Determination of Sulfadimethoxine and Ormetoprim Residues in Channel Catfish Fillets After Treatment with Romet and Evaluation of a Commercially Available Rapid Diagnostic Test for Drug Residues in Fish Fillets

1994 ◽  
Vol 77 (4) ◽  
pp. 875-881 ◽  
Author(s):  
Nicholas P Milner ◽  
Michael R Johnson ◽  
Kim J Perry

Abstract Sulfadimethoxine (SDM) and ormetoprim (OMP) residues were determined in catfish fillets after treatment with Romet. A liquid chromatographic (LC) method capable of simultaneously detecting SDM and OMP at 0.05–40 ppm was used. The recoveries were 92% for SDM and 108% for OMP. The intra- assay variabilities were determined for SDM and OMP at fortification levels of 0.05–40 ppm, and a coefficient of variation (CV) of less than 10% was achieved at all levels. The interassay variations were determined at fortification levels of 0.1 ppm (CVs: SDM, 6.4%; OMP, 4.9%) and 1.0 ppm (CVs: SDM, 2.8%; OMP, 3.5%). SDM and OMP residues in catfish fillets were rapidly depleted after treatment with Romet. By day 2 posttreatment, SDM and OMP were essentially nondetectable. The use of an enzyme-linked immunoassay (ELISA)-based rapid diagnostic test to determine SDM and OMP in catfish fillets was evaluated. An assay procedure to adapt the test for residues in tissue samples was developed. SDM and OMP were extracted from ground catfish fillet with methanol–water (80 + 20, v/v); the extract was diluted with buffer and filtered, and the filtrate was then tested with an EZ Screen test card. The effectiveness of the rapid test assay to detect SDM residues at levels above the U.S. Food and Drug Administration tolerance (0.1 ppm) was verified with fillets from Romet-treated catfish. All samples with residues at >0.1 ppm were identified correctly by the test. The results indicate that the diagnostic test could be used as a rapid method for monitoring Romet residues in catfish.

1980 ◽  
Vol 63 (1) ◽  
pp. 49-55
Author(s):  
Iwao Okuno ◽  
Dennis L Meeker

Abstract An analytical method is described for the determination of Compound 1080 (sodium fluoroacetate) residues in 1–10 g tissue. Sample extracts of tissues are cleaned up with silica gel, and Compound 1080 (as fluoroacetic acid) is separated by a micro-distillation procedure. The fluoroacetic acid in the distillate is derivatized with pentafluorobenzyl bromide to form pentafluorobenzyl fluoroacetate which is measured by electron capture gas-liquid chromatography. Recoveries of sodium fluoroacetate from fortified tissue samples averaged about 25%. Despite the limited recoveries, results were quite reproducible, and levels as low at 2 ppm were determined in fortified 1 g samples, and 0.2 ppm in 10 g samples. The method is relatively simple and has been used routinely in our laboratory for the analysis of various types of samples such as grain, and tissues from birds, rodents, and larger animals.


1988 ◽  
Vol 71 (2) ◽  
pp. 290-294
Author(s):  
Ramesh J Trivedi

Abstract A sensitive, specific liquid chromatographic (LC) procedure was developed for determination of allantoin [(2,5-dioxo-4--imidaazolidinyl) urea or 5-ureidohydantion] in cosmetic lotion. A reverse-phase, ionsuppression mechanism separated allantoin from interfering constituents of the sample matrix, and the compound was determined with a UV detector at 240 nm with a sensitivity limit of ((.20 mg/mL. The chromatographic parameters were optimized for retention time, efficiency, and relative response to the analyte. The assay procedure was validated with spiked laboratory-prepared samples at 100 ± 15% levels. An average recovery of 99.4% with a relative standard deviation of 1.5% (n = 7) was obtained. The stability-indicating characteristics of the method were established by recovery study (99.8%) of samples spiked with known degradation products (urea, allantoic acid, and glyoxylic acid).


