Method for determining narcotics in sewage by ultra-high performance liquid chromatography-tandem mass spectrometry and application

Abstract

The invention provides a method for determining narcotics in sewage by ultra-high performance liquid chromatography-tandem mass spectrometry and application of the method. The method comprises the following steps: filtering sewage, adjusting the pH value, adding a salting-out reagent, carrying out vortex uniform mixing, extracting, carrying out high-speed centrifugation, taking the supernatant, purifying, detecting in an ultra-high performance liquid chromatography-tandem mass spectrometry multiple reaction ion monitoring mode, and quantifying by an external standard method. The ultra-high performance liquid chromatography-tandem mass spectrometry established by the invention can rapidly and accurately detect multiple drugs in sewage at the same time, and a more efficient detection method is provided for mass sample analysis, so that the purposes of improving the detection efficiency and shortening the case handling time are achieved.

Description

Technical Field

[0001] The invention belongs to the technical field of analysis and testing, and specifically relates to a method for determining drugs in sewage by ultra-high performance liquid chromatography-tandem mass spectrometry and its application. Background Art

[0003] There are many kinds of drugs. If a single indicator test method is used to detect the drug content in samples one by one, the efficiency will undoubtedly be extremely low and the workload will be huge. Therefore, it is particularly important to carry out research on multi-drug detection methods to improve detection efficiency and shorten the case handling time of public security organs. At present, multi-drug detection generally uses capillary electrophoresis mass spectrometry, gas chromatography-mass spectrometry, liquid chromatography-mass spectrometry and other methods for determination. However, the drug content in sewage is extremely low, and the sensitivity of capillary electrophoresis mass spectrometry is relatively low, which cannot meet the daily detection needs. The common method for detecting drugs by gas chromatography-mass spectrometry is to derivatize them and then measure the content of their derivatives. The pretreatment method is cumbersome and the derivatization conditions are strictly controlled, which is not conducive to large-scale rapid detection. Therefore, liquid chromatography-mass spectrometry is the most frequently used method in daily detection. Summary of the invention

[0004] The present invention selects methamphetamine (MAMP), amphetamine (AMP), morphine, 6 - For 11 kinds of drugs including monoacetylmorphine, ketamine, cocaine, norketamine, 3,4-methylenedioxymethamphetamine (MDMA), 3,4-methylenedioxyethylamphetamine (MDEA), 3,4-methylenedioxyamphetamine (MDA), and cannabinol, an ultra-high performance liquid chromatography-tandem mass spectrometry method was established, which can quickly and accurately detect 11 kinds of drugs in sewage at the same time, bringing a more efficient detection method for large-scale sample analysis, so as to achieve the purpose of improving detection efficiency and shortening case handling time.

[0005] One of the purposes of the present invention is to provide a method for determining drugs in sewage by ultra-high performance liquid chromatography-tandem mass spectrometry, comprising:

[0006] (1) After the sewage is centrifuged, the supernatant is filtered and an alkaline solution is added to the filtrate (I) to adjust the pH;

[0007] (2) adding the salting-out reagent, vortexing, and then adding the extraction solvent, vortexing, and centrifuging;

[0008] (3) taking the upper organic phase after centrifugation, adding the adsorbent and vortexing;

[0009] (4) After filtering through an organic phase filter membrane, the mixture is blown almost dry with nitrogen, and after re-dissolving with an organic solvent, the mixture is filtered again through an organic phase filter membrane to obtain a filtrate (II);

[0010] (5) The filtrate (II) is subjected to ultra-high performance liquid chromatography-tandem mass spectrometry for qualitative and quantitative analysis of drugs in the sewage.

[0011] In the test method provided by the present invention, the drugs include methamphetamine (MAMP), amphetamine (AMP), morphine, 6 - At least one of monoacetylmorphine, ketamine, cocaine, norketamine, 3,4-methylenedioxymethamphetamine (MDMA), 3,4-methylenedioxyethylamphetamine (MDEA), 3,4-methylenedioxyamphetamine (MDA), and cannabinol.

