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Method for determining contents of drugs and metabolites thereof in sewage

A technology for metabolites and drugs, applied in the field of chemical detection, can solve problems such as interference detection and complex components, and achieve the effect of improving accuracy, meeting analysis requirements and high accuracy

Inactive Publication Date: 2021-08-06
NANKAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In addition, the composition of the actual water environment is complex, which will seriously interfere with the detection. Therefore, when establishing a method for the detection of several drugs and their metabolites in sewage, not only a detection instrument with high sensitivity is required, but also an appropriate high-recovery pretreatment method is required. The treatment method minimizes the interference of impurities in environmental samples, and selectively enriches trace target substances at a high rate to ensure the sensitivity of the analysis

Method used

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  • Method for determining contents of drugs and metabolites thereof in sewage
  • Method for determining contents of drugs and metabolites thereof in sewage
  • Method for determining contents of drugs and metabolites thereof in sewage

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0059] The invention provides a method for determining several kinds of drugs in sewage. The method takes the added sample as a control, adds an isotope internal standard to the filtered sewage sample, and carries out extraction, purification and concentration. The instrument is used for detection, the qualitative analysis is carried out by the retention time and the characteristic fragment ions of the mass spectrum, and the quantitative analysis is carried out by the isotope internal standard method.

[0060] 29 sewage treatment plants in Tianjin were selected as the analysis objects for concentration determination. The analysis methods and results are as follows:

[0061] Stock solution (for establishing working curve, measuring recovery rate, liquid quality establishment method)

[0062] Preparation of standard stock solution: Take 0.1mg / mL or 1mg / mL standard of the target compound, mix and dilute to 5μg / mL with methanol, mix well, seal, and store in a refrigerator at -20°C...

Embodiment 2

[0084] Take the same amount of tap water as the test material sample, and operate in parallel with the test material sample to obtain a blank sample extract for instrument detection. Take the same amount of tap water as the test material sample, add the mixed standard working solution, so that the concentration of 25 substances in it is 500ng / L, 100ng / L, 50ng / L, 10ng / L, 5ng / L, 1ng / L, as the addition The sample is operated in parallel with the test material sample to obtain the sample extract for instrument detection. Carry out linear regression to the concentration (X) of each target substance in the sewage with the ratio (Y) of the peak area of ​​each target substance and the internal standard peak area respectively, obtain the linear equation of each target substance, the linearity (r 2 ) shown.

Embodiment 3

[0086] The present invention is applied in actual monitoring, and the concentration of the target compound in the samples collected by 29 sewage treatment plants is measured, and the results are shown in the following table;

[0087] The sampling method is to collect once every 2 hours, and the 12 instantaneous samples collected 24 hours a day are mixed in equal volume to obtain a daily mixed sample of 900mL. All samples used TC-8000D portable fully automatic equal-proportion water quality sampler | refrigerated water collector produced by Qingdao Traceability Environmental Protection Equipment Co., Ltd. Each sewage treatment plant is sampled for 7 days and tested once a day. The following data are all within the range of the detected values ​​of 7 samples.

[0088]

[0089]

[0090]

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Abstract

The invention discloses a method for determining the content of narcotics 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 into the solid-phase extraction column, leaching by using ultrapure water, vacuumizing the solid-phase extraction column, eluting by using a 5% ammonia methanol solution, vacuumizing the solid-phase extraction column, and collecting eluent; blowing the eluent to be nearly dry, adding and evenly mixing 0.1% formic acid aqueous solution, wherein a 0.22-micron nylon microfiltration membrane is used for filtering, and the eluent is used as a detection material sample extracting solution for instrument detection; and step 3, carrying out liquid chromatography-tandem mass spectrometry analysis on the sample extracting solution, and detecting the contents of the drugs and the metabolites thereof. The invention basically comprises various drugs involved in the existing case, so as to meet the requirements of actual work.

Description

technical field [0001] The invention relates to the technical field of chemical detection, in particular to a method for measuring the content of drugs and their metabolites in sewage. Background technique [0002] Drugs refer to compounds that have a strong excitatory or inhibitory effect on the human central nervous system, mainly including opioids such as morphine, cocaine, heroin, methadone, amphetamines such as amphetamine, methamphetamine (ice), and ecstasy, ketamine, norketamine, etc. . Drugs are excreted with urine in the form of raw drugs or metabolites after ingestion and enter domestic sewage. In addition, the drugs in the sewage may also come from the illegally discharged wastewater from drug factories and the destruction of them during raids. Evidence Drugs etc. flushed down the sewer. Drugs and their metabolites have good stability in sewage. By analyzing the concentration of various drugs and their metabolites in sewage, and then correcting the total amount ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/14G01N30/72
CPCG01N30/02G01N30/06G01N30/14G01N30/72G01N2030/062G01N2030/146
Inventor 姬亚芹林孜林宇高玉宗杨益
Owner NANKAI UNIV
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