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
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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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