[0012] In the test method step (1) provided by the present invention:

[0013] The alkaline compound in the alkaline solution is selected from at least one of sodium hydroxide, potassium hydroxide, sodium carbonate, and sodium sulfide, preferably sodium hydroxide and sodium sulfide, and more preferably, the mass ratio of sodium hydroxide to sodium sulfide is 1:(1-4); the addition of sodium hydroxide and sodium sulfide is beneficial to the extraction of the compound to be tested and avoids the influence of heavy metal ions in sewage; the hydrolysis of sulfide ions is further inhibited under the action of hydroxide ions, and the role of sodium sulfide in removing heavy metal ions can be better exerted.

[0014] The concentration of the alkaline compound in the alkaline solution can be adjusted within a wide range as long as the pH of the filtrate can be adjusted. For example, the concentration of the alkaline compound in the alkaline solution is 0.005 to 0.2 mol / L, preferably 0.01 to 0.05 mol / L. The alkaline solution is added to adjust the pH to 8 to 10, preferably, the pH is 9.

[0015] In step (2) of the test method provided by the present invention:

[0016] The salting-out reagent is sodium chloride and sodium sulfate. Preferably, the mass ratio of sodium chloride to sodium sulfate is 1:(1-5); the combined use of sodium chloride and sodium sulfate can reduce the solubility of the aqueous phase in ethyl acetate and reduce the water content in ethyl acetate; the mass dosage of the salting-out reagent is 10-40wt% of the filtrate (I), preferably 15-35wt%; the added salting-out reagent makes it present an oversaturated state in the sample solution to be tested, thereby improving the extraction efficiency of the compound to be tested;

[0017] The extraction solvent is selected from at least one of ethyl acetate, n-hexane, and dichloromethane, preferably ethyl acetate; the amount of the extraction solvent can be adjusted within a wide range, for example, the volume of the extraction solvent is 0.2 to 2 times the volume of the filtrate (I), preferably 0.8 to 1.2 times.

[0018] In step (3) of the test method provided by the present invention:

[0019] The adsorbent is selected from at least one of ethylenediamine-N-propyl silane silica gel (PSA), silica powder (Si), lipophilic divinylbenzene and hydrophilic N-vinyl pyrrolidone copolymer (HLB), and octadecylsilane bonded silica gel (C18), preferably octadecylsilane bonded silica gel (C18); the amount of the adsorbent can be adjusted within a wide range, for example, based on the volume of the upper organic phase being 1 mL, the amount of the adsorbent is 1 to 30 mg, preferably 5 to 15 mg;

[0020] The oscillation vortexing in step (2) and step (3) can adopt a commonly used oscillation vortexing device and conditions, for example, the oscillation vortexing time is 0.5 to 2 minutes.

[0021] In step (4) of the test method provided by the present invention:

[0022] The organic phase filter membrane is selected from at least one of a polyvinylidene fluoride filter membrane, a polytetrafluoroethylene filter membrane, and a mixed fiber membrane; the pore size of the organic phase filter membrane is 0.1 to 0.8 μm, preferably 0.22 to 0.45 μm;

[0023] The organic solvent is selected from at least one of acetonitrile, water and methanol, preferably acetonitrile;

[0024] The nitrogen blowing near-drying condition is: 30-60°C, preferably 40-50°C.

[0025] The testing method provided by the present invention, the detection conditions of ultra-high performance liquid chromatography are:

[0026] A reverse phase C18 column was used;

[0027] Column temperature 30-40°C;

[0028] Injection volume 2-10 μL;

[0029] Flow rate: 0.1~0.5mL / min;

[0030] Mobile phase A: 0.1% formic acid in water, mobile phase B: 0.1% formic acid / acetonitrile solution;

[0031] The gradient elution conditions were: 0 min, 78%-82% A; 0-3 min, 48%-52% A; 3-5 min, 8-12% A; 5-7 min, 8-12% A; 7-10 min, 78%-82% A.

