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1 Scope of application
It is suitable for the determination of 16 sulfonamide residues in beef, mutton, pork, chicken and rabbit meat by liquid chromatography-tandem mass spectrometry
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Detection limit of method: sulfamethizole is 2.
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2 Principle of the method
Sulfonamide residues in livestock and poultry meat were extracted with acetonitrile.
After centrifugation, the supernatant was concentrated by a rotary evaporator to nearly dryness.
The residue was dissolved in mobile phase and degreased with n-hexane.
The sample solution was measured by liquid chromatography-tandem mass spectrometry.
Quantification by external standard method
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3 Reagents and materials
Acetonitrile : chromatographically pure isopropanol, n-hexane , ammonium acetate: analytically pure
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Anhydrous sodium sulfate: analytically pure, burned at 650°C for 4h, and placed in a desiccator.
Mobile phase: acetonitrile + 0.
01mol/L ammonium acetate solution (12+88, v/v)
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16 kinds of sulfa standard stock solutions: 0.
1mg/mL
Matrix mixed standard working solution: According to the sensitivity of each sulfonamide and the linear range of the instrument, the blank sample extract is used to prepare matrix mixed standard working solutions of different concentrations (ng/mL).
The matrix mixed standard working solution is stored at 4℃, and can be used 1 Week
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4 Apparatus and equipment
Liquid chromatography-tandem mass spectrometer: equipped with electrospray ion source; homogenizer, rotary evaporator, liquid mixer, centrifuge; analytical balance: sensitivity 0.
1 mg, 0.
01 g; pipette: 1 mL, 2 mL; chicken heart Bottle: 100mL; sample bottle: 2mL, with Teflon screw cap
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5 Sample pretreatment
(1) Sample preparation
Take out a representative sample of about 1 kg from all the samples, fully mash, mix, and divide them into two parts, and put them into clean containers
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Seal as a sample and mark it
(2) Sample extraction and purification
Weigh 5g sample, accurate to 0.
01g, place it in a 50mL centrifuge tube, add 20g anhydrous sodium sulfate and 20mL acetonitrile, homogenize for 2 minutes, and centrifuge at 3000r/min for 3 minutes
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Pour the supernatant into a 100 mL chicken heart bottle, add 20 mL of acetonitrile to the residue, and repeat the above operation once
Related links: Determination of 18 sulfonamide residues in royal jelly by liquid chromatography-tandem mass spectrometry (3)
