Matrix Solid-Phase Dispersion (MSPD) Isolation and Liquid Chromatographic Determination of Oxytetracycline, Tetracycline, and Chlortetracycline in Milk

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  • Austin R Long
    Louisiana State University, School of Veterinary Medicine, Department of Veterinary Physiology, Pharmacology and Toxicology, Baton Rouge, LA 70803
  • Lily C Hsieh
    Louisiana State University, School of Veterinary Medicine, Department of Veterinary Physiology, Pharmacology and Toxicology, Baton Rouge, LA 70803
  • Marsha S Malbrouh
    Louisiana State University, School of Veterinary Medicine, Department of Veterinary Physiology, Pharmacology and Toxicology, Baton Rouge, LA 70803
  • Charles R Short
    Louisiana State University, School of Veterinary Medicine, Department of Veterinary Physiology, Pharmacology and Toxicology, Baton Rouge, LA 70803
  • Steven A Barker
    Louisiana State University, School of Veterinary Medicine, Department of Veterinary Physiology, Pharmacology and Toxicology, Baton Rouge, LA 70803

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<jats:title>Abstract</jats:title> <jats:p>A multlresldue method for the isolation and liquid chromatographic determination of oxytetracycline (OTC), tetracycline (TC), and chlortetracycllne (CTC) antibiotics In milk Is presented. Blank and tetracycline (OTC, TC, and CTC) fortified milk samples (0.5 mL) were blended with octadecylsllyl (C18, 40 /an, 18% load, endcapped, 2 g) derivatized silica packing material containing 0.05 g each of oxalic acid and dlsodlum ethylenedlamlnetetraacetlc. A column made from the C18/milk matrix was first washed with hexane (8 mL), following which the tetracyclines were eluted with ethyl acetate-acetonltrlle (1 + 3; v/v). The eluate contained tetracycline analytes that were free from Interfering compounds when analyzed by liquid chromatography with UV detection (photodiode array, 365 nm). Correlation coefficients of standards curves for Individual tetracycline isolated from fortified samples were linear (from 0.982 ± 0.009 to 0.996 ± 0.004) with average percentage recoveries from 63.5 to 93.3 for the concentration range (100,200,400,800,1600, and 3200 ng/ mL) examined. The Inter-assay variability ranged from 8.5 ± 2.4% to 20.7 ± 13.0% with an Intra-assay variability of 1.0- 9.3%.</jats:p>

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