[0032] The test method provided by the present invention has the following detection conditions for mass spectrometry:

[0033] Electrospray ion source (ESI source), positive ion mode;

[0034] Drying gas temperature: 280-320°C, drying gas flow rate: 4-8 L / min;

[0035] Sheath gas temperature: 250-300°C, sheath gas flow rate: 8-16 L / min;

[0036] Capillary voltage: 3000~4000V, nozzle voltage: 400~600V;

[0037] Scanning mode: multiple reaction ion monitoring (MRM).

[0038] The test method provided by the present invention, the step (5) also includes the step of drawing a standard curve, specifically: preparing at least 3 mixed solutions containing drug standards of different concentrations for measurement, and drawing a standard curve with the quantitative ion pair peak area of ​​each drug standard as the ordinate and the mass concentration of each drug standard as the abscissa; wherein the drug standard includes methamphetamine, amphetamine, morphine, O 6 - At least one of monoacetylmorphine, ketamine, cocaine, norketamine, 3,4-methylenedioxymethamphetamine, 3,4-methylenedioxyethylamphetamine, 3,4-methylenedioxyamphetamine, and cannabinol;

[0039] Preferably, in the drug-containing standard solution, the mass concentrations of 3,4-methylenedioxyethyl amphetamine (MDEA), ketamine, and cocaine are independently 0.05 to 1.0 ng / mL, and the mass concentrations of morphine, 6 -The mass concentration of monoacetylmorphine, 3,4-methylenedioxyamphetamine (MDA), and norketamine is independently 0.5 to 10 ng / mL, the mass concentration of methamphetamine (MAMP) and amphetamine (AMP) is independently 0.1 to 2.0 ng / mL, the mass concentration of 3,4-methylenedioxymethamphetamine (MDMA) is 0.025 to 0.5 ng / mL, and the mass concentration of cannabinol is 10 to 200 ng / mL.

[0040] The second purpose of the present invention is to provide a method for determining drugs in sewage by the above-mentioned ultra-high performance liquid chromatography-tandem mass spectrometry, which is used in the rapid detection of drug residues in sewage, and is particularly suitable for the rapid detection of large quantities of sewage.

[0041] The present invention adds salting-out reagent to the sewage after filtering, vortex mixing, and then extracts with organic solvent. After high-speed centrifugation, the supernatant is purified, concentrated and fixed, and detected by ultra-high performance liquid chromatography-tandem mass spectrometry multiple reaction ion monitoring mode (multiple reaction monitoring, MRM), and quantified by external standard method. The results show that in the range of 0.025-10 ng / mL, various chemical drugs such as methamphetamine have a good linear relationship, and the correlation coefficient (r) is greater than 0.99. At a concentration of 3 times the addition level, the average recovery rate of various chemical drugs such as methamphetamine is 64.7%-108.2%, the relative standard deviation (relative standard deviation, RSD) is 0.3%-11.3%, and the quantitative limit of various chemical drugs such as methamphetamine in sewage is 0.25-100 ng / L. The test method provided by the present invention is simple and fast to operate, consumes less reagents and consumables, and has high sensitivity. It is suitable for rapid processing of large quantities of sewage and the detection of various chemical drugs such as methamphetamine residues. BRIEF DESCRIPTION OF THE DRAWINGS

[0042] Figure 1 The mass spectra of 11 kinds of drugs obtained in Example 1, a: AMP; b: cannabinol; c: O 6 -monoacetylmorphine; d: cocaine; e: ketamine; f: MAMP; g: MDA; h: MDEA; i: MDMA; j: morphine; k: norketamine.

[0043] Figures 2 to 4 They are respectively the extraction efficiencies of the 11 drug compounds at different pH values ​​in Examples 1 to 3, the horizontal axis is the 11 drug compounds, and the vertical axis is the extraction efficiency (%). DETAILED DESCRIPTION

[0044] The present invention is described in detail below in conjunction with specific embodiments. It is necessary to point out that the following embodiments are only used to further illustrate the present invention and cannot be understood as limiting the scope of protection of the present invention. Some non-essential improvements and adjustments made to the present invention by those skilled in the art based on the contents of the present invention still fall within the scope of protection of the present invention.

