CN113219102A - Method for measuring content of toxic substances and metabolites thereof in sewage - Google Patents
Method for measuring content of toxic substances and metabolites thereof in sewage Download PDFInfo
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N30/14—Preparation by elimination of some components
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/62—Detectors specially adapted therefor
- G01N30/72—Mass spectrometers
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N2030/062—Preparation extracting sample from raw material
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N30/14—Preparation by elimination of some components
- G01N2030/146—Preparation by elimination of some components using membranes
Abstract
The invention discloses a method for measuring the content of drugs and metabolites thereof in sewage, which comprises the following steps: step 1, adjusting the pH value of a sewage sample to be less than 2, and filtering impurities for analysis; step 2, solid phase extraction: activating a solid-phase extraction column by using methanol and ultrapure water in sequence before extraction, uniformly mixing the mixed deuterated internal standard working solution with a sample to be detected, transferring the mixed deuterated internal standard working solution into the solid-phase extraction column, leaching the mixed solid-phase extraction column by using the ultrapure water, vacuumizing the solid-phase extraction column, eluting the mixed solid-phase extraction column by using a 5% ammonia methanol solution, vacuumizing the solid-phase extraction column, and collecting eluent; blowing the eluent to near dryness, adding 0.1% formic acid water solution, mixing well, filtering with 0.22 μm nylon microporous membrane, and using as sample extract for instrument detection; and 3, performing liquid chromatography-tandem mass spectrometry on the extract of the test material sample to detect the content of each drug and metabolites thereof. The invention basically comprises various drugs involved in the prior case so as to meet the requirements of practical work.
Description
Technical Field
The invention relates to the technical field of chemical detection, in particular to a method for measuring the content of a drug and a metabolite thereof in sewage.
Background
The drug is a compound having strong exciting or inhibiting effect on human central nervous system, and mainly comprises opium such as morphine, cocaine, heroin and methadone, amphetamines such as amphetamine and methamphetamine (methamphetamine), ecstasy, ketamine, norketamine and the like. Besides, the drugs in the sewage can also come from waste water illegally stolen by a virus manufacturing factory and drugs which are washed away by a sewer pipe as damage evidences during the assault investigation period. The drug and the metabolite thereof have better stability in the sewage, and the consumption of a certain class of drugs of a unit population can be obtained by analyzing the concentrations of various drug and the metabolite thereof in the sewage and correcting the product of the total amount of the sewage and the metabolic rate of the drugs. Therefore, the abuse condition of drugs in a certain area can be objectively evaluated by collecting the domestic sewage sample and analyzing the content of the original drugs or metabolites of the drugs in the domestic sewage sample.
Due to the human metabolism and the dilution effect of the receiving water body, the actual concentration of drugs and metabolites thereof in the sewage is extremely low and exists in concentration level of nanograms per liter. In addition, the actual water environment components are complex and can seriously interfere the detection, so that when a method for detecting a plurality of drugs and metabolites thereof in sewage is established, a detection instrument with higher sensitivity is required, a proper pretreatment method with high recovery rate is also required, the impurity interference in an environmental sample is reduced as much as possible, and trace target substances are selectively enriched at high times, so that the sensitivity of analysis is ensured.
Disclosure of Invention
The invention aims to provide a method for measuring the content of drugs and metabolites thereof in sewage, aiming at the problems in the detection of the drugs and the metabolites thereof in the prior art.
