Method for performing high performance liquid chromatography with fluorescence detection on residues of ampicillin and amoxicillin in aqueous product

Abstract

The invention discloses a method for performing high performance liquid chromatography with fluorescence detection on residues of ampicillin and amoxicillin in an aqueous product, which belongs to the field of food safety detection. The method comprises the following steps of: 1, preparing standard solution; 2, performing sampling, namely, uniformly dividing not less than 500 grams of mashed sample into two parts and storing the sample at -18 DEG C; 3, performing extraction, namely, adding 5 grams of sample into sodium dihydrogen phosphate, adding water for dissolution until the volume is fixed to be 500 milliliters, preparing 30 milliliters of extract, performing secondary homogenization and centrifugation, extracting supernate and adding a trichloroacetic acid into the supernate for later use; 4, performing purification, namely, rinsing a small solid-extraction column sequentially with methanol, distilled water and the trichloroacetic acid at the controlled speed of 20 drops per minute, performing complete pumping, and performing elution with 5 milliliters of ethanol; and 5, performing derivation, namely, performing blow-drying with nitrogen at 40 DEG C, adding the trichloroacetic acid and 7 percent formaldehyde solution into 0.5 milliliter of standard solution for uniform mixing, placing the mixed solution in a sealing way into a boiling water bath to perform heating for 30 minutes, eluting the solution with ecetonitrile after the solution is cooled until the volume is fixed to be 1 milliliter, and performing filtration for the liquid chromatography, wherein the limit of detection is less than 5 mu g / kg.

Description

technical field [0001] The invention relates to a high performance liquid chromatography fluorescence detection method for ampicillin and amoxicillin residues in aquatic products, belonging to the field of food safety detection. Background technique [0002] The detection methods of ampicillin and amoxicillin include thin-layer chromatography, capillary electrophoresis, chemiluminescence, liquid chromatography and chromatography. Thin-layer chromatography, capillary electrophoresis, and chemiluminescence are simple methods that do not require expensive instruments, but the detection limit is not high. The high performance liquid chromatography ultraviolet detection method has high stability and good reproducibility, but because most penicillin compounds have no characteristic absorption spectrum in the ultraviolet region, generally there is absorption at 200-235nm, but the selectivity in this wavelength range is poor. Chromatography has problems such as expensive eq...

AI Technical Summary

Problems solved by technology

Thin-layer chromatography, capillary electrophoresis, chemiluminescence, the method is simple and does not require expensive instruments, but the detection limit is not high

High-performance liquid chromatography ultraviolet detection method has high stability and good reproducibility, but because most penicillin compounds have no characteristic absorption spectrum in the ultraviolet region, generally there is absorption at 200~235nm, but the selectivity in this wavelength range is poor

Chromatography technology has problems such as expensive equipment, high requirements for testing personnel, and time-consuming analysis

The residual amount of penicillin in the sample is on the order of ug / L, and the background interference is serious. So far, there has been no report on an economical and correct detection method for the residual amount of ampicillin and amoxicillin in aquatic products, so it is necessary to study it

Images