[0045] The test instruments and test conditions used in the examples are as follows:

[0046] Methamphetamine (MAMP), amphetamine (AMP), morphine, O 6-Monoacetylmorphine, ketamine, cocaine, norketamine, 3,4-methylenedioxymethamphetamine (MDMA), 3,4-methylenedioxyethylamphetamine (MDEA), 3,4-methylenedioxyamphetamine (MDA), cannabinol (1000 μg / mL, Cerilliant, USA); acetonitrile (chromatographic grade, Supelco, USA); sodium hydroxide, sodium sulfide, sodium chloride, sodium sulfate (analytical grade, Nanjing Chemical Reagent Co., Ltd.), C18 powder (Tianjin Bona Aiger Technology Co., Ltd.).

[0047] WH-3 oscillator (Shanghai Huxi Analytical Instrument Factory Co., Ltd.); KDC-160HR high-speed centrifuge (Anhui Zhongke Zhongjia Scientific Instrument Co., Ltd.); AutoVap S60 fully automatic nitrogen blowdown instrument (ATR Company, USA); Agilent 1290-6470B liquid chromatography-mass spectrometry (Agilent Company, USA).

[0048] Example 1

[0049] Qualitative analysis of samples

[0050] (1) Sample pretreatment

[0051] 11 kinds of drug compounds (methamphetamine, amphetamine, morphine, O 6 -monoacetylmorphine, ketamine, cocaine, norketamine, 3,4-methylenedioxymethamphetamine, 3,4-methylenedioxyethylamphetamine, 3,4-methylenedioxyamphetamine, cannabinol), as sewage sample 1#.

[0052] Take 100mL of sewage and centrifuge at 10000r / min for 5min, then take the supernatant and filter it. Accurately measure 10mL of filtrate in a 50mL plastic centrifuge tube, add 0.02mol / L sodium hydroxide / sodium sulfide mixed solution (the mass ratio of sodium hydroxide and sodium sulfide is 1:2) to adjust the sample pH to 9, add 2.5g of sodium chloride and sodium sulfate mixture (the mass ratio of sodium chloride and sodium sulfate is 1:3), oscillate and vortex for 1min, then add 10mL of ethyl acetate, oscillate and vortex for 2min, centrifuge at 10000r / m for 3min, take all the upper organic phase in a 10mL centrifuge tube, add 100mgC18 powder, oscillate and vortex for 1min, then pass through a 0.22μm polytetrafluoroethylene filter in a 10mL nitrogen blowpipe, blow nitrogen to near dryness in a 40℃ water bath, add 100μL of acetonitrile in the nitrogen blowpipe, oscillate and vortex, pass through a 0.22μm polytetrafluoroethylene filter, and bottle for use.

[0053] (2) Chromatographic conditions

[0054] An Agilent Poroshell 120EC-C18 (2.1x100mm, 2.7μm) chromatographic column was used, with a column temperature of 35°C and an injection volume of 5μL; a flow rate of 0.3mL / min, and a 0.1% formic acid aqueous solution (A): 0.1% formic acid / acetonitrile solution (B) as the mobile phase. The elution conditions are shown in Table 1.

[0055] Table 1. Gradient elution conditions

[0056] Time (min) A(％) B(％) 0 80 20 3 50 50 5 10 90 7 10 90 10 80 20

[0057] (3) Mass spectrometry conditions

[0058] Electrospray ion source (ESI source), positive ion mode, drying gas temperature: 300°C, drying gas flow rate: 6 L / min, sheath gas temperature: 280°C, sheath gas flow rate: 12 L / min, capillary voltage: 3500 V, nozzle voltage: 500 V, scanning mode: multiple reaction ion monitoring (MRM), the ion detection conditions of 11 chemicals are shown in Table 2. The mass spectra of the 11 drugs detected are shown in Figure 1 .

[0059] Table 2. Detection conditions of multiple reactive ions for 11 drugs

[0060]

[0061] Note: * indicates quantitative ion.

