Method for simultaneously detecting 15 antibiotics in aquaculture sediment by combining microwave extraction-solid phase extraction pretreatment with liquid chromatography-mass spectrometry technology

A technology of aquaculture and liquid mass spectrometry, which is applied in the field of organic pollutant residue detection, can solve the problems of limited types and quantities of antibiotics, unstable detection methods, limited recovery rate, etc., achieve stable detection results, reduce the amount of extractant, The effect of high recovery rate

Inactive Publication Date: 2019-02-15
SHANGHAI ACADEMY OF ENVIRONMENTAL SCIENCES
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  • Abstract
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Problems solved by technology

However, at present, there is no complete and reliable detection method for the separation, enrichment and co-detection of various antibiotics in aquaculture sediment. Therefore, there is an urgent need for a method with stable detection results, low interference, fast, efficient, sensitive and accurate detection of as many antibiotic residues as possible in aquaculture sediments, including separation, enrichment and co-detection. Complete and reliable detection method

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  • Method for simultaneously detecting 15 antibiotics in aquaculture sediment by combining microwave extraction-solid phase extraction pretreatment with liquid chromatography-mass spectrometry technology
  • Method for simultaneously detecting 15 antibiotics in aquaculture sediment by combining microwave extraction-solid phase extraction pretreatment with liquid chromatography-mass spectrometry technology
  • Method for simultaneously detecting 15 antibiotics in aquaculture sediment by combining microwave extraction-solid phase extraction pretreatment with liquid chromatography-mass spectrometry technology

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] Embodiment 1: the pretreatment of sample

[0045] There are many kinds of target antibiotics, and their physicochemical properties vary greatly. In order to maximize the extraction efficiency of various antibiotics in the sediment, the present invention uses a single factor test to study the extraction effects of five different extracts on the target substances.

[0046] Specifically follow the steps below:

[0047] After the collected bottom mud was freeze-dried, it was ground and passed through a sieve with a pore size of 0.25 mm. Set up two sets of sediment samples for comparative tests, one set is the standard sample set, the other set is the blank sample set, and each set has two parallels. Accurately weigh 2.00 g of sediment samples into 100 mL beakers. Add respectively low, medium and high antibiotic mixed standard solutions (i.e. the mixed standard solution of 15 kinds of antibiotics) of three concentrations in the standard sample group, promptly add the antib...

Embodiment 2

[0053] Embodiment 2: the establishment of detection method

[0054] (1) Optimization of mass spectrometry conditions

[0055] Liquid chromatography-tandem mass spectrometry enables accurate quantitation using characteristic fragment ions. Therefore, it is necessary to optimize the fragmentation voltage and collision energy to obtain the best molecular ion-fragment ion pairs, so as to make the subsequent detection and analysis of actual water samples more accurate.

[0056] Using the direct injection method, each solution sample containing 100 μg / L target antibiotic was injected into the ion source respectively, and the parent ion full scan was performed in the positive ion detection mode to obtain the parent ion with the maximum response value of each antibiotic, and then carried out Secondary mass spectrometry scans to obtain qualitative ions and quantitative ions. The mass spectrometric analysis parameters of 15 antibiotics in multiple reaction mode (MRM) are listed in Tab...

Embodiment 3

[0081] Embodiment 3: the mensuration of actual sample

[0082] Collect the bottom mud of fish ponds, shrimp ponds, and crab ponds in an aquaculture area in Shanghai, first use the pretreatment method of the present invention to extract, enrich and purify the samples, and then use the detection method of the present invention to detect and analyze the actual concentration of the samples , to examine the applicability of this method to different types of sediment samples.

[0083] Specifically follow the steps below:

[0084] (1) Extraction of antibiotics: microwave extraction

[0085] After the collected bottom mud was freeze-dried, it was ground and passed through a sieve with a pore size of 0.25 mm. Add 100ng of sulfamethoxazole- 13 C 6 , Norfloxacin-D 5 , Penicillin G Potassium Salt-D 5 , Tetracycline-D 6 , olaquindox-D 4 , Amoxicillin- 13 C 6 and trimethoprim-D 3 The seven internal standards indicating the recovery rate were thoroughly mixed with the sediment sam...

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Abstract

The invention relates to a method for simultaneously detecting 15 antibiotics in aquaculture sediment by combining microwave extraction-solid phase extraction pretreatment with a liquid chromatography-mass spectrometry (LC-MS) technology. The method comprises the following steps: step (1) pretreating sediment samples, adding internal standard substances sulfamethoxazole-13C6, norfloxacin-D5, penicillin G potassium salt-D5, tetracycline-D6, olaquindox-D4, amoxicillin-13C6 and trimethoprim-D3 indicating a recovery rate, adding an acetonitrile-phosphate buffer solution for microwave extraction ofextraction liquid; step (2) performing solid phase extraction, enrichment and purification on target antibiotics; and step (3) quantitatively detecting 15 antibiotics of seven types in sediment witha liquid chromatograph/mass spectrometer. The method can simultaneously detect residues of 15 antibiotics containing 8 new antibiotics in the aquaculture sediment at a time by optimizing the internalstandard substances, screening appropriate pretreatment method and optimizing detection conditions, and has the advantages of high recovery rate, high sensitivity, high stability, low detection limit,more true and reliable detection results and the like.

Description

technical field [0001] The invention belongs to the technical field of residual detection of organic pollutants, and relates to a method for detecting trace antibiotics in aquaculture bottom mud, in particular to a microwave extraction-solid phase extraction pretreatment combined with liquid chromatography tandem mass spectrometry technology to simultaneously detect aquaculture bottom mud Methods for the content of 15 antibiotics. technical background [0002] In recent years, my country's aquaculture industry has developed rapidly, and scale and intensification have become the trend of aquaculture, while the frequency of aquatic animal diseases is also increasing. In order to prevent fish diseases and accelerate fish growth and reproduction, antibiotics are widely used in aquaculture. Antibiotics are mainly used in the aquaculture process by adding to feed or direct input. Studies have shown that only 20%-30% of antibiotics are absorbed by aquatic animals, and the rest are...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88G01N30/08
CPCG01N30/08G01N30/88
Inventor 胡双庆沈根祥张洪昌郭春霞钱晓雍李贞金汪仙仙王真
Owner SHANGHAI ACADEMY OF ENVIRONMENTAL SCIENCES
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