Method for detecting mental anesthesia drugs in environmental sludge based on alkaline condition pretreatment and application

Abstract

The invention provides a method for detecting mental anesthesia drugs in environmental sludge based on alkaline condition pretreatment, which comprises the following steps: S1, obtaining a to-be-detected sludge sample, freeze-drying the to-be-detected sludge sample, performing pressurized fluid extraction to obtain an extract, performing solid-phase extraction on the extract, and eluting to obtain an eluent, redissolving the eluent to obtain a solution to be detected, wherein the pressurized fluid extraction condition is 0.1% ammonia water and heating is not carried out; s2, the solution to be detected is subjected to liquid chromatography-mass spectrometry detection, a mass spectrum is obtained, the condition is that the mental anesthetic drugs are one or a combination of more than two of morphine, acetyl norfentanil and THC-COOH, and detection of the multiple mental anesthetic drugs in the environmental sludge is achieved.

Description

Technical Field

[0001] The present application relates to the field of drug detection, and in particular to a method and application for detecting psychotropic narcotic drugs in environmental sludge based on alkaline pretreatment. Background Art

[0002] In recent years, with the intensification of global drug manufacturing, trafficking and abuse, psychotropic drugs have been continuously discharged into the environment, which may cause harm to the ecological environment and human health. The process of producing psychotropic drugs often discharges harmful chemicals and wastewater, which contain heavy metals, acid and alkali solutions, organic solvents and other toxic components, which can directly pollute the soil, water and air.

[0003] Due to the illegality and low prevalence of drug abuse, it is difficult to obtain real data on drug abuse through traditional drug abuse investigation methods. At present, the conventional practice is to detect whether there are psychotropic drugs in sewage, but less attention is paid to the long-term residual and cumulative effects of drug use traces in sludge, especially the drug components deposited in sludge generated during sewage treatment. In real life, drugs and their metabolites in sewage will flow and dilute rapidly with the water flow, and the substances excreted by drug users will eventually accumulate in the sludge generated during sewage treatment. As a deposit of solid matter in sewage, sludge can preserve drug use records for a long time. And because sewage has strong fluidity, sewage detection often reflects the situation of the entire sewage treatment area, which is difficult to accurately identify specific communities or blocks. However, sludge is relatively stable and contains a large number of metabolites of human consumption drugs. By analyzing the drug residues in municipal sludge and combining information such as human metabolic ratios, the use of such drugs and the health and usage habits of the relevant population can be inferred. Testing psychotropic drugs in sludge can more objectively, quickly and accurately reflect the drug abuse of the local population.

[0004] Of course, there are still many ways to test human urine for drugs on the market. At this time, the drugs are excreted from the body through urine after being metabolized by the human body. Usually, the concentration of drug residues in urine is high. After the urine is extracted and separated and derivatized, the residual drugs can be detected more easily. When human urine enters the sewage collection system and is mixed with municipal sludge, the drug residues therein are usually diluted hundreds or even thousands of times, and the concentration is usually only at the nanogram level. Therefore, it is more difficult to analyze drug residues from sludge than from urine. In addition, sludge contains a more complex matrix than sewage, and the high content of organic matter, microorganisms and inorganic particles interferes with the extraction and detection of psychotropic drugs.

[0005] In summary, there is currently a lack of highly sensitive detection solutions for psychotropic drugs in sludge on the market. Summary of the invention

[0006] The present application provides a method and application for detecting psychotropic narcotic drugs in environmental sludge based on alkaline pretreatment, which realizes rapid and accurate detection of psychotropic narcotic drugs in environmental sludge by combining pressurized extraction, solid phase extraction and triple quadrupole tandem mass spectrometry.

