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Biomedical subjects

R B Ashworth

Publications and source records attributed to R B Ashworth.

17 recordsLinked to original sources

Tissue sulfonamide concentration and correlation in turkeys.

Nineteen hen turkeys (10 to 12 kg each) were used in a feeding study to determine sulfadimethoxine and sulfaquinoxaline concentrations in blood serum, liver, and skeletal muscle, as well as the respective ratios at selected withdrawal intervals. Two feeds were prepared by use of premixes to achieve 60 mg of sulfadimethoxine/kg and 100 mg of sulfaquinoxaline/kg, respectively. Each of the medicated feeds was given to 9 turkeys for 7 days. The turkeys were then fed nonmedicated feed at intervals from 24 to 56 hours and were slaughtered. One turkey was used as control. The serum/liver and serum/muscle ratios for sulfaquinoxaline were 60 to 70% higher than for sulfadimethoxine. However, the liver/muscle ratio for both sulfonamides was equivalent, approximately 3. Disposition of both sulfonamides approximated first-order pharmacokinetics. The calculated half-life of sulfadimethoxine was half that of sulfaquinoxaline, approximately 16 vs 30 hours. The coefficients of variation in the serum/tissue ratios for both sulfonamides were between 13% and 25% for serum/liver and less than 15% for serum/muscle, indicating excellent potential for using serum as a predictor of actionable concentrations of sulfonamide residues.

Animal Feed

Chloramphenicol concentrations in calf muscle tissue.

Twenty-five 9- to 11-week-old calves were administered 2 doses of chloramphenicol prepared in propylene glycol (13.6 mg/kg of body weight IV; 6.8 mg/kg IM; or 13.6 mg/kg IM) at 24-hour intervals. Calves were euthanatized at designated times from 2 to 72 hours after the last dose was administered. Muscle tissues were collected immediately after euthanasia, and chloramphenicol concentrations in the tissues were determined.

Animals

Sulfamethazine blood/tissue correlation study in swine.

Seventy market-weight hogs (90 to 113 kg) were used in a feeding study to determine the correlation of serum sulfamethazine concentrations with sulfamethazine concentrations in liver and muscle at time of slaughter. Test groups were fed medicated feeds prepared from commercial medicated premixes containing 110 g of sulfamethazine/metric ton for 30 days. Fifteen days before hogs were slaughtered, test groups were given maintenance feeds containing 1.1 to 13.9 g of sulfamethazine/metric ton and were fed these diets until slaughtered. Comparison of data from positive- and negative-control groups indicated that total withdrawal of sulfamethazine in the feed was not necessary for the liver to contain less than the allowed tolerance of 0.1 mg of sulfamethazine/kg of liver at slaughter. Feed concentrations of up to 2 g of sulfamethazine/metric ton could be tolerated in withdrawal feeds before liver sulfamethazine values exceeded 0.1 mg/kg of liver. Serum/tissue sulfamethazine ratios were erratic in hogs given 1.1 to 2.7 g of sulfamethazine/metric ton, but became less variable in hogs given greater than 5.7 g/metric ton. Feed concentrations greater than 8 g of sulfamethazine/metric ton produced values greater than 0.1 mg/kg of muscle and values of about 0.4 mg/kg of liver. When serum sulfamethazine concentrations alone were used as a predictor for tissue sulfamethazine values, 100% of the liver values exceeded 0.10 mg/kg of liver when sulfamethazine in serum was greater than 0.45 mg/L. However, 57.4% of samples having serum concentrations between 0.10 and 0.45 mg/L had associated sulfamethazine values greater than 0.1 mg/kg of liver. All hogs having serum sulfamethazine concentrations less than 0.1 mg/L had sulfamethazine concentrations less than 0.1 mg/kg of liver.

Animal Feed

Quantitative thin layer chromatographic multi-sulfonamide screening procedure: collaborative study.