The technical scheme adopted for realizing the purpose of the invention is as follows:
a method for measuring the content of a toxic substance and a metabolite thereof in sewage comprises the following steps:
step 1, adjusting the pH value of a sewage sample to be less than 2, and filtering impurities for analysis;
step 2, solid phase extraction: activating a solid-phase extraction column by using methanol and ultrapure water in sequence before extraction, uniformly mixing the mixed deuterated internal standard working solution with a sample to be detected, transferring the mixed deuterated internal standard working solution into the solid-phase extraction column, leaching the mixed solid-phase extraction column by using the ultrapure water, vacuumizing the solid-phase extraction column, eluting the mixed solid-phase extraction column by using a 5% ammonia methanol solution, vacuumizing the solid-phase extraction column, and collecting eluent;
blowing the eluent to near dryness, adding 0.1% formic acid water solution, mixing well, filtering with 0.22 μm nylon microporous membrane, and using as sample extract for instrument detection;
and 3, performing liquid chromatography-tandem mass spectrometry on the extract of the test material sample to detect the content of each drug and metabolites thereof.
In the above technical scheme, the eluent in the step 2 is placed on a nitrogen-blowing concentrator and blown to be nearly dry.
In the above technical solution, the drug and its metabolites include Methamphetamine (METH), Amphetamine (AMP), Ketamine (KET), Norketamine (NK), Morphine (MOR), O6-monoacetylmorphine (O)6) Codeine (COD), cocaine (COC), Benzoylidenine (BE), 3, 4-Methylenedioxyamphetamine (MDA), 3, 4-methylenedioxymethamphetamine (MDMA), Methylenedioxypyrovalerone (MDPV), p-methoxymethylphenylamine (4-METH), Methoxyephedrine (MEP), 1- (3-chlorophenyl) piperazine (1-3CPH), 2C-D, Tramadol (TMD), (pseudo) Ephedrine (EPH), Cotinine (COT), Methylcardinone (MC), Fentanyl (FEN), Valerylfentanyl (VAL), Furanfentanyl (FUR) and/or Carfentanyl (CAR).
In the technical scheme, the internal standard substance comprises methamphetamine-D5 (METH-D5), amphetamine-D11 (AMP-D11), ketamine-D4 (KET-D4), norketamine-D4 (NK-D4), morphine-D3 (MOR-D3), O-D46-monoacetylmorphine-D3 (O)6-D3), codeine-D3 (COD-D3), cocaine-D3 (COC-D3), benzoylekonin-D3 (BE-D3),3, 4-methylenedioxyamphetamine-D5 (MDA-D5), 3, 4-methylenedioxymethamphetamine-D5 (MDMA-D5), methylenedioxypyrrolpentanone-D8 (MDPV-D8), tramadol-D3 (TMD-D3), ephedrine-D3 (EPH-D3), methcathinone-D3 (MC-D3), cotinine-D3 (COT-D3) and/or fentanyl-D5 (FEN-D5).
In the technical scheme, in the step 1, concentrated hydrochloric acid is added into the sewage sample to adjust the pH value.
In the technical scheme, in the step 1, a solvent filter and a 0.45-micron glass fiber filter membrane are used for filtration. The fiber filter membrane is used for filtering, so that the impurities can be filtered, and the molecules to be detected cannot be filtered.
In the technical scheme, the flow rate is controlled to be 1.0mL/min during leaching and elution in the step 2, and the solid-phase extraction column is pumped for not less than 30min during vacuum pumping.
In the above technical scheme, in the step 2, the eluent is placed on a nitrogen-blowing concentrator and blown to be nearly dry at a temperature of not higher than 40 ℃.
In the technical scheme, the chromatographic column of the liquid chromatogram is a C18 column.
In the above technical scheme, the liquid chromatography conditions are as follows:
(1) a chromatographic column: ACQUITY UPLC BEH C18 column, (2.1 mm. times.100 mm,1.7 μm), column temperature: at 40 ℃.
(2) Mobile phase: mobile phase a phase: 20mmol/L ammonium acetate and 0.1% aqueous formic acid, mobile phase B: 0.1% formic acid acetonitrile solution; flow rate: 0.4 mL/min.
(3) Sample introduction amount: 10 μ L.