[0007] To achieve the above objectives, the present technical solution provides a method for detecting psychotropic narcotic drugs in environmental sludge based on alkaline pretreatment, comprising the following steps:

[0008] S1: obtaining a sludge sample to be tested, freeze-drying the sludge sample and then performing pressurized fluid extraction to obtain an extract, performing solid phase extraction on the extract and then eluting to obtain an eluent, and re-dissolving the eluent to obtain a solution to be tested, wherein the condition of the pressurized fluid extraction is 1‰ ammonia water without heating;

[0009] S2: Performing liquid chromatography-mass spectrometry on the test solution to obtain a mass spectrum, and judging whether the current sludge sample to be tested contains psychotropic narcotic drugs based on the base peak mass-to-charge ratio of the mass spectrum, wherein the chromatographic conditions are: mobile phase A is methanol, mobile phase B is 0.1% formic acid water, and gradient elution; the conditions are: the psychotropic narcotic drugs are one or a combination of two or more of morphine, acetylnorfentanyl and THC-COOH.

[0010] It should be noted that the traditional scheme for detecting psychotropic narcotic drugs in sewage does not require pressurized fluid extraction. Most schemes directly perform solid phase extraction or perform large-volume online solid phase extraction. The present scheme detects psychotropic narcotic drugs in sludge. Compared with the sewage detection environment, the sludge sample matrix is ​​more complex and the concentration of psychotropic narcotic drugs is lower. This is because the sludge is composed of multiple components such as water, microorganisms, organic matter, inorganic particles, etc. Its complex matrix may lead to strong adsorption and masking of target compounds. At the same time, some psychotropic narcotic drugs in the sludge will be partially degraded or absorbed by microorganisms. Therefore, the present scheme also performs pressurized fluid extraction on the sludge sample before solid phase extraction, and optimizes the conditions for pressurized fluid extraction.

[0011] The morphine, acetylnorfentanyl and THC-COOH detected in this scheme are suitable for pretreatment based on alkaline conditions. In the pretreatment step of the sludge sample to be tested in step S1:

[0012] In some embodiments, the sludge sample to be tested is placed in a low-temperature environment and frozen for a period of time, and the frozen sludge sample to be tested is dehydrated and dried.

[0013] When extracting psychotropic drugs from sludge using pressurized fluid extraction, the different water contents in the sludge samples to be tested have a significant impact on the absolute recovery rate of the deuterated internal standard of psychotropic drugs in the extract. Generally speaking, the higher the water content in the sludge sample, the lower the absolute recovery rate of the deuterated internal standard of psychotropic drugs. This is because the surface tension of water is relatively large. Therefore, when the water content in the sample to be tested is higher, it is more difficult for the extract to enter the gap space between the sample particles. At the same time, the water in the sample to be tested dilutes the extract, causing the acidity and alkalinity of the extract to change during extraction, affecting the extraction effect. Therefore, this solution requires freeze drying the sludge sample to be tested so that the water content of the sludge sample to be tested after freeze drying is less than 5%. Preferably, the water content of the sludge sample to be tested after freeze drying is controlled to be less than 1%.

[0014] This scheme controls the water content of the sample for fluid extraction by freeze-drying the sludge sample to be tested. However, since psychotropic narcotics have certain volatility, the longer the freeze-drying time, the greater the loss of psychotropic narcotics as the target. When the freeze-drying time is short, insufficient drying will lead to a high water content in the sludge, resulting in reduced extraction efficiency during extraction. In an embodiment of this scheme, the freeze-drying time is set to be greater than 2 hours. Specifically, this scheme places the sludge sample to be tested in a high and low temperature test box at -50°C for 2 hours for pre-freezing, and then uses a vacuum freeze dryer to dehydrate and dry the sample for 2 hours.

[0015] This scheme uses pressurized fluid extraction to obtain an extract from the freeze-dried sludge to be treated. Compared with QuEChERS extraction purification and oscillation extraction, the pressurized fluid extraction method has the best extraction effect on psychotropic narcotics. Since there are many types of psychotropic narcotics and their physical and chemical properties vary greatly, many psychotropic narcotics are easily degraded under environmental conditions, and their properties are between volatile and semi-volatile, making the overall extraction difficult. After verifying different extraction methods, this scheme found that QuEChERS is not ideal for the extraction of psychotropic narcotics, and the absolute recovery rate of the internal standard is generally below 10%; the oscillation extraction method also has a very low overall spike recovery rate for psychotropic narcotics, and there are even cases where some target substances cannot be extracted.