[0062] Quantitative analysis of samples

[0063] (4) Draw a standard curve

[0064] Five mixed standard solutions #1 to #5 containing 11 drug standards of different concentrations were prepared in sequence. In the mixed standard solutions #1 to #5, the mass concentrations of MDEA, ketamine, and cocaine were the same, which were 0.05, 0.1, 0.2, 0.5, and 1.0 ng / mL, respectively; morphine, O 6 -The mass concentrations of monoacetylmorphine, MDA, and norketamine are the same, which are 0.5, 1.0, 2.0, 5.0, and 10 ng / mL, respectively; the mass concentrations of AMP and MAMP are the same, which are 0.1, 0.2, 0.4, 1.0, and 2.0 ng / mL, respectively; the mass concentrations of MDMA are 0.025, 0.05, 0.1, 0.25, and 0.5 ng / mL; and the mass concentrations of cannabinol are 10, 20, 40, 100, and 200 ng / mL. The above mixed standard solution was measured, and the peak area of ​​each drug quantitative ion was used as the ordinate (Y) and the mass concentration was used as the abscissa (x). The standard curve was drawn to obtain the linear regression equation and correlation coefficient (r) shown in Table 3.

[0065] Table 3 Detection limit, quantification limit and linear parameters

[0066]

[0067] (5) Quantitative analysis of 11 drugs in sewage

[0068] The peak area of ​​the quantitative ion of each drug compound measured in sewage sample 1# is substituted into the standard curve to obtain the content of each drug compound in the sewage sample, as shown in Table 4.

[0069] Table 4 Contents of 11 drugs in sample 1#

[0070]

[0071] (6) Precision test

[0072] Eleven compounds in the blank wastewater sample were spiked with three times the quantitative limit and measured six times in parallel according to the set instrument conditions (test conditions were the same as in Example 1). The relative standard deviation (RSD) of the measured values ​​was 1.5% to 7.0%. The detailed results are shown in Table 5. This shows that the above method has good precision.

[0073] Table 5 Precision test results (n = 6)

[0074] Compound Added value (ng / L) Precision RSD (%) MDMA 0.75 5.5 MDEA 1.5 2.5 Ketamine 1.5 3.5 cocaine 1.5 6.8 AMP 3 4.4 MAMP 3 2.5 morphine 15 7.0 <![CDATA[O 6 -Monoacetylmorphine]]> 15 2.4 MDA 15 1.5 Norketamine 15 2.3 Cannabidiol 300 5.5

[0075] (7) Repeatability test

[0076] Eleven compounds in the blank wastewater samples were spiked with three times the limit of quantification, and the pretreatment method of Example 1 was used in parallel for 6 times. The relative standard deviation (RSD) of the measured values ​​was 2.4% to 9.9%. The detailed results are shown in Table 6. This shows that the above method has good repeatability.

[0077] Table 6 Repeatability test results (n=6)

[0078] Compound Added value (ng / L) RSD(%) MDMA 0.75 5.8 MDEA 1.5 5.7 Ketamine 1.5 6.7 cocaine 1.5 9.9 AMP 3 2.9 MAMP 3 2.6 morphine 15 2.7 <![CDATA[O 6 -Monoacetylmorphine]]> 15 5.4 MDA 15 2.9 Norketamine 15 2.4 Cannabidiol 300 5.1

[0079] (8) Accuracy test

[0080] The blank wastewater samples were taken for spiked experiments at three concentrations, and each concentration was measured three times in parallel. The average spiked recovery results are shown in Table 7. The spiked recovery and RSD of the present invention both prove the accuracy and feasibility of the test method of the present invention.

[0081] Table 7 Recovery test results (n=3)

[0082]

[0083] The results in Tables 3 to 7 show that in the range of 0.025 to 10 ng / mL, methamphetamine and other chemical drugs have a good linear relationship, and the correlation coefficient (r) is greater than 0.99. At the 3-fold concentration addition level, the average recovery rate of methamphetamine and other chemical drugs is 64.7% to 108.2%, and the relative standard deviation (RSD) is 0.3% to 11.3%. The quantitative limit of methamphetamine and other chemical drugs in sewage is 0.25 to 100 ng / L.

