Method for determining 10 kinds of antibiotics in water environment through combination of sample pre-treatment technology and HPLC-MS

Abstract

The present invention relates to a method for determining 10 kinds of antibiotics in a water environment through combination of a sample pre-treatment technology and HPLC-MS, and belongs to the field of detection of safety of trace organic contaminant residue in the water environment. The method is characterized in that a water sample is separated and enriched through combination of solid phase extraction and dispersive liquid-liquid microextraction (SPE-DLLME), and then an ultra-high performance liquid chromatography-mass spectrometry instrument (UPLC-MS / MS) is adopted as a detection tool to directly determine the contents of 10 kinds of common antibiotics in the water environment (drinking water, tap water, river water, sewage treatment plant influent and effluent), wherein the 10 kinds of the common antibiotics respectively are sulfadiazine, sulfamethoxazole, oxytetracycline, tetracycline, doxycycline, ciprofloxacin, levofloxacin, chloramphenicol, cefuroxime axetil and tinidazole. According to the present invention, the water sample pre-treatment method and the instrument detection conditions are investigated and optimized, and the optimal SPE-DLLME-UPLC-MS / MS method is established and is successfully applied for the real sample determination; and compared with the traditional method, the method of the present invention has advantages of high sensitivity, high extraction recovery rate, wide application objects, environmental protection, and the like.

Description

【Technical field】 [0001] The present invention relates to a detection method for determining trace organic pollutants in water, and in particular provides a new sample pretreatment method and a sensitive detection method. The content of a common antibiotic 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 usage rate of antibiotics among patients has reached 70%, twice that of European and American countries, but less than 20% actually need to use them. In addition, the a...

AI Technical Summary

Problems solved by technology

The invention adopts solid-phase extraction combined with 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 large consumption of organic reagents, many interferences and detection limits in the existing methods. It can quickly detect sulfadiazine, sulfamethoxazole, mycin, tetracycline, doxycycline, ciprofloxacin, levofloxacin, chloramphenicol, cefuroxime axetil and tinidazole 10 kinds of antibiotics in the water environment content, wide range of application objects, sensitive and accurate measurement results, less interference

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