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Method for detecting residual quantity of sulfonamide in milk and meat products

A technology of sulfa drugs and residues, which is applied in the preparation of test samples, chemiluminescence/bioluminescence, and analysis through chemical reactions of materials, etc. Time and other issues, to achieve the effect of fast detection speed, large application prospects, and low detection cost

Inactive Publication Date: 2011-09-14
杨亚玲
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The above-mentioned methods have their own strengths in terms of detection precision, etc., but they also have their own shortcomings, some have low sensitivity and poor selectivity; The shortcomings of these methods bring a lot of inconvenience to the detection of sulfonamide antibiotics
Chinese invention patent 200710066347.6 (CN 101430325) discloses the "rapid color development method for sulfamethazine residues" which involves the determination of sulfa drugs by color reaction, which has a huge gap with the present invention in terms of selectivity and sensitivity, especially in the detection of residues Difficult to implement; although the enzyme-linked immunoassay kit has great advantages in residual detection, it is also essentially different from the present invention

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] 1. Prepare 500 mL of sulfadiazine sodium standard aqueous solution with a concentration of 40 mg / L, and dilute it step by step when used.

[0023] 2. Take 0.5mL of sulfadiazine sodium aqueous solution with a concentration of 1mg / L and place it in a 10mL colorimetric tube, add 2mL of tri-acid buffer solution with pH 1.8, 0.1mL of 10g / L o-phthalaldehyde methanol solution, and dilute to volume with water to the mark, shake well, heat in a water bath at 90°C for 10 min, then extract twice with 2.5 mL of n-butanol, and extract the organic phase to obtain the derivative compound.

[0024] 3. Scan the above derivative compound solution in the wavelength range of 220-770nm, measure the fluorescence intensity at the maximum excitation wavelength of 305nm and the maximum emission wavelength of 415nm, and make a reagent blank at the same time.

[0025] 4. Take 1mL of sulfadiazine sodium standard solutions with concentrations of 0.01, 0.1, 0.5, 1.00, 5.00, and 10.00mg / L and place t...

Embodiment 2

[0032] 1. Prepare 50 mL of sulfaguanidine standard aqueous solution with a concentration of 50 mg / L, and dilute it step by step when used.

[0033]2. Take 0.5mL of sulfaguanidine aqueous solution with a concentration of 5mg / L and place it in a 10mL colorimetric tube, add 2mL of tri-acid buffer solution with pH 3 and 0.1mL of 5g / L vanillin solution successively, dilute to the mark with water, shake well Heated in a water bath at 40° C. for 35 min, and then extracted twice with 3 mL of dichloromethane to obtain a derivative compound.

[0034] 3. Measure the fluorescence intensity of the above-mentioned derivative compound solution at a maximum excitation wavelength of 290 nm and a maximum emission wavelength of 425 nm, and simultaneously make a reagent blank.

[0035] 4. Take 1mL of sulfaguanidine standard solutions with concentrations of 0.001, 0.01, 0.1, 1.00, 5.00, and 10.00mg / L, add 2mL of pH3 tri-acid buffer solution and 0.1mL of 5g / L vanillin solution in a 10mL colorimetri...

Embodiment 3

[0039] 1. Prepare 50 mL of sulfamethoxazole standard aqueous solution with a concentration of 40 mg / L, and dilute it step by step when used.

[0040] 2. Take 1 mL of sulfamethoxazole aqueous solution with a concentration of 1 mg / L and place it in a 10 mL colorimetric tube, add 1 mL of pH 5 acetic acid-sodium acetate buffer solution and 0.5 mL of 1 g / L glutaraldehyde methanol solution successively, and dilute to the mark with water , shake well, heat in a water bath at 60° C. for 25 min, and extract once with 5 mL of ethyl acetate to obtain the derivative compound.

[0041] 3. Measure the fluorescence intensity F of the above-mentioned derivative compound solution at an excitation wavelength of 303nm and an emission wavelength of 430nm, and make a reagent blank at the same time.

[0042] 4. Take 1 mL of sulfamethoxazole standard solutions with concentrations of 0.01, 0.5, 1.00, 10.00, 30.00, and 50.00 mg / L, add 1 mL of pH5 acetic acid-sodium acetate buffer solution and 0.5 mL o...

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PUM

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Abstract

The invention discloses a method for detecting residual quantity of sulfonamide in milk and meat products. Sulfonamide antibiotic residues in the milk and meat products are measured by four steps of: pretreating a sample; performing chemical reaction on the sulfonamide antibiotic and an aldehyde reagent; extracting; and adopting fluorophotometry. In the technique, derivative substances emitted by strong fluorescence are generated through the derivative reaction of sulfanilamide; and the derivative substances are extracted, so that detection sensitivity is improved, interference is eliminated, a low residual quantity detection requirement is met, system stability is improved obviously, and the defect of low fluorescence detection stability is overcome. The method has the characteristics of simpleness and quickness in operation, high detection sensitivity and the like and is operable in actual detection application.

Description

technical field [0001] The invention belongs to the technical field of food safety inspection, and relates to a method for detecting residual antibiotics in animal source food, in particular to a method for detecting residual sulfonamides in milk and meat products. Background technique [0002] Sulfonamide drugs refer to the general term of a class of drugs with p-aminobenzenesulfonamide structure, which is a class of traditional synthetic antibacterial drugs. It has a similar chemical structure to p-aminobenzoic acid (PABA). The two compete with dihydrofolate synthase, inhibit the synthesis of bacterial dihydrofolate, affect the production of bacterial nucleic acids, and prevent the growth and reproduction of bacteria. Sulfa drugs have a broad antibacterial spectrum and have inhibitory effects on most Gram-positive bacteria. Sulfa drugs can be divided into three categories according to their application, namely, sulfa drugs used for systemic infection (such as sulfadiazine...

Claims

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Application Information

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IPC IPC(8): G01N21/76G01N1/28
Inventor 杨亚玲唐慧楠
Owner 杨亚玲
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