Matrix Solid Phase Dispersion (MSPD) Isolation and Liquid Chromatographic Determination of Furazolidone in Pork Muscle Tissue

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%.

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%.


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%.


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.


1992 ◽  
Vol 75 (4) ◽  
pp. 659-662 ◽  
Author(s):  
Frank J Schenck ◽  
Steven A Barker ◽  
Austin R Long

Abstract This method outlines the necessary steps for the isolation and determination of the drug nicarbazin in chicken liver and muscle tissue. Tissue samples were blended with octadecylsilyl-derivatized silica packing material (C18). A column made from the C18-tissue matrix is first washed with hexane, and then the 4,4-dinitrocarbanilide (DNC) portion of the nicarbazin complex is eluted with acetonitrile. After further cleanup using alumina cartridge chromatography, DNC is determined by reversed-phase liquid chromatography with UV detection at 340 nm. Recoveries based on DNC were 95.8 and 83.7% from liver and muscle tissues, respectively. This method and a classical ethyl acetate extraction method gave comparable results on 4 chicken liver and 3 muscle samples that contained incurred nicarbazin residues. C18 sorbents from different manufacturers as well as lipophilic sorbents other than ds were also studied. The proposed extraction and cleanup procedure requires less than 30 mL solvent, fewer sample manipulations, and does not require solvent partitioning or backwashing of extracts. This combination of characteristics makes this method more attractive than classical isolation procedures for nicarbazin.


1990 ◽  
Vol 73 (6) ◽  
pp. 860-863 ◽  
Author(s):  
Austin R Long ◽  
Marsha S Malbrough ◽  
Lily C Hsieh ◽  
Charles R Short ◽  
Steven A Barker

Abstract A multlresidue method for Isolation and liquid chromatographic determination of 5 benzimidazole anthelmintics (thiabendazole, oxfendazole, mebendazole, albendazole, and fenbendazole) in beef liver tissue is presented. Blank or benzlmldazole-fortlfled liver samples (0.5 g) were blended with octadecylsilyl derlvatlzed silica packing material (C18, 18% load, endcapped, 2 g). A column made from the C18/ liver matrix was first washed with hexane (8 ml_), following which the benzlmldazoles were eluted with acetonltrile. The acetonltrlle extract was then passed through an activated alumina column. The eluate contained benzimidazole analytes that were free from Interfering compounds as determined by UV detection (photodlode array, 290 nm). Correlation coefficients of standard curves for Individual benzlmldazoles Isolated from fortified samples, using internal standardization, were linear (0.996 ± 0.002 to 0.999 ± 0.001) with average relative percentage recoveries from 62.0 ± 6.7 to 86.8 ± 8.6% for the concentration range (100- 3200 ng/g) examined. The interassay variability was 7.0 ± 4.1 to 12.9 ± 10.2% with an Intra-assay variability from 2.2 to 4.0%.


1990 ◽  
Vol 73 (3) ◽  
pp. 379-384 ◽  
Author(s):  
Austin R Long ◽  
Lily C Hsieh ◽  
Marsha S Malbrouh ◽  
Charles R Short ◽  
Steven A Barker

Abstract A multlresldue method for the isolation and liquid chromatographic determination of oxytetracycline (OTC), tetracycline (TC), and chlortetracycllne (CTC) antibiotics In milk Is presented. Blank and tetracycline (OTC, TC, and CTC) fortified milk samples (0.5 mL) were blended with octadecylsllyl (C18, 40 /an, 18% load, endcapped, 2 g) derivatized silica packing material containing 0.05 g each of oxalic acid and dlsodlum ethylenedlamlnetetraacetlc. A column made from the C18/milk matrix was first washed with hexane (8 mL), following which the tetracyclines were eluted with ethyl acetate-acetonltrlle (1 + 3; v/v). The eluate contained tetracycline analytes that were free from Interfering compounds when analyzed by liquid chromatography with UV detection (photodiode array, 365 nm). Correlation coefficients of standards curves for Individual tetracycline isolated from fortified samples were linear (from 0.982 ± 0.009 to 0.996 ± 0.004) with average percentage recoveries from 63.5 to 93.3 for the concentration range (100,200,400,800,1600, and 3200 ng/ mL) examined. The Inter-assay variability ranged from 8.5 ± 2.4% to 20.7 ± 13.0% with an Intra-assay variability of 1.0- 9.3%.


1984 ◽  
Vol 67 (5) ◽  
pp. 861-862 ◽  
Author(s):  
John Morawski ◽  
Glenn Kyle

Abstract A rapid, reliable separation and quantitation of zoalene (3,5-dinitroo-toluamide) from feeds is accomplished by using reverse phase liquid chromatography (LC) and ultraviolet detection. An extraction technique which is similar to the present AOAC official colorimetric method is used before chromatographic analysis. This extraction is followed by an activated alumina cleanup and LC to separate zoalene from feed matrix. The methodology was applied to a variety of spiked feed matrices, and yielded good recoveries. Liquid chromatographic results were shown to correlate with colorimetric determinations.


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