scholarly journals Determination of Halofuginone and Amprolium in Chicken Muscle and Egg by Liquid Chromatography

2001 ◽  
Vol 84 (1) ◽  
pp. 43-46 ◽  
Author(s):  
Yuzo Yamamoto ◽  
Fusao Kondo
Keyword(s):  
Lower Limit ◽  
Solid Phase ◽  
Lauryl Sulfate ◽  
Ultraviolet Detection ◽  
Chicken Egg ◽  
Chicken Muscle ◽  
Limit Of Determination ◽  
Cleanup Procedure ◽  
Liquid Chromatographic

Abstract A liquid chromatographic (LC) method was developed for simultaneous measurement of halofuginone (HFN) and amprolium (APL) in chicken muscle and egg. HFN and APL were extracted from chicken muscle and egg with acetonitrile. In chicken egg, they were partially purified by solid-phase extraction (SPE) to separate them from impurities. The LC separation was performed on a 4.6 mm id × 250 mm TSK-gel ODS-80TM column using acetonitrile–McIlvaine buffer, pH 3.4, containing 0.01M sodium lauryl sulfate (42 + 58) as the mobile phase. Ultraviolet detection of HFN and APL was performed at wavelengths of 242 and 265 nm, respectively. Recoveries of HFN and APL from chicken muscle spiked at 0.5 μg/g were 74.8 ± 17.7 and 94.2 ± 5.0%, respectively (mean ± standard deviation [SD], n = 10). In chicken muscle, the lower limit of determination for both APL and HFN was 0.03 μg/g. Recoveries of HFN and APL from chicken egg spiked at 0.5 μg/g by a cleanup procedure using SPE were 54.6 ± 3.4 and 85.0 ± 2.4%, respectively (mean ± SD, n = 5). In chicken egg, the lower limit of determination for both APL and HFN was 0.04 μg/g.

scholarly journals Application of a Mixed-Mode Solid-Phase Extraction and Cleanup Procedure for LC/MS Determination of Thiabendazole and Carbendazim in Apple Juice

2001 ◽  
Vol 84 (5) ◽  
pp. 1608-1614 ◽  
Author(s):  
Michael S Young ◽  
Michael F Early ◽  
Claude R Mallet ◽  
Jim Krol
Keyword(s):  
Solid Phase Extraction ◽  
Mixed Mode ◽  
Apple Juice ◽  
Solid Phase ◽  
Ionization Mass ◽  
Phase Extraction ◽  
Cleanup Procedure ◽  
Sample Preparation Procedure ◽  
Liquid Chromatographic

Abstract Recently, a mixed-mode solid-phase extraction (SPE) procedure was developed for rapid extraction and cleanup for determination of the fungicides thiabendazole and carbendazim in various fruit juices. This paper reports the application of that sample preparation procedure to the liquid chromatographic/mass spectrometric determination of these fungicides in apple juice with detection by positive electrospray ionization mass spectrometry (ESI/MS). Response was linear for sample concentrations from 2 to 500 μg/L (ppb). Recoveries averaged 74% (9% RSD) for carbendazim and 93% (9% RSD) for thiabendazole. After SPE cleanup, no matrix supression was observed for the ESI+ response for either compound studied. The method was applied to the analysis of incurred residues in 4 store-bought apple juices; carbendazim levels ranged from 10 to 70 μg/L and thiabendazole levels ranged from less than 2 to 130 μg/L.

scholarly journals Determination of Nonylphenol and Octylphenol Ethoxylates in Effluent by Liquid Chromatography with Fluorescence Detection

1997 ◽  
Vol 80 (2) ◽  
pp. 401-407 ◽  
Author(s):  
Lindsey G Mackay ◽  
Marguerite Y Croft ◽  
David S Selby ◽  
Robert J Wells
Keyword(s):  
Fluorescence Detection ◽  
Nonionic Surfactants ◽  
Solid Phase ◽  
Graphitized Carbon Black ◽  
Phase Extraction ◽  
Matrix Interferences ◽  
Graphitized Carbon ◽  
Cleanup Procedure ◽  
Liquid Chromatographic

Abstract A robust liquid chromatographic (LC) method with fluorescence detection is described for the simultaneous determination of the nonionic surfactants nonylphenol ethoxylates (NPEO) and octylphenol ethoxylates (OPEO) in effluent samples from sewerage treatment plants. The cleanup procedure uses graphitized carbon black solid-phase extraction cartridges. A subsequent derivatization step removes matrix interferences that are no longer fluorescent after acetylation. The efficiency of the method is monitored by inclusion of a surrogate compound designed and synthesized specifically for this purpose. The limit of reporting for the method is 5 μg/L for 100 mL effluent samples. Studies on confirmation of identity of NPEO and OPEO by electrospray LC/mass spectrometry are described.