1982 ◽  
Vol 65 (3) ◽  
pp. 753-756
Author(s):  
Walter F Schmidt

Abstract A high performance liquid chromatographic procedure has been developed for the assay of phenprocoumon in tablets. In comparison to the present official USP assay procedure, it is equivalent in precision and accuracy and is faster and more specific. A mobile phase consisting of a 1% solution of acetic acid in acetonitrile-water (4 + 3) separates phenprocoumon from warfarin internal standard on a 6 μm octadecylsilane (ODS) column with UV detection at 311 nm. The method enables the concurrent determination of phenprocoumon and possible contaminants such as salicylic acid.


1976 ◽  
Vol 59 (5) ◽  
pp. 1094-1096
Author(s):  
Vincent B Stein ◽  
Kenneth A Pittman

Abstract A new method for the determination of azinphos ethyl (O,O-diethyl-S-(4-oxo-1,2,3-benzotriazin-3(4H)-ylmethyl) phosphorodithioate) in human plasma and in mouse plasma, tissue, and fat has been developed. The method is based on extraction with benzene or hexane and cleanup of fat and tissue samples by a minicolumn containing Florisil and sodium sulfate. Azinphos ethyl is eluted from the column with 10% acetonitrile in benzene and is concentrated to an appropriate volume for gas-liquid chromatographic analysis, using a 63Ni electron capture detector and a glass column containing 3% OV-1 on Gas-Chrom Q. The method is sensitive to 0.005 ppm in human plasma, 0.01 ppm in mouse plasma, 0.08 ppm in mouse liver, 0.05 ppm in mouse brain, and 0.10 ppm in mouse fat. The limit of detection is 2 pg; mean recoveries ranged from 96 to 98%.


1980 ◽  
Vol 63 (5) ◽  
pp. 988-991
Author(s):  
Graeme L Blackman ◽  
Ah Chai Ho ◽  
Alex Jozsa ◽  
John D Kelly

Abstract A high performance liquid chromatographic (HPLC) technique is described for the determination of residue levels of the anthelmintic drug phenothiazine in sheep tissues. Phenothiazine was administered to sheep which were slaughtered after withholding periods of 24, 48, and 72 h. Residues of phenothiazine were then extracted from tissue samples by homogenization in methanol. The HPLC analysis of the extracts involved separation on a 10 μm silica column using a mobile phase of 0.3% n-propanol in cyclohexane. The lower limit of detection by ultraviolet absorption at 254 nm was 0.05 ppm


Author(s):  
Lucia Campos Pellanda ◽  
Eliana Márcia da Ros Wendland ◽  
Alan John Alexander McBride ◽  
Luciana Tovo-Rodrigues ◽  
Marcos Roberto Alves Ferreira ◽  
...  

AbstractBackgroundWhile the recommended laboratory diagnosis of COVID-19 is a molecular based assay, population-based studies to determine the prevalence of COVID-19 usually use serological assays.ObjectiveTo evaluate the sensitivity and specificity of a rapid diagnostic test for COVID-19 compared to quantitative reverse transcription polymerase chain reaction (qRT-PCR).MethodsWe evaluated the sensitivity using a panel of finger prick blood samples from participants >18 years of age that had been tested for COVID-19 by qRT-PCR. For assessing specificity, we used serum samples from the 1982 Pelotas (Brazil) Birth Cohort participants collected in 2012 with no exposure to SARS-CoV-2.ResultsThe sensitivity of the test was 77.1% (95% CI 66.6 - 85.6), based upon 83 subjects who had tested positive for qRT-PCR at least 10 days before the rapid diagnostic test (RDT). Based upon 100 sera samples, specificity was 98.0% (95% CI 92.9 - 99.8). There was substantial agreement (Kappa score 0.76) between the qRT-PCR results and the RDT.InterpretationThe validation results are well in line with previous assessments of the test, and confirm that it is sufficiently precise for epidemiological studies aimed at monitoring levels and trends of the COVID-19 pandemic.