(4) Gradient elution conditions: design and adjustment according to different bonded phase chromatographic columns, for C18Bonded phase chromatography column, performed in the manner of the table below:
in the technical scheme, the mass spectrum adopts positive ion mode (ESI +) scanning of electrospray ionizer mass spectrum and multiple reaction ion mode monitoring (MRM).
In the technical scheme, the ion spray voltage of the mass spectrometer is 1000V; the ion source temperature is 150 ℃; desolventizing temperature: 350 ℃; desolventizing air flow rate: 800L/Hr, taper hole air flow rate: 150L/Hr; and (4) directly feeding samples, and then screening parent ions and child ions, and screening the taper hole voltage and collision energy to obtain the maximum ion strength and keep the collision dissociation energy stable.
Compared with the prior art, the invention has the beneficial effects that:
1. the invention overcomes the defect that only one or a few drugs can be measured in the prior art, and provides a liquid chromatogram-tandem mass spectrum combined method which can effectively detect the content of a plurality of drugs in sewage.
2. The invention analyzes the 25 drugs and the metabolites thereof by a liquid chromatogram-tandem mass spectrometer, and can realize the simultaneous detection of the 25 drugs and the metabolites thereof after confirming the retention time, the molecular ion peak (parent ion/child ion pair), the abundance ratio of the molecular ion peak, the signal-to-noise ratio and other parameters, thereby improving the accuracy and greatly saving the detection time.
3. The method has the advantages that the recovery rate is high, different solid-phase extraction activation, leaching and elution conditions and different redissolving solvents and microporous filter membrane selections are optimally selected, 25 kinds of drugs and metabolites thereof are measured, and the recovery rate is 76.4% -127.0% (the recovery rate is calculated by the following method that a mixed standard working solution is added into a blank substrate such as tap water, and the ratio of the concentration detected by pretreatment and an instrument to the added concentration is the recovery rate), so that the method is superior to other pretreatment conditions and methods.
4. The method has the advantages of high accuracy, high sensitivity, good qualitative capability and good selectivity by adopting a liquid chromatography-tandem mass spectrometry combined method, and reduces matrix interference, thereby improving the accuracy of analysis. The method can better meet the analysis requirements of drug and metabolite detection thereof, and in addition, the method meets the current requirements of drug abuse monitoring in China, and is expected to become an important tool for monitoring illegal drug consumption in the future.
Drawings
FIG. 1 is a chromatogram of AMP.
Fig. 2 is a chromatogram of METH.
FIG. 3 is a chromatogram of EPH.
Fig. 4 is a chromatogram of BZP.
FIG. 5 is a chromatogram of COT.
FIG. 6 is a chromatogram of a MEP.
FIG. 7 is a chromatogram of MDA.
FIG. 8 is a chromatogram of 4-METH.
Figure 9 is a chromatogram of MDMA.
FIG. 10 is a chromatogram of 2C-D.
FIG. 11 is a chromatogram of 1-3 CPH.
Fig. 12 is a chromatogram of NK.
Figure 13 is a chromatogram of KET.
FIG. 14 is a chromatogram of TMD.
FIG. 15 is a chromatogram of MDPV.
FIG. 16 is a chromatogram of MOR.
FIG. 17 is a chromatogram of BE.
FIG. 18 is a chromatogram of COD.
FIG. 19 is a chromatogram of COC.
FIG. 20 is O6The chromatogram of (2).
FIG. 21 is a chromatogram of FEN.
FIG. 22 is a chromatogram of VAL.
FIG. 23 is a chromatogram of FUR.
FIG. 24 is a chromatogram of CAR.
FIG. 25 is a chromatogram of MC (MC is the peak at 2.50 in the drawing)
Detailed Description
The present invention will be described in further detail with reference to specific examples. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Example 1
The invention provides a method for measuring a plurality of drugs in sewage, which takes an added sample as a control, adds an isotope internal standard into a filtered sewage sample, performs extraction, purification and concentration, adopts a liquid chromatogram-mass spectrometer for detection, performs qualitative analysis by retention time and mass spectrum characteristic fragment ions, and performs quantitative analysis by the isotope internal standard method.
