High performance liquid chromatography for detection of residual ceftiofur in pork tissues

A technology of high performance liquid chromatography and ceftiofur, which is applied in the field of high performance liquid chromatography, can solve the problems of non-detection high performance liquid chromatography, and achieve the effects of high repeatability, high resolution and high analysis accuracy

Inactive Publication Date: 2016-01-27
JIANGSU WISE SCI & TECH DEV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

There is currently no patent on HPLC for the detection of ceftiofur residues

Method used

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  • High performance liquid chromatography for detection of residual ceftiofur in pork tissues
  • High performance liquid chromatography for detection of residual ceftiofur in pork tissues
  • High performance liquid chromatography for detection of residual ceftiofur in pork tissues

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Experimental program
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Embodiment Construction

[0013] 1. Solution preparation:

[0014] Ceftiofur stock solution (100mg / L): Weigh 10.0mg of ceftiofur standard product into a 100mL volumetric flask, dissolve in methanol and make to volume, store at -20°C, and it can be used for 6 months;

[0015] Ceftiofur intermediate solution (5mg / L): Pipette 250μL of 100mg / L ceftiofur stock solution into a 5mL volumetric flask, dilute to volume with 0.025mol / L phosphate buffer (pH7.0), shake well (ready for immediate use) ;

[0016] 0.025mol / L phosphate buffer (pH7, 0) ： Dissolve 3.4g potassium dihydrogen phosphate in 900mL water, adjust the pH value to 710 with 450g / L potassium hydroxide solution, and dilute to 1L with water;

[0017] 0.05mol / L boric acid buffer: weigh 19g sodium borate and 3.7g potassium chloride, and dilute to 1L with water;

[0018] 4g / L dithioerythritol solution: Weigh 1.0g dithioerythritol and dissolve in 250mL0.05mol / L boric acid buffer solution (preparation and use now);

[0019] 40g / L iodoacetamide solution ...

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Abstract

The invention discloses a high performance liquid chromatography (HPLC) for detection of residual ceftiofur in pork tissues. The ceftiofur relevant residual amount in cattle and pig muscles and kidneys is determined by the high performance liquid chromatography. A sample is extracted by a dithioerythritol solution, is derived by amide, is purified by solid phase extraction columns (C18, SAX and SCX), is separated by 8 column chromatography, and is subjected to gradient elution with acetonitrile-water (with the volume ratio of 15 to 85) containing a 0.1% trifluoroacetic acid as a mobile phase, and is subjected to 6 nm ultraviolet detection. The ceftiofur residual amount shows good linearity with a peak area within 0.016-1.28 mg/L, and the correlation coefficient r is more than 0.9999. The recovery rate with the sample addition concentration of 200-8000 [mu]g/kg is 90%-91%, and the relative standard deviation is 118%-315%. The detection limit of the method (the signal-to-noise ratio S/N is 3) is 50 [mu]g/kg. The method comprises the following steps: 1, instruments and reagents; 2, solution preparation; 3, sample treatment; 4, standard substance treatment; 5, experiment implementation; and 6, data processing.

Description

technical field [0001] The invention relates to a high-performance liquid chromatography method for detecting ceftiofur residue in pork tissue, belonging to the field of biological detection. Background technique [0002] Ceftiofur (ceftiofur), also known as Saidefu, is the first third-generation cephalosporin antibiotic exclusively for animals. In 1988, the FDA approved ceftiofur sodium for the treatment of bovine respiratory bacterial diseases, when the drug was first marketed in the United States. Since then, FDA has successively approved ceftiofur sodium, ceftiofur hydrochloride and ceftiofur crystalline free acid for the treatment of respiratory diseases in 1-day-old chickens, turkeys, pigs, beef cattle, dairy cows, horses, goats and sheep. Canada, Japan and some European countries have also officially approved it for the treatment of respiratory diseases in pigs, beef cattle, dairy cows and sheep. Ceftiofur has a broad antibacterial spectrum and strong antibacterial ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
Inventor 杜霞刘静洪霞
Owner JIANGSU WISE SCI & TECH DEV
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