[0016] QuEChERS is commonly used to extract pesticide residues in food and agricultural products. It achieves rapid purification through salting out and phase separation technology. However, for compounds such as psychotropic drugs, their physical and chemical properties are very different from those of pesticides, making them unsuitable for the standard extraction solvents and conditions of QuEChERS. In addition, the QuEChERS method cannot effectively release and stabilize psychotropic drugs when treating such sludge, resulting in a large number of psychotropic drugs not being extracted or being destroyed during the treatment process. Oscillating extraction usually relies on solvent immersion and mechanical stirring to promote the dissolution and transfer of target compounds. This extraction method is not enough to break the strong interaction within the solid phase, especially for psychotropic drugs that are easily degraded in the environment and have physical and chemical properties between volatile and semi-volatile. Therefore, this scheme selects the pressurized fluid extraction method to extract psychotropic drugs from the sludge samples to be tested. By selecting a suitable solvent, it can more effectively penetrate the solid matrix, increase the solubility of the target compound, and thus improve the extraction efficiency.

[0017] In some embodiments, the pressurized fluid extraction condition is 1‰ ammonia water without heating, and the cycle is repeated 3 times.

[0018] In an embodiment of the present scheme, the freeze-dried sludge sample to be tested is placed in an extraction tank filled with an extracting solution for pressurized fluid extraction. Considering that the present scheme is to extract psychotropic narcotic drugs, which have certain instability, easy degradation and strong volatility, the present scheme sets the conditions for pressurized fluid extraction as no heating to reduce the impact on psychotropic narcotic drugs.

[0019] In addition, the extracting liquid of the pressurized fluid extraction has a significant impact on the extraction effect. The solubility, acidity and alkalinity and other physical and chemical properties of different drugs vary greatly, so this scheme needs to select the most suitable extracting liquid. This scheme selects 1‰ ammonia water as the extracting liquid. This is because most of these psychotropic narcotic drugs are weakly acidic, and using 1‰ ammonia water as the extracting liquid has the best extraction effect.

[0020] Ammonia, as an alkaline solvent, can change the molecular state of morphine, acetylnorfentanyl and THC-COOH, and promote their release from sludge samples. For many organic compounds, especially those with acidic functional groups, the alkaline environment can promote their ionization or form salts that are more soluble in water, thereby improving the extraction efficiency. At the same time, 1‰ ammonia can break the interaction between a large number of organic and inorganic components without extracting a large amount of interfering substances, and effectively extract the target drugs.

[0021] This scheme obtains an extract by pressurized fluid extraction, and then performs solid phase extraction and elution to obtain an eluent. In an embodiment of this scheme, the extract is injected into an activated solid phase extraction column, the solid phase extraction column is eluted with pure water, and then the solid phase extraction column is air-pushed to dryness, and then the solid phase extraction column is eluted with methanol to obtain the eluent.

[0022] Since the content of psychotropic drugs in environmental sludge is extremely low and the matrix is ​​very complex, in order to effectively improve the efficiency of drug extraction and detection and achieve high sensitivity, fast speed and other effects, this scheme combines solid phase extraction with liquid chromatography tandem mass spectrometry, which can ensure detection sensitivity, reduce matrix interference, and realize the screening of drugs in sludge. In the embodiment of this scheme, Poly-Sery HLB Pro is selected as a solid phase extraction column. Considering that the Poly-Sery HLB Pro solid phase extractant has good retention and recovery capabilities for compounds with a wide range of polarities, Poly-Sery HLB Pro can effectively adsorb and retain these target compounds of different polarities, improve extraction efficiency and recovery rate, and its chemical stability and mechanical strength ensure that it can maintain good performance under repeated use and high pressure conditions.

