Matrix Solid Phase Dispersion Isolation and Liquid Chromatographic Determination of Oxytetracycline in Catfish (Ictalurus punctatus) Muscle Tissue

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%.

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%.


1996 ◽  
Vol 79 (3) ◽  
pp. 645-651 ◽  
Author(s):  
Christiaan A J Hajee ◽  
Nel Haagsma

Abstract An analytical method is presented for liquid chromatographic (LC) determination of mebendazole (MBZ), hydroxymebendazole (MBZ-OH), and aminomebendazole (MBZ-NH2) in eel muscle tissue. Muscle tissue is extracted with ethyl acetate at pH 7.5. After addition of n-hexane, the extract is cleaned up and concentrated on an aminopropyl solid-phase extraction column. The test solutions are analyzed isocratically on a ChromSpher B LC column with acetonitrile–phosphate buffer, pH 6.2, as mobile phase. Limits of detection and quantitation were 0.7 and 1.1 ¼g/kg, respectively, for MBZOH; 1.4 and 2.3 ¼g/kg, respectively, for MBZ; and 1.5 and 2.1 ¼g/kg, respectively, for MBZ-NH2. Interand intraday coefficients of variation were 3.5 and 3.4%, respectively, for MBZ-OH; 2.5 and 3.1%, respectively, for MBZ; and 5.8 and 4.8%, respectively, for MBZ-NH2. Mean recoveries were 90% for MBZ, 74% for MBZ-NH2, and 92% for MBZ-OH. A linear range of applicability of at least 10–1000 ¼g/kg was found for each analyte. Incurred MBZ-NH2 (181.3 ¼g/kg) was identified in eel muscle tissue apart from MBZ (23.7 ¼g/kg) after 48 h exposure ina treatment bath containing MBZ at 1 mg/L.


The Analyst ◽  
1994 ◽  
Vol 119 (12) ◽  
pp. 2749-2751 ◽  
Author(s):  
Vittorio Maria Moretti ◽  
Gian Luca Maggi ◽  
Attilia Albertini ◽  
Federica Bellagamba ◽  
Umberto Luzzana ◽  
...  

1992 ◽  
Vol 75 (3) ◽  
pp. 428-432 ◽  
Author(s):  
Herman H Jarboe ◽  
Kevin M Kleinow

Abstract Matrix solid-phase dispersion Isolation and liquid chromatographic techniques were developed to quantify oxolinic acid (OA) and OA-related metabolites in channel catfish (Ictalurus punctatus) muscle tissue and bile. Mean percent recovery, correlation coefficient, and inter- and intra-assay variabilities were 82.8 ±15.0%, 0.996 ±0.004,12.5 ±8.9%, and 1.22%, respectively, for OA Isolated from fortified muscle tissue. Using the methodologies described in the current study, incurred OA In muscle tissue and 4 OA-related metabolites were Isolated In the bile of dosed catfish.


1991 ◽  
Vol 74 (2) ◽  
pp. 292-294 ◽  
Author(s):  
Austin R Long ◽  
Lily C Hsieh ◽  
Marsha S Malbrough ◽  
Charles R Short ◽  
Steven A Barker

Abstract A method for the Isolation and liquid chromatographic (LC) determination of furazolidone In pork muscle tissue is presented. Blank or furazolldone-forllfled pork muscle tissue samples (0.5 g) were blended with octadecylsllyl (C18,18% load, endcapped, 2 g) derlvatlzed silica. A column made from C18/pork matrix was first washed with hexane (8 mL), followed by elution of furazolidone with ethyl acetate. The ethyl acetate extract was then passed through an activated alumina column. The eluate contained furazolidone that was free from Interfering compounds when analyzed by LC with UV detection (photodlode array, 365 nm). Detector response with Increasing concentrations of furazolidone Isolated from fortified samples was linear (r = 0.998 ± 0.002) with an average percentage recovery of 89.5 ± 8.1% for the concentration range (7.8-250 ng/g) examined and resulted in a minimum detectable limit of 390 pg on column, and a detector response of more than 5 times baseline noise. The interassay variability was 9.9 ± 5.4% with an Intra-assay variability of 1.5%.


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