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Method for extraction and derivatization of piperazine residues in tissue of fowls and pigs

A derivatization and piperazine technology, applied in the fields of solid phase extraction purification and acetic anhydride pre-column derivatization, can solve the problems of poor peak shape and tailing

Active Publication Date: 2016-09-21
YANGZHOU UNIV
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Problems solved by technology

Since there are two imino groups in the molecular structure of piperazine, the polarity is strong, the peak shape in the gas chromatography separation is poor, and there is serious tailing phenomenon, so the piperazine molecule is directly applied to the research and analysis of gas chromatography tandem mass spectrometry. Application not yet reported

Method used

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  • Method for extraction and derivatization of piperazine residues in tissue of fowls and pigs
  • Method for extraction and derivatization of piperazine residues in tissue of fowls and pigs
  • Method for extraction and derivatization of piperazine residues in tissue of fowls and pigs

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Experimental program
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Embodiment Construction

[0014] 1. Experiment with poultry and pig feeding and sample collection

[0015] Three-way cross-bred pigs and poultry were selected at the market age, namely, 16-week-old Jinghai yellow chicken, 10-week-old Yangzhou goose, 8-week-old cherry valley duck, and 6-month-old Du×long×big three-way crossbred pigs 6 The head, half male and half female, are raised in a single cage (column), fed with full feed without any drugs, and free drinking water. After 2 weeks of feeding, muscle, liver, kidney, skin and adipose tissue of the test animals were taken as blank tissue samples when they were slaughtered, and stored at -35°C. The samples were minced and homogenized during use.

[0016] 2. The extraction, purification and derivatization steps of the present invention

[0017] 1) Accurately weigh (2.0±0.02)g of a homogenized blank tissue sample, grind and mix with 3.0g anhydrous sodium sulfate in a mortar to absorb sample moisture;

[0018] 2) Add about 3.0g of diatomaceous earth and grind it t...

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Abstract

The invention specifically relates to a method for extraction, purification and derivatization of piperazine residues in the tissue of fowls and pigs. The method comprises the following steps: with pure acetonitrile as an extraction solvent and n-hexane as a degreasing agent, treating a tissue sample by using an accelerated solvent extraction instrument (ASE); continuously carrying out on-line degreasing and piperazine extraction; subjecting the obtained extract to purification via a solid-phase extraction method, concentration by a vacuum centrifugation concentration instrument and acetic anhydride-process precolumn derivatization; and carrying out confirmatory analysis on the extracted, purified and derivatized sample by using gas chromatography-tandem mass spectrometry (GC-MS / MS). With the method, the extraction rate of piperazine reaches 90% or above.

Description

Technical field [0001] The invention relates to the field of veterinary drug residue detection, in particular to a method for accelerated solvent extraction method extraction, solid phase extraction method purification and acetic anhydride method precolumn derivatization of piperazine residue in poultry and pig tissues. Background technique [0002] When testing veterinary drugs in animal-derived foods, only when the drugs are extracted from the sample can an efficient detection method be established. Anhydrous piperazine is transparent needle-like or leaf-like crystals, odorless, hygroscopic and typical ammonia smell. It absorbs water and carbon dioxide in the air. It is easily soluble in water and glycerin, slightly soluble in ethanol, and insoluble in ether. There are many reports on the extraction method of piperazine at home and abroad. The extraction agent is generally methanol, acetonitrile, trichloroacetic acid solution and perchloric acid solution, etc., and the extracti...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06G01N2030/025G01N2030/062G01N2030/067
Inventor 谢恺舟刘亚楠庞茂达谢星崔璐璐王波高强张杨杨张跟喜戴国俊卜仕金王冉王金玉
Owner YANGZHOU UNIV
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