[0023] In some embodiments, methanol is used to activate the solid phase extraction column at a flow rate of no more than 1 mL / min, and then pure water is added to rinse the solid phase extraction column to obtain an activated solid phase extraction column. The extract is added to the activated solid phase extraction column at a flow rate of 4 mL / min, and the solid phase extraction column is eluted with pure water at a rinsing flow rate of 2 mL / min. Subsequently, the solid phase extraction column is eluted with methanol at an elution flow rate not exceeding 1 mL / min to obtain an eluate.

[0024] It should be noted that the flow rate during solid phase extraction will affect the extraction results. This scheme sets the extract to be added to the activated solid phase extraction column at a flow rate of 4 mL / min, aiming to quickly and effectively transfer the psychotropic narcotics in the extractant to the solid phase extraction column, while minimizing the retention or loss of psychotropic narcotics in front of the column. For samples containing a large amount of matrix or solvent, an appropriate high flow rate can help reduce column pressure and speed up processing, but it is necessary to ensure that the adsorbed impurities or targets are not washed away; while a lower elution flow rate can help more thoroughly remove non-specifically adsorbed impurities, such as salts, pigments and small molecule interferences, while maintaining the adsorption of psychotropic narcotics on the column; using methanol to activate the solid phase extraction column at a flow rate of no more than 1 mL / min helps ensure that methanol fully contacts and wets all adsorbent surfaces, so that the solid phase extraction column reaches the optimal adsorption state; a methanol elution flow rate of no more than 1 mL / min is also conducive to the efficient release of psychotropic narcotics adsorbed on the solid phase extraction column. A slow flow rate can ensure a gentler elution process, allowing the psychotropic narcotics enough time to desorb from the adsorbent and be completely eluted, while reducing the column pressure, maintaining the stability of the eluent, and avoiding the failure of psychotropic narcotics to be fully eluted or uneven dispersion of the eluent due to too fast a flow rate.

[0025] In some embodiments, the eluent is concentrated by nitrogen blowing and injected with 20% methanol water to obtain a test solution. In a specific embodiment, the eluent is concentrated to near dryness by nitrogen blowing at 40°C until there are tiny liquid pits on the surface of the eluent, and the test solution is obtained by constant volume with 20% methanol water.

[0026] In the detection step of the sludge sample to be tested in step S2:

[0027] In this scheme, the test solution is injected into liquid chromatography for separation, and mass spectrometry is used for detection. The separation of each psychotropic narcotic drug on the chromatographic column is observed to determine the gradient elution conditions. The retention time of each component is determined by obtaining the mass-to-charge ratio m / z information of the quasi-molecular ion in the primary mass spectrum of each psychotropic narcotic drug. The secondary mass spectrometry is optimized using the quasi-molecular ions of each psychotropic narcotic drug as parent ions, and the fragmentation voltage and collision energy are optimized to obtain the corresponding daughter ions produced by the fragmentation of each parent ion.

[0028] In the embodiment of this scheme, a triple quadrupole liquid-mass spectrometer is selected, and ACQUITY UPLC HSS T3 (2.1×100mm×1.8μm) is selected as the chromatographic column. The reason why this scheme specifically selects a triple quadrupole liquid-mass spectrometer is that it greatly reduces background interference and significantly improves the sensitivity and specificity of detection through two mass screenings (selection of parent ions and daughter ions), which is crucial for trace analysis, especially for the detection of psychotropic narcotic drugs in sludge samples with complex matrices; the reason why ACQUITY UPLC HSS T3 (2.1×100mm×1.8μm) is selected as the chromatographic column is that the HSS T3 column is suitable for separating polar compounds, and its 1.8-micron particle size reduces the diffusion path and improves the separation efficiency. It is particularly suitable for the rapid and efficient separation of targets in complex samples, providing clean chromatographic peaks for mass spectrometry analysis. Compared with traditional HPLC, UPLC ultra-high performance liquid chromatography technology provides faster separation speed and higher column efficiency, which can significantly shorten the analysis cycle and improve the throughput of the laboratory.