29 Tianjin sewage treatment plants are selected as analysis objects for concentration determination, and the analysis method and the effect are as follows:
stock solution (method for establishing working curve, yield and quality of liquid)
Preparing a standard substance stock solution: mixing 0.1mg/mL or 1mg/mL standard substance of the target compound, diluting with methanol to 5 μ g/mL, mixing, sealing, and storing at-20 deg.C in refrigerator. The effective period is 6 months. The mixed standard working solutions of other concentrations used in the experiment were each obtained by diluting 5. mu.g/mL of the mixed standard working solution with 0.1% aqueous formic acid.
Preparing an internal standard substance stock solution: taking 0.1mg/mL or 1mg/mL internal standard of the target compound, mixing, diluting with methanol to 5 μ g/mL, mixing, sealing, and storing in a refrigerator at-20 deg.C (freezing). And (3) transferring the mixed deuterated internal standard working solution of 5 mu g/mL, diluting the mixed deuterated internal standard working solution with methanol to 25ng/mL, uniformly mixing, sealing, and storing in a refrigerator at 0-5 ℃ for later use.
Method
2.1 sample pretreatment
And (3) filtering: unfreezing and fully shaking the sewage material sample, adding concentrated hydrochloric acid to adjust the pH value to be less than 2, filtering by using a solvent filter and a 0.45 mu m glass fiber filter membrane, and transferring 50mL of filtrate to a plastic wide-mouth bottle for analysis.
Solid phase extraction process: before extraction, a solid phase extraction column (
PRIME MCX column (150mg, 6CC)) was activated with 6mL of methanol followed by 6mL of ultrapure water (methanol was added during activation to open the functional groups bound to the adsorbent and allow them to function sufficiently and remove possible interferences on the adsorbent; the water is used for mixing with the sample solutionPhase dissolution and equilibration) were carried out, and the activation flow rate was 1.0 mL/min. In a plastic jar containing 50mL of the filtrate, 100. mu.l of the mixed deuterated internal standard working solution at 25ng/mL was added and mixed by vortexing. Transferring to a solid phase extraction column, controlling the flow rate of the column to be 1.0mL/min, after the sample loading is finished, rinsing the plastic bottle with 1mL of ultrapure water, and transferring to the solid phase extraction column. And (4) carrying out leaching by using ultrapure water with the flow rate of 1.0mL/min, and vacuumizing the solid-phase extraction column for 30min, wherein the leaching aims at removing interferents to the maximum extent, and simultaneously does not wash off a target object adsorbed on the solid-phase extraction column, and a balance point needs to be found between the recovery rate and the purification effect when the leaching solution is selected. Eluting with 4mL of 5% ammonia methanol solution (the purpose of elution is to allow the solvent with stronger elution ability to pass through the adsorbent, interrupt the acting force between the adsorbent and the retained target, and allow the target to flow out of the solvent), controlling the flow rate at 1.0mL/min, vacuum-pumping the solid phase extraction column for 30min, and collecting the eluent.
And (3) concentrating: blowing the eluate on a nitrogen-blowing concentrator at 40 deg.C to near dryness, adding 250 μ L0.1% formic acid water solution, vortex for 3min, mixing, filtering with 0.22 μm nylon microporous membrane, and making into sample extractive solution for instrument detection.
The determination process comprises the following steps: and transferring the redissolved sample to a brown sample introduction bottle for liquid chromatography-tandem mass spectrometry.
2.2 apparatus conditions
2.2.1 liquid chromatography conditions
(1) A chromatographic column: ACQUITY UPLC BEH C18 column, (2.1 mm. times.100 mm,1.7 μm), column temperature: at 40 ℃.
