Animal source food sulfonamide residual medium solid phase dispersion-highly effective liquid phase chromatography determination method

Abstract

The present invention relates to 'method for examining solid-phase dispersion -high performance liquid chromatogram of residues substrate of sulfonamides in animal derived food' which belongs to the field of food safety-veterinary drug residues. The method comprises of chromatogram examining steps of substrate solid-phase dispersion and high performance liquid, wherein, the mobile phase of sodium dihydrogen phosphate-acetonitrile is 50mmol / L in high performance liquid chromatogram examining method, the volume ratio of sodium dihydrogen phosphate and acetonitrile is 70:30, because the sodium dihydrogen phosphate solution is buffer solution which has a certain PH buffer capability and makes the PH value stable, the stability of pH value of HPLC mobile phase is ensured, and repeatability and reproducibility of analysis result are ensured also, at the same time, the classical process of extraction, separation, concentration and purification are simplified, the operation is simple, the milk combination phenomenon is eliminated. The method of present invention has the merits of ideal precision and sensitivity, and environment protecting by using the less toxicity organic solvent eluting analyte employed.

Description

technical field [0001] The invention belongs to the field of food safety-veterinary drug residues, in particular to a method for detecting sulfonamide drug residues in animal-derived food. Background technique [0002] Sulfonamides (SAs) are a general term for a class of drugs with the structure of p-aminobenzenesulfonamide, which are a class of traditional synthetic antibacterial drugs. It is similar to p-aminobenzoic acid (PABA) in chemical structure. The two compete with dihydrofolate synthase, inhibit the synthesis of bacterial dihydrofolate, and affect the production of bacterial nucleic acid, thereby preventing the growth and reproduction of bacteria. Sulfonamides have a broad antibacterial spectrum and have inhibitory effects on most gram-positive bacteria and some gram-negative bacteria. In animal feeding, sulfonamides are commonly used to treat livestock metritis, respiratory and digestive tract infections, swine atrophic rhinitis, fowl cholera, typhoid, paratyphoi...

AI Technical Summary

Problems solved by technology

[0007] 1) In HPLC analysis, acid (formic acid, acetic acid, phosphoric acid, etc.)-organic solvents are often used as mobile phases. Phosphoric acid, formic acid, acetic acid, etc. are volatile, and their concentration or content will change if they are left for a long time, so they are very unstable at different times. It is difficult to prepare the same precise pH value, which affects the repeatability of the analysis results in different analysis time, leads to the change of retention time, and even makes the analytes unable to separate from each other

[0008] 2) MSPD elution uses toxic organic solvent dichloromethane, which is harmful to the environment and operators

[0009] 3) The above extraction-purification pretreatment method often uses toxic organic solvents (methanol, acetonitrile) as extractants; at the same time, there are processes such as liquid-liquid distribution and concentration. Due to the poor heat resistance of sulfonamides, these processes will Cause losses and reduce the recovery rate; and this traditional sample processing method includes cumbersome and lengthy operational steps such as extraction, separation, concentration, and purification, which consume a large amount of solvents, which limits the improvement of analysis efficiency

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