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

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.

1986 ◽  
Vol 69 (4) ◽  
pp. 697-699
Author(s):  
George M Ware ◽  
Allen S Carman ◽  
Octave J Francis ◽  
Shia S Kuan

Abstract A method is described for the determination of individual ergot alkaloids in wheat. The sample is extracted with ethyl acetate-4% ammonium hydroxide (100 + 10), and the extract is cleaned up by liquidliquid partition. The ergot alkaloids are resolved by liquid chromatography (LC), using a porous cross-linked polystyrene-divinylbenzene resin column and a mobile phase consisting of acetonitrile-0.05M dibasic ammonium phosphate (55 + 45) buffered at pH 10.0. The ergot alkaloids ergonovine, ergonovinine, ergotamine, ergotaminine, α-ergocryptine, α-ergocryptinine, ergocristine, and ergocristinine are separated by LC and detected with a fluorescence detector. Recovery of ergot alkaloids added to wheat at levels of 16-760 ng/g averaged 85.6% with a coefficient of variation of 11.1%.


1998 ◽  
Vol 81 (4) ◽  
pp. 869-872 ◽  
Author(s):  
Stephen J Doherty ◽  
Allen Fox ◽  
David W Fink

Abstract An analytical method for determining ivermectin in feed at 0.50- 3 ppm is presented. The method is based on liquid chromatographic measurement after sample preparation by adsorption chromatography on alumina and solid-phase extraction. Two complete, final, finished medicated feeds and the corresponding control feeds used in their preparation were analyzed. Recoveries from feeds fortified at 50-150% of the 2 ppm ivermectin use concentration also were determined. Mean recoveries from replicate analyses ranged from 90 to 100%, and coefficients of variation (CVs) were less than 4.5%. No significant interferences were found in control feeds. The pooled distribution of individual analytical results (n = 100) gave a mean recovery of 100%, a recovery range of 90-111%, and an overall CV of 5.5%. Resolution of the total variance into its 2 components gave a withinlaboratory CV of 4.1% and a between-laboratory CV of 3.4%. There was no significant difference in recoveries among laboratories, days, concentrations, and feed base or between fortified and medicated feeds (P > 0.2)


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