[0029] In some embodiments, the mobile phase A is methanol, and the mobile phase B is 0.1% formic acid water. The elution conditions of the gradient elution are shown in Table 1 below:

[0030] Table 1 Elution conditions

[0031]

[0032]

[0033] In some embodiments, 5.0 μL was injected; column temperature: 40° C.; flow rate: 0.4 ml / min.

[0034] In some embodiments, the mass spectrometry conditions are set as follows: electrospray ion source (ESI); ion source temperature: 550° C.; detection mode: multiple reaction monitoring (MRM); scanning mode: positive / negative ion scanning.

[0035] In addition, it should be noted that the method for detecting psychotropic narcotic drugs in environmental sludge based on alkaline pretreatment provided in this scheme can not only qualitatively detect psychotropic narcotic drugs, but also quantitatively detect psychotropic narcotic drugs through the internal standard method. At this time, the internal standard is the deuterated isotope internal standard of each psychotropic narcotic drug.

[0036] It should be noted that this scheme verifies that when the deuterated isotope internal standard and the psychotropic narcotic drug exist separately, when the deuterated isotope internal standard and the psychotropic narcotic drug exist at the same time and are treated, the absolute recoveries of the deuterated internal standard and the target do not change significantly, indicating that there is no "hydrogen-deuterium exchange" reaction in the environmental sludge, so the deuterated isotope internal standard can be selected as the quantitative internal standard.

[0037] In the second aspect, the present scheme provides the application of the method for detecting psychotropic narcotic drugs in environmental sludge based on alkaline pretreatment mentioned in the first aspect, and applies it to the detection of psychotropic narcotic drugs in environmental sludge.

[0038] This program can timely and accurately reflect the local consumption quantity by detecting psychotropic narcotic drugs in environmental sludge. The detection method has the advantages of convenient sampling and analysis, less time consumption, low cost and strong objectivity. It can truly reflect the actual consumption of different psychotropic narcotic drugs, and can reflect the short-term consumption trend of small-scale and daily consumption changes such as communities. At the same time, it can also determine the consumption of psychotropic narcotic drugs and predict their use development trend. It is suitable for investigating the prevalence and abuse of drugs on a large scale.

[0039] Compared with the prior art, this technical solution has the following characteristics and beneficial effects:

[0040] This scheme combines pressurized fluid extraction and solid phase extraction, uses alkaline pretreatment to achieve the extraction of psychotropic narcotic drugs from environmental sludge, and cooperates with high performance liquid chromatography tandem mass spectrometry to achieve efficient detection of psychotropic narcotic drugs in sludge. This scheme optimizes the optimal extraction conditions of pressurized fluid extraction and solid phase extraction to achieve the best extraction of psychotropic narcotic drugs. Through the detection of actual sludge samples, the detection method of common psychotropic narcotic drugs in sludge in the determination environment is used to conduct rapid and accurate quantitative detection of samples, providing technical support for public security departments, and making important contributions to the improvement of the drug control and prevention system. BRIEF DESCRIPTION OF THE DRAWINGS

[0041] The drawings described herein are used to provide a further understanding of the present application and constitute a part of the present application. The illustrative embodiments of the present application and their descriptions are used to explain the present application and do not constitute an improper limitation on the present application. In the drawings:

[0042] Figure 1 This is a schematic diagram of the absolute recovery rate of the internal standard of psychotropic narcotic drugs with different extraction solutions.

[0043] Figure 2 It is the standard chromatogram for the detection of psychotropic drugs in environmental sludge in this scheme.

