Method for detecting sulfamethazine in animal-derived food

A sulfamethazine, animal-derived technology, applied in the fields of food safety testing and analytical chemistry, can solve the problems of high price and poor selectivity, and achieve the effects of low cost, small sample volume and good adsorption performance.

Inactive Publication Date: 2013-05-15
FUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the existing solid-phase extraction columns are all disposable, the pr...

Method used

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  • Method for detecting sulfamethazine in animal-derived food
  • Method for detecting sulfamethazine in animal-derived food
  • Method for detecting sulfamethazine in animal-derived food

Examples

Experimental program
Comparison scheme
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Embodiment 1

[0038] Example 1: Preparation of sulfamethazine molecularly imprinted polymer and preparation of solid phase extraction column:

[0039] In a glass container, the template molecule sulfamethazine (SM2) 0.278 g (1 mmol), the functional monomer methacrylic acid (MAA) 0.35 mL (4.0 mmol), the cross-linking agent ethylene glycol dimethyl diacrylate (EGDMA) 3.85mL (20.0 mmol) was mixed uniformly according to the molar ratio of 1:4:20, and added to 10 mL of porogen acetonitrile together, and 50 mg of initiator azobisisobutyronitrile (AIBN) was added, and ultrasonic treatment was performed for 10 Minutes, purged with nitrogen for 10 minutes, sealed, placed in a water bath at 60°C, and thermally initiated polymerization for 24 hours to obtain a block polymer.

[0040] The resulting massive polymer is ground by a mortar, passed through 200 mesh and 400 mesh sieves, the resulting polymer particles are in the range of 35-75 microns, wrapped with filter paper and placed in a Soxhlet ex...

Embodiment 2

[0042] Example 2: Extraction and Raman-enhanced detection of sulfamethazine in fish samples:

[0043] 1. Sample pretreatment and sulfamethazine extraction

[0044] The edible part of the fish sample was taken, chopped, homogenized, and stored frozen at -18°C. During the test, after the frozen sample is equilibrated to room temperature, accurately weigh 5 g of the sample, add 5 g of anhydrous sodium sulfate and 25 mL of ethyl acetate, vortex for 2 minutes, centrifuge at 4000 rpm for 2 minutes, and collect the ethyl acetate. ester solution. Repeat the extraction with ethyl acetate once more, combine the ethyl acetate solutions, and distill under reduced pressure at 30°C until nearly dry. Add 10% methanol to dissolve, add 3 mL of n-hexane, vortex for 2 minutes, transfer to a centrifuge tube; repeat the dissolving process, combine the mixed solution in a centrifuge tube, vortex for 2 minutes, discard n-hexane, then add 6 mL of n-hexane and repeat the operation once. Add ultrap...

Embodiment 3

[0053] A method for detecting sulfamethazine in food of animal origin, said method comprising the following steps:

[0054] (1) Synthesize the molecularly imprinted material of sulfamethazine by using the method of bulk polymerization: template molecule sulfamethazine (SM2), functional monomer methacrylic acid (MAA), cross-linking agent B in a glass container Glycol dimethyl diacrylate (EGDMA) is mixed evenly according to the molar ratio of 1:4-10:20-50, and added to the porogen together, and the initiator azobisisobutyronitrile (AIBN) is added, and ultrasonic treatment For 10 minutes, pass nitrogen gas to remove oxygen for 10 minutes, seal, place in an oil bath at 60°C, and heat-initiate polymerization for 20 hours to obtain a block polymer; grind the obtained block polymer through 200 mesh and 400 mesh The obtained polymer particles are 35-75 microns, wrapped in filter paper and placed in a Soxhlet extraction reactor, extracted with methanol-acetic acid (9 / 1, v / v) mixture f...

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Abstract

The invention provides a method for detecting sulfamethazine in animal-derived food. The method comprises the following steps of: synthesizing a molecularly imprinted material; preparing a practical sample; extracting the sulfamethazine from an aquatic product by ethyl acetate; carrying out rotary evaporation on an extracting solution; dissolving the product in a methanol aqueous solution again; performing purification and enrichment by a molecularly imprinted solid phase extraction column; and detecting the sulfamethazine by a Raman enhanced spectrum with combination of shell isolated nanoparticles. The method has the positive effects that a synthesized molecularly imprinted material is high in specificity and can be taken as a filler of the solid phase extraction column and used for separating and gathering target molecules to be detected from a practical sample; the method can be used for detecting the sulfamethazine by Raman enhancement with combination of the shell isolated nanoparticles and is high in detection sensitivity, high in speed, less in sample comsuption and convenient to operate; and the method can be used for rapidly detecting the sulfamethazine in the animal-derived food and can reach the detection sensitivity of 50ppb.

Description

technical field [0001] The invention belongs to the fields of analytical chemistry and food safety detection, and in particular relates to a detection method for sulfamethazine in animal-derived food. Background technique [0002] Sulfonamide synthetic antibacterial drugs are a class of antibacterial drugs that inhibit nucleic acid synthesis and are widely used to prevent and stimulate animal growth. Their main function is to achieve the purpose of antibacterial by inhibiting bacterial reproduction. Sulfamethazine is one of the sulfonamides. It has the characteristics of stable properties, broad-spectrum antibacterial, easy oral absorption and low price. It is widely used in the control and treatment of animal diseases in animal husbandry and aquaculture. One of the most widely used sulfa drugs in production. After entering the animal body through various routes of administration, it can remain in the meat, eggs, milk and other tissues and products of the animal. If these f...

Claims

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Application Information

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IPC IPC(8): G01N21/65G01N1/34G01N1/40
Inventor 杨黄浩张晓龙宋良柯开美刘威田中群
Owner FUZHOU UNIV
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