Rapid Cleanup Procedure for Gas-Liquid Chromatographic Determination of Chlorpyrifos-Methyl Residues in Cat Food

1981 ◽  
Vol 64 (5) ◽  
pp. 1227-1231
Author(s):  
Richard A Simonaitis ◽  
R Spencer Cail ◽  
James M Zehner
Keyword(s):  
Chromatographic Determination ◽  
Flame Photometric Detector ◽  
Integration Limit ◽  
Photometric Detector ◽  
Limit Of Determination ◽  
Cleanup Procedure ◽  
Liquid Chromatographic Determination ◽  
Electronic Integration ◽  
Liquid Chromatographic

Abstract A simple and rapid gas-liquid chromatographic (GLC) method was developed for the determination of residues of chlorpyrifos-methyl in dry cat food. Cat food fortified with chlorpyrifos-methyl was extracted with acetone and cleaned up on a modified acetonitrile-on-Florisil partitioning column. The chlorpyrifos-methyl was determined by GLC with a flame photometric detector. Results were compared with those for known standards that had undergone the same cleanup procedure. The quantitative electronic integration limit of determination was 0.03 ppm. Average recoveries for 5 analyses at fortification levels from 0.052 to 51 ppm ranged from 90 to 102% and averaged 97%.

Matrix Solid-Phase Dispersion Extraction and Liquid Chromatographic Determination of Nicarbazin in Chicken Tissue

1992 ◽  
Vol 75 (4) ◽  
pp. 659-662 ◽  
Author(s):  
Frank J Schenck ◽  
Steven A Barker ◽  
Austin R Long
Keyword(s):  
Solid Phase ◽  
Chromatographic Determination ◽  
Reversed Phase ◽  
Chicken Liver ◽  
Tissue Samples ◽  
Chicken Tissue ◽  
Cleanup Procedure ◽  
Tissue Matrix ◽  
Liquid Chromatographic

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.

scholarly journals Determination of Tetracycline Antibiotics in Salmon Muscle by Liquid Chromatography Using Post-Column Derivatization with Fluorescence Detection

2003 ◽  
Vol 86 (5) ◽  
pp. 925-929 ◽  
Author(s):  
Angelina L Pena ◽  
Celeste M Lino ◽  
M Irene N Silveira
Keyword(s):  
Fluorescence Detection ◽  
Solid Phase ◽  
Polymeric Sorbent ◽  
Tetracycline Antibiotics ◽  
Liquid Chromatographic Method ◽  
Limit Of Quantitation ◽  
Ethylenediaminetetracetic Acid ◽  
Cleanup Procedure ◽  
Liquid Chromatographic

Abstract A simple and accurate cleanup procedure using polymeric sorbent was developed for the determination of oxytetracycline (OTC) and tetracycline (TC) residues in salmon muscle. It was applied to the analysis of 20 salmon samples during a month period. The OTC and TC residues were extracted with ethylenediaminetetracetic acid (EDTA)–McIlvaine buffer acidified at pH 4.0 and cleaned up by solid-phase extraction with a polymeric sorbent. The advantages of the polymeric sorbent over the silica-based sorbent in the cleanup of salmon muscle samples are described. A liquid chromatographic method with post-column derivatization and fluorescence detection is proposed because of its sensitivity and specificity. The average recoveries of OTC and TC from muscle salmon tissue fortified at 50, 100, and 200 μg/kg levels, ranged from 83.9 to 93.4% with a coefficient of variation between 4.09 and 5.80%. The limit of quantitation for OTC and TC in salmon muscle was 50 μg/kg.

Liquid Chromatographic Determination of Abamectin in Fruits and Vegetables

1993 ◽  
Vol 76 (3) ◽  
pp. 691-694 ◽  
Author(s):  
Narong Chamkasem ◽  
Michael L Papathakis ◽  
S Mark Lee
Keyword(s):  
Fruits And Vegetables ◽  
Solid Phase ◽  
Ammonium Hydroxide ◽  
Chromatographic Determination ◽  
Phase Extraction ◽  
Fluorescence Detector ◽  
Cleanup Procedure ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract A simplified extraction and cleanup procedure was developed for determining abamectin in fruits and vegetables. Abamectin is extracted from sample matrices by acetonitrile, and the acetonitrile phase is separated from the aqueous phase by saturating the extract with sodium chloride. Abamectin is then partitioned into hexane from the acetonitrile, and the hexane layer is cleaned up with an aminopropyl solid-phase extraction (SPE) system. The fluorescent abamectin derivative is formed by dehydration with trifluoroacetic anhydride-1-methylimidazole in dimethylformamide for 1 h at 30°C and with methanolic ammonium hydroxide for another 30 min at 30°C. The derivatized residues are separated from the reaction mixture by a silica SPE. The abamectin derivative is determined by reversedphase liquid chromatography with a fluorescence detector. The method yields recoveries of 85-97% at fortification levels of 10 and 50 μg/kg for orange, pears, spinach, and celery.

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