A thin layer chromatographic procedure suitable for detection of multiple sulfonamides at 0.1 ppm was studied in an interlaboratory collaborative study. Sulfamethazine, sulfadimethoxine, and sulfaquinoxaline were variously analyzed in liver and muscle tissues from swine, turkey, and duck. The average recovery for all drugs across all tissues was 95%. The corresponding repeatability and reproducibility were 7.7% and 10.5%, respectively.

Animals

A high performance liquid chromatographic system for the analysis of tetracycline drug standards, analogs, degradation products and other impurities.

This paper describes the high performance liquid chromatographic (HPLC) analysis of eight parent tetracycline standards: tetracycline, chlortetracycline, rolitetracycline, oxitetracycline, minocycline, doxycycline, democlocycline, methacycline; and three tetracycline epimers: epitetracycline, epianhydrotetracycline, and anhydrotetracycline. The HPLC system employs an octadecylsilane reverse phase column and an isopropanol-diethanolamine-phosphate-ammonium EDTA-water mobile phase. This system produced at least partial resolution of all eight parent compounds and many of their degradation products.

Chlortetracycline

Sensitive and specific gas-liquid chromatographic-spectrophotometric screening procedure for trace levels of five sulfonamides in liver, kidney, and muscle tissue.

Free and conjugated sulfonamides are extracted from edible animal tissue with acetone. Carbohydrate is precipitated and removed, and the acetone is evaporated. The residue is transferred to a separatory funnel with ethyl ether and 1N HCl. The acid layer is drawn off and a portion of the 1N HCl is screened, using the Bratton-Marshall reaction. If this portion is positive, the remaining portion is buffered to pH 6.5 and extracted with methylene chloride. The residue is methylated with diazomethane and then acylated with pentafluoropropionic anhydride. The resulting derivatives are detected by gas-liquid chromatography, using electron capture (63Ni) detection and a column packed with 3% OV-17 on Gas-Chrom Q. This method has been validated by recovering sulfathiazole, sulfachloropyrazine, sulfamethazine, sulfadimethoxine, and sulfabromomethazine from liver, kidney, and muscle at levels of 0.1, 0.5, and 1.0 ppm. The 5 sulfonamides were recovered in excess of 60%, with an average mean recovery of 81.5% at the 0.1 ppm level, 79.1% at the 0.5 ppm level, and 76.0% at the 1.0 ppm level.

Animals

Isolation of 2,6-dibromophenol from the marine hemichordate, Balanoglossus biminiensis.

2,6-Dibromophenol has been isolated from a luminous marine enteropneust, Balanoglossus biminiensis, found on intertidal beach areas at Sapelo Island, Georgia. This compound, responsible for the characteristic "iodoform-like" odor of these animals, is present in relatively large amounts; the estimated quantity per organism is 10 to 15 milligrams. Identity of the isolated substance as 2,6 dibromophenol is based on analyses of ultraviolet, infrared, and nuclear magnetic resonance spectra, mass spectrometry analysis, and on melting-point data.

Animals

Validation study of gas chromatographic determination of pentachlorophenol in animal liver.

A validation study was conducted of a gas chromatographic procedure for the determination of pentachlorophenol (PCP) in chicken, pork, and beef liver. Five analysts representing 5 laboratories analyzed randomly numbered blind duplicates at 3 fortified tissue concentrations and one incurred tissue on 2 consecutive days. The PCP concentrations ranged from approximately 40 to 400 parts per billion (ppb). All data were reported to 3 significant figures in ppb. The coefficients of variation for repeatability were between 2.8 and 8.5%, except for the beef liver, at a mean value of 80 ppb PCP, where the CV was 11.3%. The CVs for reproducibility were in the range of 9.7-16.5% with little significant difference by species. The CV asymptotically approached 10% as the PCP level increased.

Animals

Amino acid analysis for meat protein evaluation.