[0084] Embodiment 2-3

[0085] Different amounts of 11 drug compounds were added to the sewage, and the sample pretreatment and testing steps in Example 1 were used. The quantitative analysis results obtained are shown in Table 8.

[0086] Table 8

[0087]

[0088] Embodiment 4-5

[0089] The sample pretreatment and test steps in Example 1 were used, except that sodium hydroxide / sodium sulfide solution was used to adjust the pH of the sample solution to 8 and 10, respectively. The quantitative limit recovery results are shown in Figure 2 , 4 It can be seen that when the pH of the sample solution is 9, the recovery rate of each chemical poison is higher.

[0090] Embodiment 6-7

[0091] The sample pretreatment and test steps in Example 1 were adopted, except that n-hexane and dichloromethane were used as extraction solvents instead of ethyl acetate in Examples 6-7, and the recovery rates of 11 compounds were tested, as shown in Table 9. The results in Table 9 show that when n-hexane was used as the solvent, the sample was extracted by salting out, and the extract was relatively clear, but the extraction efficiency was poor, and only the quantitative limit recovery rate of cannabinol was good. When dichloromethane was used as the solvent, the extract was slightly turbid, and the extraction efficiency was relatively poor. Only the quantitative limit recovery rates of three drugs, norketamine, 3,4-methylenedioxyamphetamine, and cannabinol, were good. When ethyl acetate was used as the solvent, the extract was relatively clear, and the quantitative limit recoveries of the 11 compounds could meet the experimental requirements.

[0092] Table 9

[0093]

[0094] The present invention uses a sodium chloride / sodium sulfate supersaturated sample solution and an organic solvent extraction method to extract the target substance, and establishes a liquid chromatography-tandem mass spectrometry method for rapidly determining 11 chemical drug residues in sewage, which can accurately and simultaneously perform qualitative and quantitative analysis on the 11 chemical drugs. The method uses C18 powder dispersion solid phase extraction as a purification method in the pretreatment process. The method is fast and simple, requires a small amount of samples, consumes low amounts of reagents, can efficiently process large quantities of samples to meet the requirements of rapid laboratory response, and can meet the requirements for detecting chemical drug residues in sewage in terms of precision, repeatability, accuracy, and sensitivity.

Claims

1. A method for determining drugs in sewage by ultra-high performance liquid chromatography-tandem mass spectrometry, comprising: (1) After the sewage is centrifuged, the supernatant is filtered and an alkaline solution is added to the filtrate (I) to adjust the pH; (2) adding the salting-out reagent, vortexing, and then adding the extraction solvent, vortexing, and centrifuging; (3) taking the upper organic phase after centrifugation, adding the adsorbent and vortexing; (4) After filtering through an organic phase filter membrane, the mixture is blown almost dry with nitrogen, and after re-dissolving with an organic solvent, the mixture is filtered again through an organic phase filter membrane to obtain a filtrate (II); (5) The filtrate (II) is subjected to ultra-high performance liquid chromatography-tandem mass spectrometry for qualitative and quantitative analysis of drugs in the sewage.

2. The method according to claim 1, It is characterized in that The drugs include methamphetamine, amphetamine, morphine, 6 - At least one of monoacetylmorphine, ketamine, cocaine, norketamine, 3,4-methylenedioxymethamphetamine, 3,4-methylenedioxyethylamphetamine, 3,4-methylenedioxyamphetamine, and cannabinol.

3. The method according to claim 1, It is characterized in that In the step (1): The alkaline compound in the alkaline solution is selected from at least one of sodium hydroxide, potassium hydroxide, sodium carbonate and sodium sulfide, preferably sodium hydroxide and sodium sulfide, more preferably, the mass ratio of sodium hydroxide to sodium sulfide is 1:(1-4); and / or, The concentration of the alkaline compound in the alkaline solution is 0.005 to 0.2 mol / L, preferably 0.01 to 0.05 mol / L; and / or, Add alkaline solution to adjust the pH to 8-10.