[0044] Figure 3 It is the mass spectrum of Example 4. DETAILED DESCRIPTION

[0045] Exemplary embodiments will be described in detail herein, examples of which are shown in the accompanying drawings. When the following description refers to the drawings, the same numbers in different drawings represent the same or similar elements unless otherwise indicated. The implementations described in the following exemplary embodiments do not represent all implementations consistent with one or more embodiments of this specification. Instead, they are merely examples of devices and methods consistent with some aspects of one or more embodiments of this specification as detailed in the appended claims.

[0046] In order to obtain the optimal extraction conditions for psychotropic narcotic drugs in this scheme, this scheme designs experiments to determine the optimal extraction conditions through spike recovery rate.

[0047] The reagents selected in this scheme are: methanol: chromatographic grade; freshly prepared ultrapure water; formic acid: analytical grade; psychotropic narcotic drug standards and internal standard;

[0048] Main instrument selection: triple quadrupole liquid-mass spectrometer: electrospray ionization (ESI) source; chromatographic column: ACQUITYUPLC HSS T3, 2.1×100mm×1.8μm; freeze dryer; pressurized fluid extractor; nitrogen blower; rotary evaporator; vortex oscillator; parallel concentrator; fully automatic solid phase extractor; balance: sensitivity 0.1mg and 0.01g; common laboratory instruments and equipment;

[0049] Embodiment 1

[0050] Select psychotropic drug standards and deuterated internal standards of morphine, acetylnorfentanyl, and THC-COOH;

[0051] Take 10g of blank sludge containing deuterated internal standard of psychotropic narcotic drugs of known concentration as sample and place it in an aluminum box, put the sample into a high and low temperature test box at -50℃ to pre-freeze the sample for 2h, and then use a vacuum freeze dryer to dehydrate and dry the sample for 2h; transfer the freeze-dried sample to the extraction pool, set the parameters of the pressurized fluid extractor: 1‰ ammonia water, extraction temperature: none or 40℃, number of cycles: 3 times, and obtain the sample extract; fix the Poly-Sery HLB Pro SPE Cartridge (60mg, 3mL) solid phase extraction column on the solid phase extraction device, add 6mL methanol to adjust the flow rate control valve to activate the solid phase extraction column at a flow rate of 1mL / min, then add 6mL ultrapure water to rinse the solid phase extraction column, and add all the sample extract to the activated Poly-Sery HLB Pro SPE Cartridge (60mg, 3mL) solid phase extraction column, column flow rate 4mL / min, pure water 4mL elution, elution flow rate 2mL / min, air push solid phase extraction column to dryness and discard the effluent, elute with methanol 6mL, elution flow rate not exceeding 1mL / min, collect the eluate, open nitrogen at 40℃ until there are fine liquid pits on the surface of the solvent, blow the purified eluted liquid nitrogen to concentrate to near dryness, and dilute to 250μL with 20% methanol water. Mix well, filter and analyze on the machine.

[0052] The elution conditions of the mobile phase gradient elution of the triple quadrupole LC / MS are set as shown in Table 1 below. The elution injection volume is set to 5.0 μL; the column temperature is 40°C; and the flow rate is 0.4 ml / min:

[0053] Table 1 Elution conditions

[0054]

[0055]

[0056] The mass spectrometry conditions were set as follows: electrospray ionization source (ESI); ion source temperature: 550°C; detection mode: multiple reaction monitoring (MRM); scanning mode: positive / negative ion scanning.

[0057] Analysis of results: In this experiment, 40℃ and no heating were used to extract various drug residues in sludge, and the absolute recovery rate of the internal standard was used as the indicator for testing. The results showed that temperature had little effect on the extraction effect. Therefore, when extracting, a lower extraction cell temperature was selected as much as possible without affecting the extraction efficiency, and finally the extraction cell was selected without heating.

[0058] Embodiment 2

[0059] The same as the first embodiment, except that: the parameters of the pressurized fluid extractor are set as follows: 0.1‰ ammonia water; or, 1‰ ammonia water, or neutral water, extraction temperature: none, and number of cycles: 3 times.