The Food Safety and Inspection Service procedure for determination of essential amino acid content of mechanically processed products from red meat animals and poultry is based on hydrolysis of a powder prepared by blending samples in acetone-chloroform. The hydrolysis procedure incorporates thioglycolic acid to prevent loss of tryptophan. Aliquots of prepared hydrolysates are injected into a liquid chromatographic system, using gradient elution on an ion-exchange column for separation. The system also uses post-column hypochlorite oxidation coupled with orthophthalaldehyde reagent and fluorescence detection. Modification of the elution program allows concurrent determination of tryptophan with minimal added cost. Chromatograms from beef, pork, and poultry products show adequate separation and quantitation of beta-alanine, 1-methyl-histidine, and 3-methyl-histidine, indicating that the procedure could be used to estimate muscle content of products. A colorimetric procedure for assay of hydroxyproline was introduced and validated as an adjunct method for protein quality estimation.

Amino Acids

Ion-exchange separation of amino acids with postcolumn orthophthalaldehyde detection.

Moore's and Stein's classical ion-exchange separation of amino acids remains the standard by which all methods are judged. The adaptation of liquid chromatography (LC) equipment to amino acid analysis was inevitable because microprocessor control of gradients allowed almost infinite variation in gradient shape, producing superior resolution with only 2 buffers. The versatility of LC equipment allowed the instruments to be used for other assays. Adaptation of orthophthalaldehyde (OPA) to amino acid analysis increased detection sensitivity to the picomole range. A method for essential amino acids analysis in mechanically separated red meat and poultry products has been adapted to liquid chromatography using postcolumn hypochlorite oxidation, OPA derivatization, and fluorescence detection. Separation is achieved with 2 sequential concave exponential gradients combining ionic strength and pH increases with halide-containing buffers. Hydroxyproline and proline are detected with increasing sensitivity through the use of 3-mercaptopropionic acid in a stabilized OPA reagent. Sample preparation is a critical part of the method. A defatting procedure removes fat and other nonprotein nitrogenous substances. The hydrolysis procedure is designed to protect tryptophan which can be routinely assayed in hydrolysates with a modified flow program. Corrosion damage to the equipment by halide buffers has brought about a search for alternative methodology.

Amino Acids

Liquid chromatographic assay of tetracyclines in tissues of food-producing animals.

A survey of the literature is presented on liquid chromatographic (LC) determination of tetracyclines in plasma, urine, and tissues of food-producing animals. Food Safety and Inspection Service (FSIS) research on tetracyclines during 1973-1984 is discussed, including the thin layer chromatographic qualitative identification method for tissues. Research on development of LC column packings for trace level chromatography of tetracyclines and anhydrotetracyclines is also discussed. Data are shown for recovery, ruggedness testing, and analyst qualification studies on the tentative version of the LC method.

Animals

Four-laboratory validation study of the determination of chloramphenicol in veal calf urine.

A four-laboratory validation study of a method for the quantitation and confirmation of low part-per-billion levels of chloramphenicol extracted from veal calf urine was done. With this method, chloramphenicol, derivatized to the bis(trimethylsilyl)ether, was quantitated by gas chromatography with electron capture detection (GC-ECD) and confirmed by selected-ion monitoring in a negative ion chemical ionization gas chromatograph-mass spectrometer (GC-NICI-MS). Four analysts from 4 laboratories participated in the portion of the study devoted to chloramphenicol quantitation. Every analyst analyzed 5 sets, one set per day, on 5 different days. Each set included 6 samples consisting of a blank, 2 fortified samples, 2 incurred urine samples, and one duplicate. Thus, each analyst worked on a total of 30 samples. Chloramphenicol concentrations ranged from 0 to 9.7 ppb. All data were reported to 0.1 ppb. Coefficients of variation for distribution, CVd, ranged from 8.82 to 14.14% and for precision, CVr, ranged from 9.15 to 14.80%. Three analysts from 3 laboratories also participated in the confirmatory portion of the study, which was carried out to test whether the NICI-MS method developed earlier for higher concentrations of chloramphenicol and for an extract of muscle tissue could be applied to lower levels of chloramphenicol and to an extract prepared from urine. The extracts of 10 of the 30 samples were designated for confirmation only, but were obtained by the same procedure as extracts used for the quantitation part of the study.(ABSTRACT TRUNCATED AT 250 WORDS)

Animals