Method for simultaneously detecting six types of 24 antibiotics in water by solid phase extraction-liquid chromatography-tandem mass spectrometry

A technology of liquid chromatography and tandem mass spectrometry, which is applied in the field of detection of trace organic pollutant residues, can solve the problems of interfering with multiple detection of antibiotic quantity and range, large consumption of organic reagents, and long time consumption, so as to avoid unnecessary damage and reduce processing time. Short, reduce the effect of matrix effect

Inactive Publication Date: 2018-01-05
SHANGHAI ACADEMY OF ENVIRONMENTAL SCIENCES
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Problems solved by technology

[0005] The purpose of the present invention is to overcome the problems of large consumption of organic reagents, long time consumption, high interference and limited quantity and range of detection antibiotics in the existing method, and provide a method with accurate and stable detection results, less interference, and low organic reagent consumption. less, less time-consuming detection process, can simultaneously determine six ty...

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  • Method for simultaneously detecting six types of 24 antibiotics in water by solid phase extraction-liquid chromatography-tandem mass spectrometry
  • Method for simultaneously detecting six types of 24 antibiotics in water by solid phase extraction-liquid chromatography-tandem mass spectrometry
  • Method for simultaneously detecting six types of 24 antibiotics in water by solid phase extraction-liquid chromatography-tandem mass spectrometry

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Embodiment 1

[0038] The present invention is a method for simultaneously detecting six types of 24 antibiotics in a water body by solid-phase extraction-liquid chromatography tandem mass spectrometry, which is specifically implemented according to the following steps:

[0039] Step 1. Pretreatment of water samples

[0040] Collect drinking water, tap water, surface water, and influent and effluent water from sewage treatment plants, respectively. The water samples are filtered through a 0.45 μm glass fiber membrane to remove suspended solids, and then accurately measure 1 L with a graduated cylinder. Use dilute sulfuric acid with a volume concentration of 10% to adjust the pH of the water sample to 3.0-4.0 (if the surface water is collected to inhibit the degradation of antibiotics by microorganisms, a certain amount of dilute hydrochloric acid will be added, and the pH adjustment step can be omitted at this time). Before solid phase extraction, 10 μL and 5 mg / L of 13 C 1 D 3 - Erythrom...

Embodiment 2-3

[0087] Example 2-3 Determination of the concentration of 24 antibiotics in two different actual water bodies

[0088] Examples 2 and 3 respectively take surface water and sewage from livestock and poultry farms as examples. First, the method of step 1 is used for pretreatment, and then the method of step 2 is used for solid-phase extraction, enrichment and purification pretreatment, and then step 3 is used. The established detection method is detected and analyzed to examine the applicability of the established detection method in step 3 of the present invention.

[0089] A kind of solid-phase extraction-liquid chromatography tandem mass spectrometry method of the present invention described in embodiment 2 and embodiment 3 simultaneously detects six types of 24 kinds of antibiotics in water body, and is specifically implemented according to the following steps:

[0090] Step 1. Pretreatment of water samples

[0091] Collect surface water and livestock and poultry farm sewage...

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Abstract

The invention discloses a method for simultaneously detecting six types of 24 antibiotics in water by solid phase extraction-liquid chromatography-tandem mass spectrometry. The method comprises (1) carrying out water sample pretreatment through adding an internal standard substance indicating a recovery rate before solid phase extraction, (2) enriching and purifying a target antibiotic with a solid phase extraction small column and (3) detecting contents of six types of 24 antibiotics in water through a liquid chromatography-tandom mass spectrometer. The method can simultaneously detect residues of six types of 24 antibiotics in water, has low time consumption in detection and has the advantages of high precision, high sensitivity, high stability, high selectivity and low detection limit.In the water sample pretreatment, an organic reagent use amount is small, environmental friendliness is realized, operation is simple, an enrichment factor is high and reproducibility is good. The method utilizes the internal standard substance indicating a recovery rate before solid phase extraction, well shows the loss of the target substances in the pretreatment and produces a real and reliablefinal result.

Description

technical field [0001] The invention belongs to the technical field of residual detection of trace organic pollutants in the water environment, relates to a detection method for trace organic pollutants in water, and particularly relates to a method for detecting trace organic pollutants in water, in particular to a solid phase extraction (SPE) pretreatment combined with liquid chromatography tandem mass spectrometry (HPLC- MS / MS), an analytical detection method that can efficiently and simultaneously detect six classes of up to 24 antibiotics in water. technical background [0002] Antibiotics are widely used in the treatment of human and animal diseases due to their antibacterial properties, promoting the growth of crops and aquaculture. Globally, about 2 million tons of antibiotics are used each year, with 250,000 tons in China alone. However, only a small part of these antibiotics are in the organism, and up to 80% are excreted into the natural environment through urine...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/08
Inventor 胡双庆沈根祥张洪昌钱晓雍王振旗朱英张玉袁哲军
Owner SHANGHAI ACADEMY OF ENVIRONMENTAL SCIENCES
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