1990 ◽  
Vol 73 (6) ◽  
pp. 868-871 ◽  
Author(s):  
Austin R Long ◽  
Lily C Hsieh ◽  
Marsha S Malbrou ◽  
Charles R Short ◽  
Steven A Barker

Abstract A method for the isolation and liquid chromatographic determination of sulfadimethoxine In catfish (Ictalurus punctatus) muscle tissue Is presented. Blank control and sulf adlmethox- Ine-fortlfled fish muscle tissue samples (0.5 g) were blended with octadecylsllyl (C18,40 /μm, 18% load, endcapped) derivatlzed silica packing material. A column made from the C18/ fish tissue blend was first washed with hexane (8 mL), following which the sulfadimethoxine was eluted with dlchloromethane (8 mL). The eluant contained sulfadimethoxine analyte that was free from Interfering compounds when analyzed by liquid chromatography with UV detection (photodlode array, 270 nm). Standard curves for sulfadimethoxine Isolated from fortified samples were linear (0.999 ± 0.001) with an average relative percentage recovery of 101.1 ± 4.2% for the concentration range (50, 100, 200,400, 800, and 1600 ng/g) examined using sulfamethoxazole as the Internal standard. The interassay variability was 10.7 ± 8.2% with an Intra-assay variability of 2.2%.


1978 ◽  
Vol 61 (1) ◽  
pp. 08-14 ◽  
Author(s):  
Charles J Stafford ◽  
William L Reichel ◽  
Douglas M Swineford ◽  
Richard M Prouty ◽  
Martha L Gay

Abstract A procedure is described for determining Kepone (decachlorooctahydro-l,3,4-metheno-2H-cyclobuta [cd]pentalene-2-one) residues in avian egg, liver, and tissue. Samples were extracted with benzene-isopropanol, and the extract was cleaned up with fuming H2SO4-concentrated H2SO4. Kepone was separated from organochlorine pesticides and polychlorinated biphenyls on a Florisil column and analyzed by electron capture gas-liquid chromatography GLC). The average recovery from spiked tissues was 86%. The analyses performed on 14 bald eagle carcasses and livers, 3 bald eagle eggs, and 14 osprey eggs show measurable levels which indicate that Kepone accumulates in the tissues of fish-eating birds. Residues were confirmed by GLC-mass spectrometry.


1990 ◽  
Vol 73 (6) ◽  
pp. 864-867 ◽  
Author(s):  
Austin R Long ◽  
Lily C Hsiesh ◽  
Marsha S Malbrough ◽  
Charles R Short ◽  
Steven A Barker

Abstract A method for Isolation and liquid chromatographic determination of oxytetracycllne In catfish (Ictalurus punctatus) muscle tissue Is presented. Blank control and oxytetracycllne- fortlfied fish muscle tissue samples (0.5 g) were blended with octadecylsilyl (C18, 40 μm, 18% load, endcapped) derlvatized silica packing material (2 g) containing 0.05 g each of oxalic acid and disodlum ethylenedlamlnetetraacetate. A column made from the C18/fish tissue matrix was first washed with hexane (8 mL), following which the oxytetracycllne was eluted with acetonltrile-methanol (1 + 1, v/v) containing 0.06% w/v each of butylated hydroxyanlsole and butylated hydroxytoluene. The eluate contained oxytetracycllne analyte that was free from Interfering compounds when analyzed by liquid chromatography with UV detection (photodlode array set at 365 nm). Standard curves for oxytetracycllne Isolated from fortified samples were linear (0.998 ± 0.002) with an average absolute percentage recovery of 80.9 ± 6.6% for the concentration range (50,100,200, 400, 800, 1600, and 3200 ng/g) examined. The Interassay variability was 11.3 ± 5.2% with an Intra-assay variability of 1.1%.


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