of atmosphere is ensured through the use of new materials. This scheme utilizes the physical properties of different gases to develop a multi-gas self-calibrating flow control algorithm. Based on a PID closed-loop control algorithm, it employs a high-precision pressure sensor (resolution 0.001 psi) and high-speed signal processing technology to solve the system's rapid balance and stability issues. The gas outlet pressure is regulated by an electromagnetic proportional valve. The outlet flow path is connected to a pressure sensor, and the pressure sensor signal is sent to the control circuit to form a closed-loop control with the electromagnetic proportional valve, ensuring that the difference between the outlet pressure and the set value is less than 0.001 psi, thus achieving the purpose of controlling gas pressure and flow. The gas pump has a built-in battery, resulting in low energy consumption, small size, portability, and ease of operation.

[0018] Atmospheric environmental samplers are primarily used for spatial gas sampling in drug use locations, drug manufacturing sites, and near drug manufacturing residues; for sampling gas from the air near drug storage or transportation sites; for sampling respiratory gases from individuals involved in drug use; and for quantitative sampling of urban atmospheric environments. These instruments preserve evidence from an atmospheric evidence perspective, confirming drug use, drug manufacturing, drug trafficking, and assessing urban drug abuse.

[0019] Beneficial effects

[0020] This invention discloses a method for detecting drugs in atmospheric environmental samples. It obtains evidence from the atmospheric perspective, accurately identifying spatial evidence of drug use, drug manufacturing, and drug trafficking. The concentration of drugs in urban atmospheric environmental samples can be used to assess the extent of drug abuse in the city.

[0021] This invention has the following four main advantages:

[0022] I. Functional Advantages: Includes a new technology for combating drug crimes, effectively collecting drugs from the atmosphere, with a detection limit of 1 pg / m³ for drugs in the atmosphere. 3 Simultaneously, multiple drugs and precursor chemicals are collected, including but not limited to: methamphetamine, MDMA, ketamine, cocaine, heroin, morphine, cannabinol, synthetic cannabinoids, fentanyl, ephedrine, and ketones. Atmospheric science can also be used to rule out drug involvement. This saves investigation time and costs.

[0023] II. Cost Advantage: The atmospheric environment sampler described in this invention has a manufacturing cost of over 3,000 yuan, and the adsorption material can be recycled, resulting in minimal cost per use.

[0024] III. Practical Advantages: The atmospheric environmental sampler described in this invention is compact, contains a power supply, weighs 300 grams, and can automatically sample continuously for more than 6 hours.

[0025] IV. Operational Advantages: The atmospheric environmental sampler described in this invention is intuitive, easy to operate, and made of stable materials. It does not require professional technical knowledge and is suitable for use by grassroots police officers. Attached Figure Description

[0026] Figure 1 : A structural diagram of the inner membrane of the adsorption material described in Example 1 of this invention;

[0027] Figure 2 Internal structure diagram of the adsorbent material described in Example 1 of this invention;

[0028] Figure 3 : A schematic diagram of the structure of the tubular adsorption material described in Embodiment 1 of the present invention;

[0029] Figure 4 Schematic diagram of an atmospheric environmental sampler;

[0030] Figure 5 A diagram illustrating the adsorption of drugs in the air;

[0031] Figure 6 Schematic diagram of the process of drug molecules being adsorbed;

[0032] Figure 7 : Chromatographic mass spectrum of methamphetamine and amphetamine components detected in the breath of a methamphetamine user three days after application example 1;

[0033] Figure 8 : Chromatographic mass spectrum of methamphetamine and amphetamine components detected in vehicle interior gas in Application Example 1;

[0034] Figure 9 : Chromatographic mass spectrometry of the synthetic cannabinoid ADB-BUTINACA detected in a room where e-cigarettes had been used in Application Example 2;

[0035] In the diagram, 1: Inlet; 2: Air pump; 3: Filter element; 4: Electromagnetic proportional valve; 5: Pressure sensor; 6: Flow restrictor; 7: Connecting pipeline. Detailed Implementation

[0036] The present invention will now be described in detail. Before proceeding with the description, it should be understood that the terminology used in this specification and the appended claims should not be construed as limited to its general or dictionary meaning, but rather should be interpreted according to the meaning and concept corresponding to the technical aspects of the invention, based on the principle that the inventors are allowed to appropriately define the terms for the best interpretation. Therefore, the description presented herein is merely a preferred example for illustrative purposes and is not intended to limit the scope of the invention. It should be understood that other equivalents or modifications can be obtained from it without departing from the spirit and scope of the invention.

[0037] The following embodiments are merely examples illustrating implementations of the present invention and do not constitute any limitation on the present invention. Those skilled in the art will understand that modifications made without departing from the spirit and concept of the present invention fall within the protection scope of the present invention. Unless otherwise specified, the reagents and instruments used in the following embodiments are commercially available products.

