Method for extracting piperazine residue from chicken tissue, egg and pork by using accelerated solvent extraction instrument and derivatizing

Abstract

The invention relates to a method for extracting a piperazine residue from a chicken tissue, an egg and pork by using an accelerated solvent extraction instrument and derivatizing. The method is as follows: grinding a blank sample of kieselguhr, putting in an extraction pond, extracting through ASE (Accelerated Solvent Extraction), sequentially extracting with n-hexane and formic acid acetonitrileat the static state; purifying an extract liquor through a Strata-X-C column, collecting a sample solution, and blowing dry in a termovap sample concentrator; redissolving with acetonitrile, conducting ultrasonic treatment, shaking up evenly, transferring a trimethylamine and dansyl chloride solution, metering the volume by using the acetonitrile, reacting in the dark place, processing through a0.22 mum organic phase syringe filter after finishing the reaction, and conducting HPLC-FLD detection on a filtrate. By adopting the method, the extraction and recovery rates of the piperazine in thechicken tissue, the egg and the pork at the fortified concentration of LOQ are both more than or equal to 72.86%, the extraction and recovery rates of the piperazine at the fortified concentrations of0.5 MRL, 1.0 MRL an 2.0 MRL are more than or equal to 82.26%, and the requirement of a method for detecting the residue of a veterinary drug is met.

Description

technical field [0001] The invention relates to the field of detection of veterinary drug residues, in particular to a method for extracting and derivatizing piperazine residues from chicken tissues, eggs and pork with an accelerated solvent extraction apparatus. Background technique [0002] When detecting veterinary drugs in food of animal origin, only by extracting the drugs from the samples can an efficient detection method be established. Piperazine is a white needle-like crystal, weakly alkaline, highly polar, and easily soluble in water, methanol, and acetonitrile. Piperazine has no ultraviolet or fluorescent groups, and needs to react with fluorescent reagents to generate ultraviolet or fluorescent substances for detection by fluorescence detectors. Domestic methods for extracting piperazine from chicken tissues, eggs and pork are mainly liquid-liquid extraction methods, and the extraction agents are generally acidic aqueous solution and acetonitrile solution. But ...

AI Technical Summary

Problems solved by technology

[0003] In order to solve the problem of extracting and derivatizing piperazine from chicken tissues, eggs and pork, the present invention adopts accelerated solvent extraction (ASE) technology to extract piperazine residues in chicken tissues, eggs and pork, and uses DNS-Cl to react with them

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