Lab Anim Res.  2011 Mar;27(1):37-40. 10.5625/lar.2011.27.1.37.

Determination of Oxyclozanide in Beef and Milk using High-Performance Liquid Chromatography System with UV Detector

• Jo K
• Cho HJ
• Yi H
• Cho SM
• Park JA
• Kwon CH
• Park HR
• Kwon KS
• Shin HC

• KMID: 2391856
• DOI: http://doi.org/10.5625/lar.2011.27.1.37

Abstract

This study was developed and validated for the determination of oxyclozanide residue concentrations in beef and commercial milk, using high-performance liquid chromatography system. Oxyclozanide was successfully separated on a reverse phase column (Xbridge-C18, 4.6x250 mm, 5 microm) with a mobile phase composed of acetonitrile and 0.1% phosphoric acid (60:40, v/v%). This analytical procedure involved a deproteinization process using acetonitrile for beef and 2% formic acid in acetonitrile for commercial milk, dehydration by adding sodium sulfate to the liquid analytical sample, and a defatting process using n-hexane; after these steps, the extract was exposed to a stream of nitrogen dryness. The final extracted sample was dissolved in the mobile phase and filtered using a 0.45 microm syringe filter. This method had good selectivity and recovery (70.70+/-7.90-110.79+/-14.95%) from the matrices. The LOQs ranged from 9.7 to 9.8 microg/kg for beef and commercial milk. The recoveries met the standards set by the CODEX guideline.

Keyword

Determination; oxyclozanide; beef; milk; HPLC

MeSH Terms

Acetonitriles
Chromatography, High Pressure Liquid
Chromatography, Liquid
Dehydration
Formates
Milk
Nitrogen
Oxyclozanide
Phosphoric Acids
Rivers
Sodium
Sulfates
Syringes
Acetonitriles
Formates
Nitrogen
Oxyclozanide
Phosphoric Acids
Sodium
Sulfates

Figure

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  Figure 1 Chromatogram of oxyclozanide standard (25 ng).

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  Figure 2 Chromatogram of blank sample of beef and spiked sample of beef (oxyclozanide 50 ng).

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  Figure 3 Chromatogram of blank sample of milk and spiked sample of milk (oxyclozanide 25 ng).

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