[0038] Example 1 Atmospheric Environmental Sampler

[0039] 1. Development of atmospheric microextraction materials specifically for drugs

[0040]

[0041] Vinyl-terminated polydimethylsiloxane reacts with a crosslinking agent, hydrogen-containing silicone oil, under the catalysis of a vinylsiloxane-coordinated platinum complex to generate a network-structured polysiloxane. This network-structured polysiloxane exhibits low intermolecular-chain interactions, low rotational resistance within the silicon-oxygen bonds, high chain mobility, large free volume, and excellent permeability to organic substances. Furthermore, the bond energy of the silicon-oxygen bonds in the polysiloxane structure is 451 kJ / mol, significantly higher than the 345 kJ / mol C-C bond energy, demonstrating superior adsorption capacity, solvent resistance, and heat resistance, making it a relatively ideal material for gas extraction of narcotics.

[0042] Activated carbon material (ACAR) is a type of material with micropore diameters between 2 and 50 nm and a specific surface area of ​​500 to 1500 m². 2 The material possesses high adsorption properties. Impurities are removed through purification processes such as solvent washing and high-temperature aging, and its surface is modified with silane coupling agent KH560 to increase its binding force with the silane system.

[0043] 2. Material structural morphology design

[0044] like Figure 1-3 As shown, the adsorbent material is designed as a hollow tube. By optimizing the tube's inner diameter, length, and film thickness based on the material's spatial structure, the material can achieve efficient enrichment, easy desorption, and reuse. Based on practical needs, the material is designed as a tube. Factors such as gas flow rate, temperature, and composition are considered, and combined with the physicochemical properties of various common drugs, a gas flow dispersion model within the material is established to optimize the optimal tubular morphology. The optimal dimensions are: length 20mm, outer diameter 2.3mm, inner diameter 1.5mm, and film thickness 0.1mm.

[0045] 3. Structure of the Atmospheric Environmental Sampler

[0046] like Figure 4 As shown, the structure of the atmospheric environment sampler is as follows: along the direction of gas flow, it includes a filter element 3, an air pump 2, an electromagnetic proportional valve 4, a pressure sensor 5, and a flow limiter 6 connected in sequence through a connecting pipe 7. The filter element 3 is filled with the aforementioned tubular adsorbent material.

[0047] The atmospheric environmental sampler achieves precise control of gas volume. Effective enrichment of the effective volume of atmosphere is ensured through the use of new materials. This scheme utilizes the physical properties of different gases to develop a multi-gas self-calibrating flow control algorithm. Based on a PID closed-loop control algorithm, it employs a high-precision pressure sensor (resolution 0.001 psi) and high-speed signal processing technology to solve the system's rapid balance and stability issues. The gas outlet pressure is regulated by an electromagnetic proportional valve 4. The outlet flow path connects to a pressure sensor 5, and the pressure sensor signal is sent to the control circuit to form a closed-loop control with the electromagnetic proportional valve 4, ensuring that the outlet pressure differs from the set value by less than 0.001 psi, thus achieving the purpose of controlling gas pressure and flow. The gas pump 2 has a built-in battery, resulting in low energy consumption, small size, and easy portability and operation.

[0048] The atmospheric environment sampler described in this invention has been applied to spatial gas sampling at drug use sites and drug manufacturing sites. Currently, it is being used for spatial gas sampling and evidence collection at drug storage or transportation sites, primarily in comparative experiments with police dog drug detection at drug trafficking sites. The next step is planned to be quantitative sampling and evidence collection of urban atmospheric environments.

[0049] The atmospheric environmental sampler described in this invention can accurately collect gaseous evidence of drug use, drug manufacturing, and drug trafficking, and assess the drug abuse situation in the city based on the drug concentration in the urban atmospheric environmental sample.

[0050] This atmospheric environmental sampler is suitable for sampling volatile pesticides, organic explosives, and volatile organic pollutants in the ambient atmosphere, and can be used in scenarios such as security activities for major missions, environmental protection, and chemical production.

[0051] Example 2

[0052] A method for detecting drugs in atmospheric environmental samples includes the following steps:

[0053] (1) Adsorbing drugs in atmospheric environmental samples using the adsorption material in the atmospheric environmental sample sampler described in Example 1;

[0054] (2) After the material adsorbs the drug, ultrasonic extraction in an organic solvent or high-temperature heating is used to desorb the drug;

[0055] (3) The extracted drugs are detected by high-sensitivity mass spectrometry, molecular immunoassay colloidal gold or quantum fluorescence method.

[0056] After the material adsorbs the drug, it is subjected to ultrasonic extraction in an organic solvent for 10 minutes or heated to a high temperature above 220°C to desorb the drug. The material can then be desorbed and directly reactivated for reuse. The drug desorbed by ultrasound can be detected by high-sensitivity mass spectrometry, molecular immunoassay, colloidal gold, or fluorescence methods.

