Publications by authors named "Philip Kijak"

Background: Oxytetracycline (OTC), chlortetracycline (CTC), and tetracycline (TC) are approved antibiotics used to treat bacterial infections in cattle. To ensure human food safety, a tolerance has been established for the sum of these three TC residues as 12 parts per million in bovine kidney in the United States The current official regulatory method for quantifying these antibiotics in the target organ is a labor-intensive microbiological assay.

Objective: Our laboratory developed and validated a fast, selective, and less laborious method utilizing LC-tandem mass spectrometry for the determination and confirmation of the three tetracyclines (TET) in bovine kidney.

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Article Synopsis
  • Antibiotics are used in ethanol production to prevent bacterial growth, but their residues in distillers grain can pose public health risks due to antimicrobial resistance.
  • An objective was to validate the robustness of an LC-MS/MS method for detecting specific antibiotic residues in distillers grain through a multi-laboratory study.
  • Results showed the method has high accuracy and acceptable reproducibility, making it suitable for regulatory compliance in monitoring antibiotic contaminants in distillers grain.
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A validation study was conducted for an immunochromatographic method (BetaStar Advanced for Beta-lactams) for the detection of beta-lactam residues in raw, commingled bovine milk. The assay detected amoxicillin, ampicillin, cloxacillin, penicillin, cephapirin, and ceftiofur below the U.S.

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A validation study was conducted for an immunochromatographic method (BetaStar Advanced for Tetracyclines) for detection of tetracycline antibiotic residues in raw, commingled bovine milk. The assay was demonstrated to detect tetracycline, chlortetracycline, and oxytetracycline at levels below the FDA tolerance levels but above the maximum sensitivity thresholds established by the National Conference on Interstate Milk Shipments. Results of internal and independent laboratory dose-response studies employing spiked samples were in agreement.

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Since 2007, the U.S. FDA's Center for Veterinary Medicine (CVM) has been investigating reports of pets becoming ill after consuming jerky pet treats.

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Ceftiofur is a widely used cephalosporin β-lactam antibiotic with frequently reported residue violations. This paper reports a liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for determining a ceftiofur metabolite, desfuroylceftiofur cysteine disulfide (DCCD), in bovine kidney, liver, and muscle tissues. Incurred tissue samples were obtained from dosed animals and analyzed to evaluate the utility of the method.

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A simple, robust LC-UV method was developed to assay erythromycin in medicated salmonid feed. In this method, erythromycin was extracted from feed with acetonitrile and water, cleaned up by SPE, evaporated to dryness, reconstituted, and analyzed by LC-UV. The resulting method produced high accuracy, 82-90%, for both salmon and trout feed that represented varied pellet sizes and ingredient amounts.

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Ceftiofur is a cephalosporin β-lactam antibiotic widely used for treating certain bacterial infections in beef and dairy cattle. The regulatory HPLC-UV method for ceftiofur residues in animal tissues is time consuming and non-specific. Additionally, because the regulatory method involves chemical reactions to convert the metabolites into a single moiety, it is virtually impossible to incorporate the procedure into a multi-residue method.

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A multiclass/multiresidue method has been developed and validated for the determination of 21 veterinary drug residues in shrimp, including sulfonamides (sulfadiazine, sulfamerazine, sulfamethazine, sulfachloropyridazine, sulfadimethoxine, and sulfaquinoxaline); tetracyclines (oxytetracycline, tetracycline, and chlortetracycline); (fluoro)quinolones (norfloxacin, ciprofloxacin, enrofloxacin, sarafloxacin, difloxacin, flumequine, oxolinic acid, and nalidixic acid); and cationic dyes (malachite green, gentian violet, leucomalachite green, and leucogentian violet), using HPLC/MS/MS. All drugs were quantifiable over a no less than 10-fold range with matrix-matched standards for linear external calibration, except for oxytetracycline, tetracycline, norfloxacin, and ciprofloxacin, for which norfloxacin-d5 was used as an internal standard. Two grams of preground shrimp sample was extracted twice with extractant at two different pH values.

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A quantitative method was developed and validated to measure the concentration of sulfadimethoxine (SDM) and its major metabolite, (4)N-acetylsulfadimethoxine (AcSDM), in bovine tissues and body fluids. Liquid chromatography/tandem mass spectrometry (LC/MS/MS) gave quantitative results for these two analytes in extracts from bovine plasma, urine, oral fluid, kidney, and liver, using SDM-d(4) as internal standard (I.S.

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A liquid chromatography-mass spectrometry (LC-MS) method was developed to screen and confirm veterinary drug residues in raw shrimp meat. This method simultaneously monitors 18 drugs of different classes, including oxytetracycline (OTC), sulfonamides, quinolones, cationic dyes, and toltrazuril sulfone (TOLS). The homogenized shrimp meat is extracted with 5% trichloroacetic acid.

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Article Synopsis
  • Chloramine-T is being developed as a disinfectant to treat bacterial gill disease in cultured fish, and a method is needed to confirm its residues in fish tissue.
  • The metabolite para-toluenesulfonamide (p-TSA) is used as a marker to track the depletion of chloramine-T residues.
  • A detailed procedure for extracting and analyzing p-TSA from fish tissue involves multiple chemical steps and uses gas chromatography/mass spectrometry to confirm its presence at levels as low as 20 parts per billion (ppb).
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