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

A high-performance liquid chromatography, sulfonamide drug technology, applied in the field of food safety-veterinary drug residues, can solve the problems of retention time change, consumption of a large amount of solvent, poor heat resistance of sulfonamide drugs, etc., and achieves easy control and stability of pH value. Results that guarantee repeatability and reproducibility, ideal accuracy and sensitivity

Inactive Publication Date: 2008-08-13
BEIJING JINXIU DADI AGRI CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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

Method used

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

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Example 1: Detection of fish meat samples

[0025] 1. Main equipment and medicines

[0026] instrument:

[0027] 1) Glass mortar;

[0028] 2) Glass syringe 5mL

[0029] 3) SPE solid phase extraction device

[0030] 4) Nitrogen blower with constant temperature water bath

[0031] 5) Pipette 1mL, 0.5mL

[0032] 6) Volumetric flask 10mL

[0033] 7) Electronic balance (division value 0.001g)

[0034] 8) Timer

[0035] 9) Vortex mixer

[0036] 10) Liquid Chromatograph

[0037] drug:

[0038] 1) Standard material (purity ≥98.5%): sulfadiazine, sulfamerazine, sulfamethazine, sulfamonomethoxine, sulfamonomethoxine ( sulfadoxine), sulfamethoxazole (sulfamethoxazole), sulfaquinoxzline (sulfaquinoxzline), sulfadimethoxine (sulfadimethoxine) standard solution.

[0039] 2) Acetonitrile, ethyl acetate, methanol (chromatographically pure)

[0040] 3) n-hexane, sodium dihydrogen phosphate (analytical grade)

[0041] 4) Anhydrous sodium sulfate (analytical grade), dried at...

Embodiment 2

[0078] Example 2 Detection of pork samples

[0079] The operation steps are the same as above, and the HPLC test results of pork samples are shown in image 3 .

[0080] Under the analytical conditions established by the present invention, the chromatograms ( image 3 , figure 2 and figure 1 ), it can be seen from the separation effect of these chromatograms that there is no matrix interference to affect the determination of the drug, and the separation effect is very good.

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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...

Claims

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Application Information

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IPC IPC(8): G01N30/50G01N30/02
Inventor 赵海香赵孟彬邓维
Owner BEIJING JINXIU DADI AGRI CO LTD
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