(2) Mobile phase: mobile phase a phase: 20mmol/L ammonium acetate and 0.1% aqueous formic acid, mobile phase B: 0.1% formic acid acetonitrile solution; flow rate: 0.4 mL/min.
(3) Sample introduction amount: 10 μ L.
(4) Gradient elution conditions: the design and adjustment are carried out according to different bonded phase chromatographic columns, and for the C18 bonded phase chromatographic column, the following modes can be referred to:
2.2.2 Mass Spectrometry conditions
The mass spectrum conditions are as follows: positive ion mode (ESI) using electrospray ionizer mass spectrometry+) Scanning, multiple reactive ion mode monitoring (MRM); the ion spray voltage of the mass spectrometer is 1000V; the ion source temperature is 150 ℃; desolventizing temperature: 350 ℃; desolventizing air flow rate: 800L/Hr, taper hole air flow rate: 150L/Hr; and (4) directly feeding samples, and then screening parent ions and child ions, and screening the taper hole voltage and collision energy to obtain the maximum ion strength and keep the collision dissociation energy stable.
By adopting the scheme, the retention time, the values of three pairs or two pairs of parent ions/daughter ions and the detection limit in sewage of the rechecking detection steps of the 25 drugs and the metabolites thereof are shown in table 2.
Table 2 part of the experimental parameters
Example 2
And taking tap water with the same amount as the material sample to be detected, and operating in parallel with the material sample to be detected to obtain a blank sample extracting solution for instrument detection. And (3) adding and mixing tap water with the same amount as the sample to be detected with the standard working solution to ensure that the concentration of 25 substances is 500ng/L, 100ng/L, 50ng/L, 10ng/L, 5ng/L and 1ng/L to serve as the added samples, and operating in parallel with the sample to be detected to obtain an added sample extracting solution for instrument detection. The concentration (X) of each target in the wastewater was subjected to linear regression with the ratio (Y) of the peak area of each target to the peak area of the internal standard to obtain a linear equation for each target, the result being shown as the linearity (r) in Table 22) As shown.
Example 3
The invention is applied to actual monitoring, concentration of target compounds in samples collected by 29 sewage treatment plants is measured, and the results are shown in the following table;
the sampling method comprises the steps of collecting the sample once every 2 hours, and uniformly mixing 12 instantaneous samples collected 24 hours a day in equal volume to obtain 900mL of mixed samples a day. All samples use TC-8000D portable full-automatic equal proportion water quality sampler | refrigeration type water sampler produced by Qingdao environment protection equipment limited. Each sewage treatment plant samples for 7 days, and the detection is carried out once a day, and the following data are the range of 7 sample detection values.
Comparative example
The recovery rates were as shown in the following table by changing the conditions of activation, elution, microfiltration, and microfiltration membranes according to the present invention.
In the comparative examples, the recovery rates were not as high as those of the present invention.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. A method for measuring the content of a toxic substance and a metabolite thereof in sewage is characterized by comprising the following steps:
step 1, adjusting the pH value of a sewage sample to be less than 2, and filtering impurities for analysis;
step 2, solid phase extraction: activating a solid-phase extraction column by using methanol and ultrapure water in sequence before extraction, uniformly mixing the mixed deuterated internal standard working solution with a sample to be detected, transferring the mixed deuterated internal standard working solution into the solid-phase extraction column, leaching the mixed solid-phase extraction column by using the ultrapure water, vacuumizing the solid-phase extraction column, eluting the mixed solid-phase extraction column by using a 5% ammonia methanol solution, vacuumizing the solid-phase extraction column, and collecting eluent;
blowing the eluent to near dryness, adding 0.1% formic acid water solution, mixing well, filtering with 0.22 μm nylon microporous membrane, and using as sample extract for instrument detection;
and 3, performing liquid chromatography-tandem mass spectrometry on the extract of the test material sample to detect the content of each drug and metabolites thereof.