4. The method according to claim 1, It is characterized in that In the step (2): The salting-out reagent is sodium chloride and sodium sulfate, preferably, the mass ratio of sodium chloride to sodium sulfate is 1:(1-5); and / or, The mass amount of the salting-out reagent is 10-40wt%, preferably 15-35wt% of the filtrate (I); and / or, The extraction solvent is selected from at least one of ethyl acetate, n-hexane and dichloromethane, preferably ethyl acetate; and / or, The volume of the extraction solvent is 0.2 to 2 times, preferably 0.8 to 1.2 times, the volume of the filtrate (I).

5. The method according to claim 1, It is characterized in that In the step (3): The adsorbent is selected from at least one of ethylenediamine-N-propyl silane silica gel, silica powder, lipophilic divinylbenzene and hydrophilic N-vinyl pyrrolidone copolymer), octadecylsilane bonded silica gel, preferably octadecylsilane bonded silica gel; and / or, Based on the volume of the upper organic phase being 1 mL, the amount of the adsorbent used is 1 to 30 mg, preferably 5 to 15 mg.

6. The method according to claim 1, It is characterized in that In the step (4): The organic phase filter membrane is selected from at least one of a polyvinylidene fluoride filter membrane, a polytetrafluoroethylene filter membrane, and a mixed fiber membrane; and / or, The pore size of the organic phase filter membrane is 0.1 to 0.8 μm, preferably 0.22 to 0.45 μm; and / or, The organic solvent is selected from at least one of acetonitrile, water and methanol, preferably acetonitrile; and / or, The nitrogen blowing near-drying condition is: 30-60°C, preferably 40-50°C.

7. The method according to claim 1, It is characterized in that The detection conditions of ultra-high performance liquid chromatography are: A reverse phase C18 column was used; Column temperature 30-40°C; Injection volume 2-10 μL; Flow rate: 0.1~0.5mL / min; Mobile phase A: 0.1% formic acid in water, mobile phase B: 0.1% formic acid / acetonitrile solution; The gradient elution conditions were: 0 min, 78%-82% A; 0-3 min, 48%-52% A; 3-5 min, 8-12% A; 5-7 min, 8-12% A; 7-10 min, 78%-82% A.

8. The method according to claim 1, It is characterized in that The detection conditions of mass spectrometry are: electrospray ion source, positive ion mode; Drying gas temperature: 280~320℃, drying gas flow rate: 4~8L / min; Sheath gas temperature: 250-300°C, sheath gas flow rate: 8-16 L / min; Capillary voltage: 3000~4000V, nozzle voltage: 400~600V; Scanning mode: multiple reaction ion monitoring.

9. The method according to claim 1, It is characterized in that The step (5) further comprises the step of drawing a standard curve, which is specifically: preparing at least three mixed solutions containing drug standards of different concentrations for determination, and drawing a standard curve with the quantitative ion pair peak area of ​​each drug standard as the ordinate and the mass concentration of each drug standard as the abscissa; wherein the drug standards include methamphetamine, amphetamine, morphine, 6 - At least one of monoacetylmorphine, ketamine, cocaine, norketamine, 3,4-methylenedioxymethamphetamine, 3,4-methylenedioxyethylamphetamine, 3,4-methylenedioxyamphetamine, and cannabinol; Preferably, in the mixed solution containing the drug standard, the mass concentration of 3,4-methylenedioxyethyl amphetamine, ketamine, and cocaine is independently 0.05 to 1.0 ng / mL, and the mass concentration of morphine, O 6 -The mass concentration of monoacetylmorphine, 3,4-MDMA, and norketamine is independently 0.5 to 10 ng / mL, the mass concentration of methamphetamine and amphetamine is independently 0.1 to 2.0 ng / mL, the mass concentration of 3,4-MDMA is 0.025 to 0.5 ng / mL, and the mass concentration of cannabinol is 10 to 200 ng / mL.

10. A method for determining drugs in sewage by ultra-high performance liquid chromatography-tandem mass spectrometry as described in any one of claims 1 to 9, which is used in the rapid detection of drug residues in sewage, and is particularly suitable for the rapid detection of large quantities of sewage.

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