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A method for sulfonamide medicine extraction and analysis by utilizing a DPX pipette tip type dispersive solid-phase extraction microcolumn

A technology of sulfonamide drugs and dispersed solid phase, which is applied in the directions of analysis materials, material separation, measuring devices, etc., can solve the problems of unfavorable qualitative and quantitative analysis, failure to meet detection requirements, complicated operation steps, etc., and achieves low total cost, The effect of heavy linear stability and convenient operation

Active Publication Date: 2018-12-04
无锡微色谱生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, some of these methods cannot meet the current detection requirements, and some of the entire operation steps are cumbersome and time-consuming, which is not conducive to accurate qualitative and quantitative analysis

Method used

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  • A method for sulfonamide medicine extraction and analysis by utilizing a DPX pipette tip type dispersive solid-phase extraction microcolumn
  • A method for sulfonamide medicine extraction and analysis by utilizing a DPX pipette tip type dispersive solid-phase extraction microcolumn
  • A method for sulfonamide medicine extraction and analysis by utilizing a DPX pipette tip type dispersive solid-phase extraction microcolumn

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specific Embodiment approach 1

[0032] Specific embodiment one: a kind of method of utilizing DPX gun tip type dispersion solid-phase microextraction column of the present embodiment to extract and analyze sulfonamides, it is to carry out according to the following steps:

[0033] 1. Sample extraction: Weigh the sample, add deionized water and homogenize it, then add acetonitrile, vortex, then centrifuge, collect the supernatant, blow dry with nitrogen, and use a volume percentage of 3-7%. After 700-800 μL of formic acid aqueous solution is dissolved, the purified solution is obtained;

[0034] 2. Purification: first clean the DPX Tips TM -CX tip-type dispersive solid-phase microextraction column is equilibrated with 450-550μL methanol and 450-550μL volume percentage of 1-3% formic acid aqueous solution; then pipette the liquid to be purified through the column; The volume percentage is 3-7% formic acid aqueous solution, 700-800 μL methanol to wash the column; finally use 700-800 μL eluent to elute; collect...

specific Embodiment approach 2

[0054] Embodiment 2: This embodiment differs from Embodiment 1 in that the mass-to-volume ratio of the sample to water described in step 1 is 202-108 mg: 1 μL. Others are the same as in the first embodiment.

specific Embodiment approach 3

[0055] Embodiment 3: This embodiment differs from Embodiment 1 in that the mass volume ratio of the sample to acetonitrile described in step 1 is 0.202-0.108 mg: 1 mL. Others are the same as in the first embodiment.

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Abstract

The invention provides a method for sulfonamide medicine extraction and analysis by utilizing a DPX pipette tip type dispersive solid-phase extraction microcolumn, and relates to sulfonamide medicineresidue detection methods for animal-sourced foods. The method is provided to overcome a problem that there is no effective method for sulfonamide medicine detection for animal-sourced foods, especially quantitative, high-precision, high-throughput and low-consumption determination. A high performance liquid chromatography-tandem mass spectrometry manner for residue analysis of twelve sulfonamidemedicines in animal-sourced foods is established in the method. The method is suitable for residue amount detection of one or a plurality of medicines selected from sulfacetamide, sulfapyridine, sulfamerazine, sulfamethazine, sulfamethoxypyridazine, sulfamonomethoxine, sulfochloropyridazine, sulfamethoxazole, sulfadimethoxypyridazine, sulfadimethisoxazol, sulfabenzamide and sulfaquinoxalin in animal-sourced foods.

Description

technical field [0001] The invention relates to a method for detecting sulfonamide residues in animal-derived foods. Background technique [0002] Sulfonamides are a class of chemotherapeutic drugs used to prevent and treat bacterial infectious diseases. They are all derivatives of sulfonamide in composition, and have a benzene ring and a para-position in the chemical structure. Amino group, 1 sulfonamide group. Because of its broad antibacterial spectrum, stable properties, many varieties, and low price, it is widely used in food animals as preventive and therapeutic drugs. Sulfonamides are commonly used to prevent pullorum, coccidiosis, appenditis, hepatitis and other bacterial diseases in animal breeding, and are widely used as feed additives, mainly for fattening livestock, preventing and treating bacterial infectious diseases. The action time and metabolism time of sulfa drugs in animals are relatively long, which often results in sulfa drug residues in edible tissues...

Claims

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Application Information

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IPC IPC(8): G01N30/06G01N30/02
CPCG01N30/02G01N30/06G01N2030/027
Inventor 王倩卡莫莱杨佳费静王珏
Owner 无锡微色谱生物科技有限公司
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