Method of using liquid chromatograph mass spectrometer for synchronously measuring four kinds of antibiotics in river sediment

Abstract

The invention relates to a method of using a liquid chromatography tandem mass spectrometry for synchronously measuring four kinds of antibiotics in river sediment. The method of using the liquid chromatography tandem mass spectrometry for synchronously measuring the four kinds of antibiotics in the river sediment includes the following steps that 1, an experimental vessel is prepared; 2, the moisture content is measured; 3, vacuum freeze drying is conducted; 4, sequential extraction, grinding and sieving are conducted; 5, ultrasonic extraction and mechanical vibration are used for preparation; 6, double-column tandem solid-phase extraction is carried out, wherein before the solid-phase extraction, a buffer solution is added into an extraction solution subjected to rotary evaporation, then, ultrapure water is adopted to dilute a mixture, and the mixture is shaken to be fully uniform; 7, the extraction solution is purified and subjected to elution; 8, concentration and constant volume are conducted; 9, high-performance liquid chromatography is adopted to carry out synchronous computer measurement. By the adoption of the method of using the the liquid chromatography tandem mass spectrometry for synchronously measuring the four kinds of antibiotics in the river sediment, the purification and enrichment effects are greatly improved, 0.2% methanoic acid-2mmol / L ammonium acetate is used, acetonitrile and a citric acid buffer solution of which the pH value is 3 are used as the extraction solution of a solid sample, and optimal conditions are adopted to be configured and combined,so that a target analyte is better isolated, chromatographic peak area is larger, and the recovery rate is higher.

Description

technical field [0001] The present invention relates to high-efficiency and accurate pretreatment technology and detection method for sediment antibiotics in rivers, and in particular provides an extraction method of freeze-vacuum drying, subsection extraction, ultrasonic extraction plus mechanical vibration, and double solid-phase extraction for synchronous detection of rivers Methods of four antibiotics of macrolides, sulfonamides, quinolones and tetracyclines in sediments. Background technique [0002] Antibiotics are widely used as effective drugs to treat various diseases. In China, the annual consumption of antibiotics is about 210,000 tons, and more than 80% of antibiotics are transported to the environment in their original form through industrial wastewater, medical waste, animal excrement and domestic sewage. Although the half-life of most antibiotics is not long, due to their frequent use and entry into the water environment, bacterial resistance in water has inc...

AI Technical Summary

Problems solved by technology

Although the half-life of most antibiotics is not long, due to their frequent use and entry into the water environment, bacterial resistance in the water has increased, aquatic organisms have teratogenic mutations, and unpredictable harm to human health and the local ecological environment.

[0003] At present, there are relatively few studies on the detection of antibiotics in water sediments

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