2. The method of claim 1, wherein the drugs and their metabolites comprise methamphetamine, amphetamine, ketamine, norketamine, morphine, O6-monoacetylmorphine, codeine, cocaine, benzoylidenecrine, 3, 4-methylenedioxyamphetamine, 3, 4-methylenedioxymethamphetamine, methylenedioxypyrovalerone, p-methoxymethylphenylamine, methoxyephedrine, 1- (3-chlorophenyl) piperazine, 2C-D, tramadol, (pseudo) ephedrine, cotinine, methcathinone, fentanyl, valerylfentanyl, fentanyl and/or carfentanyl;
the internal standard substance comprises methamphetamine-D5, amphetamine-D11, ketamine-D4, norketamine-D4, morphine-D3, O6-monoacetylmorphine-D3, codeine-D3, cocaine-D3, benzoylidennin-D3, 3, 4-methylenedioxyamphetamine-D5, 3, 4-methylenedioxymethamphetamine-D5, methylenedioxypyrrolpentanone-D8, tramadol-D3, ephedrine-D3, methcathinone-D3, cotinine-D3 and/or fentanyl-D5.
3. The method for determining the content of drugs and metabolites thereof in wastewater according to claim 1, wherein in the step 1, concentrated hydrochloric acid is added to the wastewater sample to adjust the pH value.
4. The method for determining the content of drugs and metabolites thereof in sewage according to claim 1, wherein in the step 1, the filtration is performed by using a solvent filter and a 0.45 μm glass fiber filter membrane.
5. The method for determining the content of drugs and metabolites thereof in sewage according to claim 1, wherein the flow rate is controlled to be 1.0mL/min during rinsing and elution in step 2, and the flow rate is controlled to be not less than 30min during vacuum solid phase extraction column evacuation.
6. The method for determining the content of drugs and metabolites thereof in wastewater according to claim 1, wherein in the step 2, the eluate is placed on a nitrogen-blown concentrator and blown to near dryness at a temperature of not higher than 40 ℃.
7. The method for determining the content of drugs and metabolites thereof in wastewater according to claim 1, wherein the liquid chromatography column is a C18 column.
8. The method for determining the content of drugs and metabolites thereof in wastewater according to claim 1, wherein the liquid chromatography conditions are as follows:
(1) a chromatographic column: ACQUITY UPLC BEH C18 column, (2.1 mm. times.100 mm,1.7 μm), column temperature: 40 ℃;
(2) mobile phase: mobile phase a phase: 20mmol/L ammonium acetate and 0.1% aqueous formic acid, mobile phase B: 0.1% formic acid acetonitrile solution; flow rate: 0.4 mL/min;
(3) sample introduction amount: 10 mu L of the solution;
(4) gradient elution conditions: design and adjustment according to different bonded phase chromatographic columns, for C18Bonded phase chromatography column, performed in the manner of the table below:
9. the method for determining the content of drugs and metabolites thereof in wastewater according to claim 1, wherein the mass spectrometry is performed by positive ion mode scanning and multiple reactive ion mode monitoring of electrospray ionization mass spectrometry.
10. The method for determining the contents of drugs and metabolites thereof in wastewater according to claim 1, wherein the mass spectrometer ion spray voltage is 1000V; the ion source temperature is 150 ℃; desolventizing temperature: 350 ℃; desolventizing air flow rate: 800L/Hr, taper hole air flow rate: 150L/Hr; and (4) directly feeding samples, and then screening parent ions and child ions, and screening the taper hole voltage and collision energy to obtain the maximum ion strength and keep the collision dissociation energy stable.
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| CN115047193A (en) * | 2022-06-27 | 2022-09-13 | 上海凯创生物技术有限公司 | Method for detecting trace amount of drugs in sewage |
| CN115420817A (en) * | 2022-07-28 | 2022-12-02 | 众旺达(宁夏)技术咨询有限公司 | Method for detecting drugs and drug metabolites in sewage |
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