• Decrease font size
  • Return font size to normal
  • Increase font size
U.S. Department of Health and Human Services

CVM Publications - Detail

  • Print
  • Share
  • E-mail
-
 
TITLE:  Determination of trichlormethiazide in bovine milk by high-performance liquid chromatography
 
AUTHORS:  Shaikh B;Rummel N;
 
YEAR:  1998
 
JOURNAL ABBREV:  J Chromatogr B Biomed Sci Appl
 
MONTH:  May
 
TYPE:  JOUR
 
REFMAN INDEX:  123
 
JOURNAL FULL:  Journal of chromatography B, Biomedical sciences and applications
 
VOLUME:  709
 
ISSUE:  1
 
START PAGE:  137
 
END PAGE:  143
 
KEYWORDS:  analysis;Animals;Calibration;Cattle;Centrifugation;chemistry;Chromatography;Chromatography,High Pressure Liquid;Diuretics;Food;methods;Milk;Reproducibility of Results;Sensitivity and Specificity;Sodium;Trichlormethiazide;veterinary;Veterinary Medicine;
 
ABSTRACT:  A liquid chromatographic procedure was developed and validated for the quantitative determination of trichlormethiazide (TCMTZ) in bovine milk. Whole milk was defatted by initial centrifugation at 4 degrees C. The resulting skim milk was treated with lead acetate and acetonitrile, vortex mixed, and centrifuged. The acetonitrile from the supernatant was back extracted in ethyl acetate. The organic solvent mixture which contained TCMTZ was further treated with sodium tungstate, vortex mixed, and centrifuged. The top organic layer was removed and evaporated to dryness; the resulting residue was reconstituted in the mobile phase, and the final extract was analyzed by high-performance liquid chromatography (HPLC). The HPLC conditions employed included a polymer column, a mobile phase consisting of 30% acetonitrile or 30% acetonitrile-tetrahydrofuran (2:1, v/v) in a phosphate buffer (pH 3), and a UV detection at 225 nm. The average recoveries of TCMTZ from milk fortified at 7, 14, 35, 70, and 140 ppb were 88, 93, 117, 110, and 99%, respectively, with corresponding C.V. values of 7, 18, 11, 9, and 21%. The method was validated by assaying milk obtained from a cow dosed with Naquasone. TCMTZ concentration was detected only in the 8 h post dose milk samples and was determined to be 6 ppb
 
AFFILIATIONS:  Center for Veterinary Medicine, US Food and Drug Administration, Laurel, MD 20708, USA
 
-
-