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A method for rapid detection of sulfonamide residues in food

A technology of residue and sulfonamide, which is applied in the direction of material excitation analysis, fluorescence/phosphorescence, etc., can solve the problems of cumbersome operation steps, long detection time, low sensitivity, etc., and achieve the effect of increasing fluorescence intensity, short detection time and high sensitivity

Active Publication Date: 2016-03-30
KUNMING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The above methods have their own strengths in terms of detection precision, and some have low sensitivity and poor selectivity; Inconvenience in practical application

Method used

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  • A method for rapid detection of sulfonamide residues in food

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Embodiment 1: Using the present invention to carry out qualitative and semi-quantitative detection of sulfadiazine sodium residues in milk

[0021] (1) Prepare 5 mL of sulfadiazine sodium standard solution with concentrations of 0.1, 1.0, 10.0 and 100.0 mg / L respectively, add 0.2 mL of 0.1% (w / v) fluorescamine methanol solution, and prepare with boric acid, acetic acid and phosphoric acid Adjust the pH of the system to pH 5 with buffer solution at room temperature. After reacting at room temperature for 30 minutes, add NP-70.02mL and sodium chloride 0.05g, vortex and mix for 2 minutes, heat at 35°C for 20 minutes, and centrifuge at 4000r / min for 12 minutes. At this time, the upper layer is formed. The water phase and the lower surfactant-rich phase were removed, and the upper water phase was removed to obtain the standard product-rich phase; diluted with methanol to 0.4 mL, placed on a thin-layer silica gel plate with a length of 8 cm at an interval of 1.5 cm, and 30 μL ...

Embodiment 2

[0023] Embodiment 2: Using the present invention to carry out qualitative and semi-quantitative detection of sulfamethazine residues in pork

[0024] (1) Same as step 1 of Example 1, the difference is that the sulfonamide used is sulfamethazine;

[0025] (2) Take 0.5g of pork, add 2mL of methanol, mix well, centrifuge at 6000r / min for 10min, take the supernatant to 5mL with water, add 0.1% (w / v) fluorescamine methanol solution 0.3 mL, adjust the system to pH 5 with a buffer solution prepared from boric acid, acetic acid and phosphoric acid, react at room temperature for 30 minutes, add NP-70.05mL and sodium sulfate 0.1g, vortex mix for 2 minutes, heat at 35°C for 30 minutes, at a speed of 5000r / min Centrifuge under the conditions for 12min. At this time, the upper aqueous phase and the lower surfactant-rich phase are formed. Remove the upper aqueous phase to obtain the pork sample-rich phase, dilute it to 0.4mL with methanol, and spot on thin-layer silica gel plates with a len...

Embodiment 3

[0026] Embodiment 3: Using the present invention to carry out qualitative and semi-quantitative detection of sulfamethazine residues in honey

[0027] Step 1: Same as step 1 of Example 1, except that the sulfonamide used is sulfamethazine;

[0028] Step 2: Take 2.0g of honey, add 5mL of water, mix well, vortex for 2.0min, filter, add 3.0mL of water to the filtrate, vortex for 2.0min, centrifuge at 3000r / min for 15min, take the supernatant with water Set the volume to 5mL, add 0.5mL of 0.1% (w / v) fluorescamine methanol solution, adjust the system to pH3 with a buffer solution prepared by boric acid, acetic acid and phosphoric acid, react at room temperature for 30min, add NP-70.1mL and ammonium sulfate 0.2g, vortex mixed for 2min, heated at 35°C for 30min, centrifuged at 3000r / min for 20min, at this time the upper layer of water phase and the lower layer of surfactant-rich phase were formed, and the upper layer of water phase was removed to obtain the honey sample-rich phase ,...

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Abstract

The invention discloses a method for rapidly detecting the residual amount of sulfonamide in food, that is, first adopting the derivatization reaction of sulfonamide and fluoresceinamine, and then enriching the derivative product by cloud point extraction, adding samples enriched on a thin-layer silica gel plate. The standard plate prepared from the collected material and the sulfonamide standard substance is compared with the fluorescence intensity of the two under the ultraviolet light to determine the concentration range of sulfonamide in the sample, which is used for the determination of sulfonamide residues in food. The detection limit of the method is 0.08μg / mL; the method of the present invention is simple to operate, the amount of organic solvents is small, the detection sensitivity is high, the detection time is short, the specificity is strong, and it can be effectively separated from interfering substances. It is a simple, fast and accurate analysis method. Need large instruments, only need to configure small instruments and equipment, has a wide range of application prospects.

Description

technical field [0001] The invention belongs to the technical field of food safety detection, and relates to a detection method for residual sulfonamide in food, in particular to a method for fluorescence derivation and cloud point extraction. Background technique [0002] Animal source foods such as milk and meat products generally contain rich nutrients such as protein, fat, amino acid, sugar, calcium, phosphorus, iron, etc. With the continuous improvement of people's living standards, their proportion in the dietary structure of residents is also increasing. getting bigger. Sulfonamide drugs are widely used in animal husbandry production for the prevention and treatment of livestock and poultry diseases because of their cheapness, high curative effect, and short course of treatment. Extensive use of sulfonamides results in residues in most animal-source foods, and people eating animal-source foods with excessive sulfonamide residues will cause harm to human health. In o...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N21/64
Inventor 杨亚玲于芳赵娇
Owner KUNMING UNIV OF SCI & TECH
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