Detection method of residual amount of a plurality of macrolide veterinary drugs in casings

A technology for macrolides and veterinary drug residues, applied in the field of analytical chemistry and food safety, to achieve high recovery rate, good purification effect, and strong anti-interference ability

Inactive Publication Date: 2012-01-11
林维宣
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  • Abstract
  • Description
  • Claims
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  • Detection method of residual amount of a plurality of macrolide veterinary drugs in casings
  • Detection method of residual amount of a plurality of macrolide veterinary drugs in casings
  • Detection method of residual amount of a plurality of macrolide veterinary drugs in casings

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Embodiment 1

[0056] Example 1 Detection method of multiple macrolide veterinary drug residues in casings

[0057] 1. Sample extraction:

[0058] (1) Methanol extraction method: Weigh 5 g of uniform sample into a 50 mL centrifuge tube with a stopper, add 25 mL of methanol, vortex, centrifuge at 4000 r / min for 3 min, and collect the upper methanol extract in a 50 mL capacity Add another 20 mL of methanol to the bottle, repeat the above operation, combine the methanol extracts, add methanol to make up to 50 mL. Precisely measure 10 mL of methanol extract into a 20 mL centrifuge tube, concentrate under reduced pressure in a water bath below 45 °C until nearly dry, and dissolve the residue in 10 mL of phosphate buffer solution in stages.

[0059] (2) Acetonitrile extraction method: Weigh 5 g uniform sample into a 50 mL stoppered centrifuge tube, add 25 mL of acetonitrile, vortex, centrifuge at 4000 r / min for 3 min, collect the upper acetonitrile extract in a 50 mL capacity Add another 20 mL o...

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Abstract

The invention relates to the fields of analytical chemistry and food safety, and provides a detection method of the residual amount of a plurality of macrolide veterinary drugs in casings. The detection method comprises the following steps of: extracting a sample with methanol or acetonitrile; purifying the obtained extracting solution by a C18 or Oasis HLB (hydrophilic-lipophilic balance) solid-phase extraction column, taking an acetonitrile-methanoic acid aqueous solution with the concentration of 0.15% as a mobile phase, and performing gradient elution by adopting a ZORBAX Eclipse C8 analytical column; and performing electro-spraying, separating by a cationic scanning mode and detecting the residual amount of seven types of macrolide veterinary drugs. The detection lower limit of the seven types of macrolide veterinary drugs is 20 mu g/kg. The recovery rates of spiramycin, tilmicosin, oleandomycin, tylosin, erythrocin, roxithromycin and josamycin are respectively 71.4-78.8, 75.7-85.6, 81.1-85.8, 78.9-83.0, 87.1-89.6, 83.7-85.4 and 75.6-81.8; and the indoor relative standard deviations for the recovery rates of the spiramycin, the tilmicosin, the oleandomycin, the tylosin, the erythrocin, the roxithromycin and the josamycin are respectively 7.7-11.1, 8.0-15.7, 10.5-16.4, 8.1-12.5, 10.5-12.4, 10.6-14.4 and 7.8-18.0. The detection limit, the recovery rate, the precision and the like meet the related requirements at home and abroad.

Description

technical field [0001] The invention relates to the fields of analytical chemistry and food safety, in particular to a method for detecting residues of various macrolide veterinary drugs in casings, in particular to spiramycin, tilmicosin, oleandomycin, Liquid chromatography-mass spectrometry / mass spectrometry detection method for the residues of seven veterinary drugs such as erythromycin, erythromycin, roxithromycin, and josamycin. Background technique [0002] Macrolide antibiotics (MALs) are a class of basic antibiotics with similar chemical structures and antibacterial effects. Growth promoters occupy an important position in animal medicines and feed additives. However, when such antibiotics are used excessively or improperly, residues of macrolide antibiotics and their metabolites will be caused, and enter the human body through the food chain, and accumulate to a certain extent in internal organs, which can cause damage to the vestibule and cochlear nerves, resultin...

Claims

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Application Information

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IPC IPC(8): G01N30/88G01N30/06
Inventor 林维宣蒋维旗赵雪荣陈溪
Owner 林维宣
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