[0057] The detection method described in this invention collects evidence from an atmospheric perspective, accurately identifying spaces where drugs are used, manufactured, or trafficked. Urban atmospheric environmental samples can be used to assess the extent of drug abuse in an urban area based on drug concentrations.

[0058] Application Example 1

[0059] On August 7, 2022, Li was driving at 200 kilometers per hour on the highway, suspected of driving under the influence of drugs. After being intercepted by highway patrol officers, his breath was sampled using the atmospheric environmental sampler described in Example 1. The sample was then ultrasonically eluted in a methanol solution, and the gas was analyzed using liquid chromatography-mass spectrometry (LC-MS). Methamphetamine and amphetamine were detected in the breath. To trace the case and determine the location of drug use, the method described in this invention was used to detect methamphetamine and amphetamine in the air inside his vehicle, proving that he had used methamphetamine inside the car.

[0060] Methamphetamine and amphetamine were detected in the breath of a methamphetamine user three days after use, as shown in the chromatogram and mass spectra. Figure 7 As shown.

[0061] Drug use inside the car resulted in the detection of methamphetamine and amphetamine in the fumes, as shown in the chromatogram and mass spectra. Figure 8 As shown.

[0062] Application Example 2

[0063] On August 23, 2022, an unusual odor was detected in a KTV room in the city. The atmospheric environmental sampler described in this invention was used to absorb the air at the scene for 30 minutes to sample the breath of Mr. Li. After sampling, the drug was ultrasonically eluted in a methanol solution and detected by liquid chromatography-mass spectrometry. The synthetic cannabinoid ADB-BUTINACA was detected, proving that someone in the room had used the drug.

[0064] Synthetic cannabinoid ADB-BUTINACA was detected in a room where e-cigarettes had been used. The chromatographic mass spectrum is shown below. Figure 9 As shown.

[0065] The above embodiments are only used to illustrate the technical solutions of the present invention, and are not intended to limit them. Although the present invention has been described in detail with reference to the foregoing embodiments, those skilled in the art can still modify the technical solutions described in the foregoing embodiments or make equivalent substitutions for some of the technical features. Such modifications or substitutions do not cause the essence of the corresponding technical solutions to deviate from the spirit and scope of the technical solutions claimed by the present invention.

Claims

1. A method for detecting drugs in atmospheric environmental samples, characterized in that, Includes the following steps: (1) Adsorbing drugs in atmospheric environmental samples using adsorption materials; (2) After the material adsorbs the drug, it is extracted by ultrasonic extraction in an organic solvent or by high-temperature heating to decompose the drug; (3) The extracted drugs are detected by high-sensitivity mass spectrometry, molecular immunoassay, colloidal gold, or fluorescence methods; The adsorbent material has a tubular structure and can be directly reactivated after desorption, allowing it to be reused. The adsorbent material is prepared using a composite process of polysiloxane with a network structure and activated carbon material ACAR. The preparation method of the adsorbent material includes: Vinyl-terminated polydimethylsiloxane reacts with crosslinking agent hydrogen-containing silicone oil under the action of catalyst vinylsiloxane-coordinated platinum complex to generate polysiloxane with a network structure. Activated carbon material ACAR is a material with high adsorption performance, with micropore diameter between 2 and 50 nm and specific surface area between 500 and 1500 m2. The activated carbon material ACAR is purified by solvent washing and high temperature aging to remove impurities, and its surface is modified with silane coupling agent KH560 to increase its binding force with the silane system. Hollow tubular adsorbent materials were prepared by a composite process of network-structured polysiloxane and modified activated carbon material ACAR. The tubular structure has a length of 20 mm, an outer diameter of 2.3 mm, an inner diameter of 1.5 mm, and an enrichment film thickness of 0.1 mm.

2. The method for detecting drugs in atmospheric environmental samples according to claim 1, characterized in that, In step (1), the adsorption material in the atmospheric environmental sampler is used to adsorb the drugs in the atmospheric environmental sample.

3. The method for detecting drugs in atmospheric environmental samples according to claim 2, characterized in that, The atmospheric environment sampler has the following structure: along the direction of gas flow, it includes a filter element, an air pump, an electromagnetic proportional valve, a pressure sensor, and a flow limiter connected in sequence through connecting pipes. The filter element is filled with tubular adsorbent material.

4. The method for detecting drugs in atmospheric environmental samples according to claim 3, characterized in that, The air pump is a brushless diaphragm pump with an internal battery.

5. The method for detecting drugs in atmospheric environmental samples according to claim 3, characterized in that, A control circuit is also provided. The pressure sensor and the electromagnetic proportional valve are both electrically connected to the control circuit. The pressure sensor signal is sent to the control circuit to form a closed-loop control with the electromagnetic proportional valve. The control outlet pressure is kept less than 0.001 psi from the set value, thereby achieving the purpose of controlling gas pressure and flow.

Images