[0060] Result analysis: In this experiment, 0.1‰ ammonia water or 1‰ ammonia water or neutral water were used to extract various drug residues in sludge, and the results were obtained by testing with the absolute recovery rate of the internal standard as the indicator. Figure 1 As shown, it can be seen from 1 that 1‰ ammonia water has the best extraction effect.

[0061] Embodiment 3

[0062] Take 10g of dried sludge, add different volumes of ultrapure water to prepare sludge samples with water contents of 0%, 5%, 10% and 20%, then add deuterated internal standards containing known concentrations of psychotropic narcotic drugs, and proceed with subsequent steps according to Example 1.

[0063] Result analysis: In this experiment, samples with water content of 0%, 5%, 10% and 20% were selected for extraction of various drug residues. It can be seen that when the water content of the sample is lower than 5%, the overall extraction effect of psychotropic narcotic drugs is best.

[0064] Embodiment 4

[0065] Other conditions are the same as those in Example 1, except that: the parameters of the pressurized fluid extractor are set to 1‰ formic acid water, extraction temperature: none, number of cycles: 3 times, and sludge mixed with psychotropic narcotic drug standards of morphine, acetylnorfentanyl and THC-COOH is selected for on-machine testing.

[0066] Result analysis: The mass spectrum obtained in this example is as follows: Figure 3 As shown by Figure 3 It can be seen that this scheme can simultaneously detect the psychotropic narcotic drugs of morphine, acetylnorfentanyl and THC-COOH.

[0067] Embodiment 5

[0068] The other conditions are the same as those in Example 1, except that: the parameters of the pressurized fluid extractor are set to 1‰ formic acid water, extraction temperature: none, number of cycles: 3 times, and standard solutions of psychotropic narcotic drugs containing corresponding internal standards of 10 ng / ml are selected at 0.10, 0.20, 0.40, 1.00, 5.00, 10.0, 20.0 and 50.0 ng / mL.

[0069] Results analysis: In this test, the standard curve was drawn based on the measurement results of the peak area ratio of the internal standard in different concentrations of the same psychotropic narcotic drug. The correlation coefficient r of the standard curve was between 0.9967 and 0.9999. The standard peak area ratio result table was shown in Table 2 below:

[0070] Table 2 Peak area ratio results of different concentrations of psychotropic drugs

[0071]

[0072] Embodiment 6

[0073] Other conditions are the same as those in Example 1, except that: the parameters of the pressurized fluid extractor are set to 1‰ ammonia water, extraction temperature: none, number of cycles: 3 times, and a sludge sample with a corresponding internal standard concentration of 10 ng / kg of psychotropic drugs is selected for full-program determination.

[0074] Result analysis: The detection limit of psychotropic narcotic drugs is 10ng / kg, and the quantitative limit is 40ng / kg. The results of the method detection limit and quantitative limit are shown in Table 3 below:

[0075] Table 3 Method detection limit and quantification limit

[0076]

[0077] Embodiment 7

[0078] Other conditions were the same as those in Example 1, except that: the parameters of the pressurized fluid extractor were set to 1‰ ammonia water, extraction temperature: none, number of cycles: 3 times, and sludge samples with three different concentrations of 25 ng / kg, 250 ng / kg, and 1000 ng / kg were selected for full-program determination.

[0079] Result analysis: The relative deviation of precision is between 0.8% and 13.2%. The precision test results are shown in Table 4. Table 4 Precision test results

[0080]

[0081] Embodiment 8

[0082] Other conditions are the same as those in Example 1, except that: the parameters of the pressurized fluid extractor are set to 1‰ ammonia water, extraction temperature: none, number of cycles: 3 times, sludge samples are taken, and 0.25ng, 2.5ng, and 10ng of psychotropic drugs are added respectively for full-program determination.

