Method for measuring 12 types of remaining medicine in water environment through separation and enrichment

A technology for separation, enrichment, and residual drugs, which is applied in material separation, measuring devices, and analytical materials, etc., can solve the problems of large detection limit of organic reagent consumption, and achieve the effects of wide application range, high extraction efficiency, and high sensitivity

Active Publication Date: 2016-03-23
SHENYANG PHARMA UNIVERSITY +1
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Problems solved by technology

The invention adopts ultrasonic-assisted dispersion liquid-liquid microextraction as the pretreatment technology of water environment samples, and uses ultra-high liquid chromatography-mass spectrometry as a detector, which overcomes the problems of large consumption of organic reagents, high interference and detection limit in the existing method , can quickly detect ketoprofen, ciprofloxacin, tinidazole, tolfenamic acid, sulfadiazine, sulindac, naproxen, sulfamethoxazole, chloramphenicol, cefuroxime axetil, The content of 12 kinds of medicines such as piroxicam and mefenamic acid is suitable for a wide range of objects, and the determination results are sensitive, accurate and less interference

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  • Method for measuring 12 types of remaining medicine in water environment through separation and enrichment
  • Method for measuring 12 types of remaining medicine in water environment through separation and enrichment
  • Method for measuring 12 types of remaining medicine in water environment through separation and enrichment

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Embodiment Construction

[0050] The invention adopts ultrasonic-assisted dispersion liquid-liquid microextraction-ultrahigh phase liquid chromatography-tandem mass spectrometry to realize the detection of 12 Chinese medicines in the water environment (drinking water, tap water, river water, water in and out of sewage treatment plants), which is comparable to the traditional method It has a wide range of applications, and has the advantages of high recovery, high sensitivity, and fast analysis speed.

[0051] Concrete detection method of the present invention is as follows:

[0052] (1) Water sample pretreatment

[0053] Collect drinking water, tap water, river water, and influent and effluent water from sewage treatment plants, and then filter through quantitative filter paper for 2-3 times, and 0.45μm membrane filter for 2 times (whether to filter or not). Then measure 5mL of the filtered water sample, adjust the pH to 3.0-4.0 with 0.1mol / L HCl, and transfer it to a 12mL glass centrifuge tube;

[0...

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Abstract

The invention relates to a method for measuring 12 types of remaining medicine in a water environment through separation and enrichment at the same time, and belongs to the field of safety detection of a trace of organic pollutant residue in the water environment. The content of 12 types of frequently-used medicine in the water environment (drinking water, faucet water, river water and water discharged into and out of sewage treatment plants) is directly measured with an ultra performance liquid-chromatography-mass spectrometer (UPLC-MS / MS) as a detection tool after a water sample is subjected to solid phase extraction combined with ultrasonic-assisted dispersion liquid-liquid micro-extraction (UA-DLLME) separation and enrichment. The 12 types of antibiotic include ketoprofen, ciprofloxacin, tinidazole, tolfenamic acid, sulfadiazine, sulindac, naproxen, sulfamethoxazole, chloramphenicol, cefuroxime axetil, piroxicam and mefenamic acid. Inspection and optimization are conducted on a sample pretreatment method and instrument detection conditions of the water sample, and the optimal UA-DLLME method is established and is successfully applied to practical sample detection. Compared with a traditional method, the method has the advantages of being high in sensitivity, high in extraction and recycle rate, wide in suitable object, friendly to the environment, and the like.

Description

【Technical field】 [0001] The invention relates to a detection method for separation, enrichment and determination of residual drugs in a water environment, and in particular provides a new sample pretreatment method and a sensitive detection method, specifically, a sample pretreatment technology combined with liquid mass spectrometry technology Direct determination of the content of 12 commonly used drugs in water samples belongs to the field of safety detection of trace organic pollutant residues in the water environment. 【Background technique】 [0002] Antibiotics are mainly secondary metabolites or artificially synthesized analogs produced by bacteria, molds or other microorganisms. They are mainly used to treat various bacterial infections or diseases caused by pathogenic microbial infections, and have made great contributions to human health. However, the abuse of antibiotics has become very serious in recent years. The Ministry of Health once stated that in China, the ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/08
CPCG01N30/02G01N30/08G01N2030/027
Inventor 赵龙山王洋熊志立秦峰
Owner SHENYANG PHARMA UNIVERSITY
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