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Synchronous detection method for plurality of types of drug residues in water body

A technology for simultaneous detection and residual drug application in measurement devices, instruments, scientific instruments, etc., to achieve the effects of good reproducibility, high sensitivity and simple operation

Inactive Publication Date: 2016-06-22
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the existing research, most of the analysis and detection are carried out on a few antibiotics or the same type of antibiotics, which has certain limitations.

Method used

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  • Synchronous detection method for plurality of types of drug residues in water body
  • Synchronous detection method for plurality of types of drug residues in water body
  • Synchronous detection method for plurality of types of drug residues in water body

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] Embodiment 1 water sample pretreatment

[0043] Measure 1 L of water sample with a graduated cylinder, filter it with a 0.45 μm glass fiber filter membrane to remove the suspended matter, add internal standard C13-labeled sulfadiazine, and adjust the pH value to 2-2.5 with hydrochloric acid.

Embodiment 2

[0044] Embodiment 2 solid phase extraction

[0045] (1) Activation of HLB solid phase extraction column

[0046] The specification of the HLB solid-phase extraction column used for enrichment is 200mg / 6mL. First, 10mL of methanol is slowly dripped under the action of gravity to complete the activation; Pass through the HLB solid-phase extraction column under the action of gravity; finally, use 10mL of ultrapure water with pH=2.5 to pass through the HLB solid-phase extraction column under the action of gravity, so that the HLB solid-phase extraction column is under acidic conditions, which is convenient for subsequent enrichment work.

[0047] (2) Introduction of samples

[0048] The pretreated water sample was enriched using the activated HLB solid phase extraction column. Use a diversion tube to connect the sample and the HLB solid-phase extraction column, introduce the sample into the HLB solid-phase extraction column by vacuuming, adjust the flow control valve to control ...

Embodiment 3

[0053] Embodiment 3: The establishment of LC-MS / MS detection method on the machine

[0054] The detection parameters of LC-MS / MS are shown in Table 2, and the detection conditions of various drugs are shown in Table 3:

[0055] Table 2: LC-MS / MS detection parameters

[0056]

[0057] Table 3: Conditions for the detection of each substance

[0058]

[0059]

[0060] * Quantitative ion

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Abstract

The invention provides a method for synchronous detection of multiple residual drugs in a water environment, and belongs to the technical field of pollutant enrichment detection in a water environment. The residual drugs include antibiotics, anti-inflammatory analgesics and antihypertensive drugs, etc., and the synchronous detection method includes the following steps: (1) water sample pretreatment: filter to remove suspended matter, adjust the pH value of the water sample; (2) solidify Phase extraction: use HLB solid-phase extraction column to enrich the target drug; (3) blow nitrogen to nearly dry, dilute to 1mL and vortex for testing; (4) use LC-MS / MS for detection on the machine. The synchronous detection method of the present invention can simultaneously detect 32 pharmaceutical pollutants in the water body by one-time sample injection, and the method has the advantages of high accuracy and sensitivity and low detection limit; meanwhile, the method is environmentally friendly and easy to operate.

Description

technical field [0001] The invention belongs to the technical field of pollutant enrichment detection in water body environment, and in particular relates to a method for synchronous detection of multiple residual drugs in water body. technical background [0002] Drugs include antibiotics, steroids, anti-inflammatory drugs, antihypertensive drugs, painkillers, etc. Most of the drugs administered to humans or animals cannot be completely absorbed by the body, and are mostly excreted in the form of original form or metabolites with feces, urine, etc. Outside the body, into the environment. Among the 20 most frequently detected drugs and personal care products in natural water bodies such as rivers and lakes in my country, the top 10 are antibiotics, and 7 are antipyretic and pain-relieving drugs. my country produces about 1,300 kinds of chemical raw materials and cosmetics every year, among which the annual output of antibiotics is more than 33,000 tons. Studies have shown ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
CPCG01N30/02G01N2030/027
Inventor 何欣关颖婷马洋帆全燮
Owner DALIAN UNIV OF TECH
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