Detection of illegal additive residues in food

This standard specifies a high-performance liquid chromatography fluorescence determination method for the total residue of malachite green (MG) and its metabolite leucomala-chite green (LMG), crystalline violet (GV), and its metabolite leucogen violet (LGV) in aquatic products. This standard is applicable to the determination of residual malachite green and crystal violet in the edible part of aquatic products. 2 Normative references. The clauses in the following documents become clauses of this standard through the reference surface of this standard. All subsequent amendments (excluding corrected content) or revised versions of referenced documents with date dates are not applicable to this standard. However, parties who have reached agreements based on this standard are encouraged to study whether the latest versions of these documents can be used. For undated references, the latest version applies to this standard. GB/T 6682 Specification and Test Methods for Analytical Laboratory Water (GB/T 6682-1992, neq ISO 3696; 1987) 3. The residual malachite or crystal violet in the principle sample is reduced by potassium borohydride to its corresponding metabolite, known as malachite green or dark crystal violet. Acetonitrile ammonium acetate buffer mixture extraction, dichloromethane liquid-liquid extraction, peripheral extraction column purification, reverse phase chromatography column separation, fluorescence detector detection, external standard method quantification. 4 reagents, unless otherwise specified, All reagents are analytical pure, and the test water should comply with the GB/T6682 grade water standard. 4.1 Acetonitrile: Chromatically pure. 4.2 Dichloromethane. 1.3 Acid aluminum oxide: analytically pure, with particle size ranging from 0.071 mm to 0.150 mm. 4.4 Diethylene glycol. 4.5 Potassium hydride. 4.6 Anhydrous ammonium acetate. 4.7 Glacial acetic acid. 4.8 Ammonia water. 4.9 Potassium borohydride solution [0.03 mol/L]; Weigh 0.405 g of potassium borohydride into a beaker, dissolve it in 250 mL of water, and prepare the currently used 4.10 potassium borohydride solution [0.2 mol/L]; Weigh 0.54 g of potassium borohydride in a beaker, dissolve it in 50 mL of water, and prepare for use. 4.11 20% hydroxylamine hydrochloride solution: Dissolve 12.5 g of hydroxylamine hydrochloride in 50 mL of water. 4.12 p-toluenesulfonic acid solution [0.05 mol/L]: Weigh 0 95 g of p-toluenesulfonic acid, diluted with water to 100 mL. 4.13 ammonium acetate buffer solution [0 1 mo/L]; Weigh 7.71 g of anhydrous ammonium acetate and dissolve it in 1000 mL of water, adjust the pH to 10.0.4.14 with ammonia buffer solution [0.125 mol/L]: Weigh 9.64 g of anhydrous ammonium acetate and dissolve it in 1000 mL of water, adjust the pH to 4.5.4 with glacial acetic acid 15 acidic alumina solid-phase extraction column: 500 mg. 3 mL. Activate with 5 mI acetonitrile before use. 4 16 Varian PRS column or equivalent: 500 mg, 3 mL. Activate with 5 mL of acetonitrile before use

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