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A liquid chromatography (LC)/fluorescence procedure was validated for emamectin (EM B1a) and desmethylamino-emamectin (DMAEM B1a) residues in lobster tissue. They were extracted by shaking and sonicating with 1% ammonium acetatemethanol in the presence of sand. The extract was concentrated, partitioned with ethylacetate, and cleaned up on a propylsulfonic cation exchange cartridge. The analytes were eluted from the cartridge with 5% ammonium hydroxidemethylacetate, the eluate was concentrated, and the solvent was changed to dry 20% ethylacetateacetonitrile before derivatization with trifluoroacetic anhydrideN-methylimidizole. The products were analyzed by LCfluorescence, and no interference [&amp;gt;limit of detection (LOD)] was detected in the control samples. Lobster tissues fortified with EM B1a and DMAEM B1a at 0.5, 5, 10, 25, and 50 ng/g gave overall mean recoveries of 96.7 12.4%, relative standard deviation (RSD) 12.8% for EM B1 and 83.6 12.1%, RSD 14.5% for DMAEM B1a. Regression analysis of the calibration data gave slopes of 0.90 (EM B1a) and 0.71 (DMAEM B1a) with an r2 0.99 for both compounds. The calculated LOD and limit of quantification (LOQ) for EM B1a were 1.10 and 3.32 ng/g, respectively, and for DMAEM B1a were 0.762 and 2.31 ng/g, respectively. Residues of EM B1a and DMAEM B1a in fortified lobster tissues stored at 20C showed that residues were stable for 1012 months. No loss of EM B1a and DMAEM B1a residues was observed after 3 freeze/thaw cycles of fortified tissue in a 5-day period.

Liquid Chromatography/Fluorescence Method for Emamectin B1a and Desmethylamino-Emamectin B1a Residues in Lobster Tissue