[0083] Result analysis: The actual samples were spiked and tested, and the spike recovery rate was 80% to 120%. The accuracy test is shown in Table 5 below:

[0084] Table 5 Correctness test

[0085]

[0086] The above embodiments only express several implementation methods of the present application, and the descriptions thereof are relatively specific and detailed, but they cannot be understood as limiting the scope of the present application. It should be pointed out that, for a person of ordinary skill in the art, several variations and improvements can be made without departing from the concept of the present application, and these all belong to the protection scope of the present application. Therefore, the protection scope of the present application shall be subject to the attached claims.

Claims

1. A method for detecting psychotropic narcotic drugs in environmental sludge based on alkaline pretreatment, characterized in that: The following steps are involved: S1: obtaining a sludge sample to be tested, freeze-drying the sludge sample and then performing pressurized fluid extraction to obtain an extract, performing solid phase extraction on the extract and then eluting to obtain an eluent, and re-dissolving the eluent to obtain a solution to be tested, wherein the condition of the pressurized fluid extraction is 1‰ ammonia water without heating; S2: Performing liquid chromatography-mass spectrometry on the test solution to obtain a mass spectrum, and judging whether the current sludge sample to be tested contains psychotropic narcotic drugs based on the base peak mass-to-charge ratio of the mass spectrum, wherein the chromatographic conditions are: mobile phase A is methanol, mobile phase B is 0.1% formic acid water, and gradient elution; the conditions are: the psychotropic narcotic drugs are one or a combination of two or more of morphine, acetylnorfentanyl and THC-COOH.

2. The method for detecting psychotropic drugs in environmental sludge based on alkaline pretreatment according to claim 1, characterized in that: The method comprises the following steps: taking a sludge sample to be tested and freezing it in a low temperature environment for a period of time, and taking the frozen sludge sample to be tested and dehydrating and drying it.

3. The method for detecting psychotropic drugs in environmental sludge based on alkaline pretreatment according to claim 1, characterized in that: The water content of the sludge sample to be tested after freeze drying is less than 5%, and the freeze drying time is set to be greater than 2 hours.

4. The method for detecting psychotropic drugs in environmental sludge based on alkaline pretreatment according to claim 1, characterized in that: Poly-Sery HLB Pro was selected as the solid phase extraction column.

5. The method for detecting psychotropic drugs in environmental sludge based on alkaline pretreatment according to claim 1, characterized in that: The solid phase extraction column is activated by using methanol at a flow rate of no more than 1 mL / min, and then pure water is added to rinse the solid phase extraction column to obtain an activated solid phase extraction column. The extract is added to the activated solid phase extraction column at a flow rate of 4 mL / min, and the solid phase extraction column is eluted with pure water at a rinsing flow rate of 2 mL / min. Subsequently, the solid phase extraction column is eluted with methanol at an elution flow rate of no more than 1 mL / min to obtain an eluate.

6. The method for detecting psychotropic drugs in environmental sludge based on alkaline pretreatment according to claim 1, characterized in that: The eluate was concentrated by nitrogen blowing and injected into 20% methanol water to obtain the test solution.

7. The method for detecting psychotropic drugs in environmental sludge based on alkaline pretreatment according to claim 1, characterized in that: A triple quadrupole liquid spectrometer was selected, and ACQUITY UPLC HSS T3 was chosen as the chromatographic column.

8. The method for detecting psychotropic drugs in environmental sludge based on alkaline pretreatment according to claim 1, characterized in that: The elution conditions for gradient elution are as follows:

9. The method for detecting psychotropic drugs in environmental sludge based on alkaline pretreatment according to claim 1, characterized in that: The quantitative detection of psychotropic narcotic drugs is carried out by the internal standard method, and the internal standard is the deuterated isotope internal standard of each psychotropic narcotic drug.

10. The method for detecting psychotropic drugs in environmental sludge based on alkaline pretreatment according to claim 1, characterized in that: Psychotropic narcotic drugs of one or more combinations of morphine, acetylnorfentanyl and THC-COOH used in environmental sludge.

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