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Method for rapid detection of residual amount of sulfanilamide in food

A technology for residues and sulfonamides, applied in material excitation analysis, fluorescence/phosphorescence, etc., can solve the problems of cumbersome operation steps, long detection time, poor selectivity, etc., and achieve the effect of increasing fluorescence intensity, short detection time and simple method

Active Publication Date: 2014-04-30
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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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Example 1: Qualitative and semi-quantitative detection of residual sulfadiazine sodium in milk by using the present invention

[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, and react at room temperature for 30 minutes, add NP-7 0.02mL and sodium chloride 0.05g, vortex mix for 2 minutes, heat at 35°C for 20 minutes, and centrifuge at 4000r / min for 12 minutes. Form the upper aqueous phase and the lower surfactant-rich phase, remove the upper aqueous phase to obtain the standard product-rich phase; dilute to 0.4 mL with methanol, place 1.5 cm on a thin-layer silica gel plate with a length of 8 cm, and take 30 μL (per Spotting 5 μL each time, 6 times in total) spotting the plate, this series is used as a standard ...

Embodiment 2

[0023] Example 2: Qualitative and semi-quantitative detection of sulfamethazine residues in pork by using the present invention

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

[0025] (2) Take 0.5 g of pork, add 2 mL of methanol, mix well, centrifuge at 6000 r / min for 10 min, take the supernatant to 5 mL 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 0.05 mL of NP-7 and 0.1 g of sodium sulfate, vortex and mix for 2 minutes, heat at 35°C for 30 minutes, and rotate at 5000r Centrifuge under the condition of 12min / min for 12min. At this time, the upper layer of water phase and the lower layer of surfactant-rich phase are formed. Remove the upper layer of water phase to obtain the rich phase of pork samples. Dilute it to 0.4mL with methanol and put it...

Embodiment 3

[0026] Example 3: Qualitative and semi-quantitative detection of sulfamethazine residues in honey by using the present invention

[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-7 0.1mL and sulfuric acid Ammonium 0.2g, vortexed for 2 min, heated at 35°C for 30 min, centrifuged at 3000r / min for 20 min, at this time an upper layer of water phase and a lower layer of surfactant-rich phase were formed, and the upper layer of water phase was removed to obtain a honey sample rich in Collect the ph...

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Abstract

The invention discloses a method for rapid detection of the residual mount of sulfanilamide in food. The method comprises the following steps: firstly enabling the sulfanilamide and fluorescamine to perform derivation reaction, further enriching derivative products by using cloud point extraction, adding a sample enrichment and a standard plate prepared from a sulfanilamide standard product on a thin layer silica gel plate, comparing the fluorescence intensities of the two under an ultraviolet lamp to judge the concentration range of the fluorescamine in a sample, and determining the residual amount of the sulfanilamide in the food, wherein a detection limit of the method is 0.08 micron g / mL. The method disclosed by the invention has the advantages of simplicity in operation, small using amount of organic solvent, high detection sensitivity, short detection time, strong specificity and capability of realizing effective separation from interfering substances, is a simple, convenient, fast and accurate analytical method, does not need large-scale instruments, only needs to configure small-scale instruments and equipment, and further has extensive 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 Applications(China)
IPC IPC(8): G01N21/64
Inventor 杨亚玲于芳赵娇
Owner KUNMING UNIV OF SCI & TECH
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