Matrix Solid Phase Dispersion Isolation and Liquid Chromatographic Determination of Five Benzimidazole Anthelmintics in Fortified Beef Liver

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%.

1993 ◽  
Vol 76 (3) ◽  
pp. 531-534 ◽  
Author(s):  
Robert P Snell

Abstract A liquid chromatographic procedure is described for the determination of phthalide, monobutyl phthalate, and mono-2-ethylhexyl phthalate leached by water from solution administration sets. Recoveries varied from 88.8% for phthalide at 1 (μg/50 mL to 113% for monobutyl phthalate at 6 μg/50 mL. Relative standard deviations at 1 μg/50 mL were 2.59% for phthalide, 3.54% for monobutyl phthalate, and 11.6% for mono-2- ethylhexyl phthalate. At 6 μg/50 mL, the relative standard deviation for mono-2-ethylhexyl phthalate decreased to 3.88%. Reproducibilities for 5 standard injections were 1.40% for phthalide, 1.84% for monobutyl phthalate, and 1.95% for mono-2- ethylhexyl phthalate. Correlation coefficients were 1.00 for the 3 compounds. Five sets from 2 manufacturers were examined. No phthalide or monobutyl phthalate was found. One manufacturer’s sets contained 37.6-44.4 μg/L mono-2- ethylhexyl phthalate. The sample matrix had some interference if phthalide or monobutyl phthalate was present.


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%.


1989 ◽  
Vol 72 (5) ◽  
pp. 739-741 ◽  
Author(s):  
Austin R Long ◽  
Lily C Hsieh ◽  
Marsha S Malbrough ◽  
Charles R Short ◽  
Steven A Barker

Abstract A multiresidue method for the isolation and liquid chromatographic determination of 7 benzimidazole anthelmintics (thiabendazole, oxfendazole, para-hydroxyfenbendazole, fenbendazole sulfone, mebendazole, albendazole, and fenbendazole) in milk is presented. Blank or benzimidazole-spiked milk samples (0.5 mL) were blended with octadecylsilyl (C-18, 18% load, end-capped) derivatized silica packing material. A column made from the C-18/milk matrix was first washed with hexane (8 mL), and then the benzimidazoles were eluted with methylene chloride-ethyl acetate (1 + 2, v/v; 8 mL). The eluate contained benzimidazole analytes which were free from interfering compounds as determined by UV detection (photodiode array, 290 nm). Correlation coefficients of standard curves for individual benzimidazoles isolated from spiked samples were linear (0.989 ± 0.003 to 0.998 ± 0.001) with recoveries ranging from 70 ± 9% to 107 ± 2% for the concentration range (62.5-2000 ng/mL) examined. The inter- assay variabilities ranged from 4 ± 1% to 9 ± 7% with intra-assay variabilities of 3-6%.


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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