Method for determining residues of seven sulfonamide antibiotics in sediment sample

A sediment and sulfonamide technology is applied in the field of determination of 7 kinds of sulfonamide antibiotic residues in sediment samples, which can solve the problems of poor anti-interference ability and insufficient sensitivity, and achieve the improvement of accuracy, high detection sensitivity and grinding precision. Effect

Inactive Publication Date: 2018-09-14
NANJING INST OF ENVIRONMENTAL SCI MINIST OF ECOLOGY & ENVIRONMENT OF THE PEOPLES REPUBLIC OF CHINA +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The technical problem that the present invention solves is: there is certain limitation in view of existing detection method, sensitivity is not high enough, problems such as poor anti-interference ability, a kind of method for measuring 7 kinds of sulfonamide antibiotic residues in the sediment sample is provided, the method With low detection limit and good stability, it can basically meet the detection requirements of 7 kinds of sulfonamide antibiotic residues in sediment samples

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  • Method for determining residues of seven sulfonamide antibiotics in sediment sample
  • Method for determining residues of seven sulfonamide antibiotics in sediment sample
  • Method for determining residues of seven sulfonamide antibiotics in sediment sample

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Embodiment 1

[0041] A method for determining residues of 7 kinds of sulfa antibiotics in sediment samples, 7 kinds of sulfa antibiotics include sulfadiazine, sulfamethoxazole, sulfamethizole, sulfathiazole, sulfamethazine, sulfabenzopyrazole, sulfamethazine pyrimidine, comprising the steps of:

[0042] S1: Sample Collection:

[0043] Collect sediment samples at the sampling point, remove impurities, freeze-dry, put them in a grinding storage device for grinding and store them for testing. The grinding conditions are 60-mesh sieve, and the storage temperature is -20°C;

[0044] S2: Sample pretreatment:

[0045] Accurately weigh 5±0.01g of the above-mentioned ground sediment sample, mix it with 2g±0.05g of diatomaceous earth, put it into a 33ml extraction pool, and use Dionne 300 Accelerated Solvent Extraction (ASE) system for extraction, the extraction condition is a pressure of 1400psi , temperature 70°C, keep 10min, 60% flushing volume, flush 50s, use methanol / acetone (50 / 50, V / V) to ob...

Embodiment 2

[0059] A method for determining residues of 7 kinds of sulfa antibiotics in sediment samples, 7 kinds of sulfa antibiotics include sulfadiazine, sulfamethoxazole, sulfamethizole, sulfathiazole, sulfamethazine, sulfabenzopyrazole, sulfamethazine pyrimidine, comprising the steps of:

[0060] S1: Sample Collection:

[0061] Collect sediment samples at the sampling point, remove impurities, freeze-dry, put them in a grinding storage device for grinding and store them for testing. The grinding conditions are 60-mesh sieve, and the storage temperature is -20°C;

[0062] S2: Sample pretreatment:

[0063] Accurately weigh 5±0.01g of the above-mentioned ground sediment sample, mix it with 2g±0.05g of diatomaceous earth, put it into a 33ml extraction pool, and use Dionne 300 Accelerated Solvent Extraction (ASE) system for extraction, the extraction condition is a pressure of 1500psi , the temperature is 80°C, keep 10min, 60% of the washing volume, wash for 60s, use methanol / acetone (5...

Embodiment 3

[0077] A method for determining residues of 7 kinds of sulfa antibiotics in sediment samples, 7 kinds of sulfa antibiotics include sulfadiazine, sulfamethoxazole, sulfamethizole, sulfathiazole, sulfamethazine, sulfabenzopyrazole, sulfamethazine pyrimidine, comprising the steps of:

[0078] S1: Sample collection:

[0079] Collect sediment samples at the sampling point, remove impurities, freeze-dry, put them in a grinding storage device for grinding and store them for testing. The grinding conditions are 60-mesh sieve, and the storage temperature is -20°C;

[0080] S2: Sample pretreatment:

[0081] Accurately weigh 5±0.01g of the above-mentioned ground sediment sample, mix it with 2g±0.05g of diatomaceous earth, put it into a 33ml extraction pool, and use Dionne 300 Accelerated Solvent Extraction (ASE) system for extraction, the extraction condition is a pressure of 1600psi , the temperature is 90°C, keep 10min, 60% of the washing volume, wash for 70s, use methanol / acetone (5...

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Abstract

The invention relates to the technical field of determination of antibiotics in sediments, in particular to a method for determining the residues of seven sulfonamide antibiotics in a sediment sample.In the method, the high-performance liquid chromatography-mass spectrometry is utilized in combination with accelerated solvent extraction and solid-phase extraction for detecting the residues of seven sulfonamide antibiotics in the sediment sample. The sediment sample is subjected to accelerated solvent extraction and solid-phase extraction purification, a high-performance liquid chromatograph-mass spectrometer is used for MRM ion mode analysis, and an external standard method is used for quantification. The method is low in detection limit, good in stability, high in recovery rate and highin detection sensitivity, is used for rapid screening of seven sulfonamide antibiotics in sediments and can basically meet the requirement for detecting target substance residues in sediments.

Description

technical field [0001] The invention relates to the technical field of water environment detection, in particular to a method for determining the residues of seven sulfonamide antibiotics in sediment samples. Background technique [0002] In addition to being used for human health, antibiotics are also used as animal production accelerators. According to reports, the annual consumption of antibiotic raw materials in my country is about 180,000 tons, which is equivalent to 138g per capita per year, which is 10 times that of the United States. Sulfonamide antibiotics are one of the most widely used antibiotics, which are derivatives containing p-aminobenzenesulfonamide structure. These drugs have a broad antibacterial spectrum and have inhibitory effects on most Gram-positive and Gram-negative bacteria. It mainly includes antibiotics such as acesulfame, sulfamethazine, sulfamethoxazole, sulfamethoxypyridazine, and sulfabenzopyrazole. Due to the widespread use of such substan...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06G01N2030/062
Inventor 张圣虎张芹宋宁慧韩志华赵欣张振华赵雅芳
Owner NANJING INST OF ENVIRONMENTAL SCI MINIST OF ECOLOGY & ENVIRONMENT OF THE PEOPLES REPUBLIC OF CHINA
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