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Development and optimisation of an improved derivatisation procedure for the determination of avermectins and milbemycins in bovine liver
Danaher, Martin O’Keeffe, Michael Glennon, Jeremy D. Howells, Laurence
Danaher, Martin
O’Keeffe, Michael
Glennon, Jeremy D.
Howells, Laurence
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2001
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Danaher, M., O’Keeffe, M., Glennon, J. and Howells, L., 2001. Development and optimisation of an improved derivatisation procedure for the determination of avermectins and milbemycins in bovine liver. The Analyst, 126(5), pp.576-580.
Abstract
A robust procedure has been developed to overcome the instability problems experienced with the fluorescent
derivative of eprinomectin. The procedure involves addition of acetic acid, together with the typical reagents
methylimidazole and trifluoroacetic anhydride, to produce a fluorescent molecule that can be determined by high
performance liquid chromatography (HPLC) with fluorescence detection. Derivatisation is completed in 30 min at
65 °C. This derivatisation procedure was shown to be suitable, also, for the related compounds, moxidectin,
abamectin, doramectin and ivermectin. A multi-residue method for these compounds in bovine liver has been
developed using the derivatisation procedure. Samples are extracted with acetonitrile; followed by clean-up on
deactivated alumina and C18 solid phase extraction (SPE) cartridges. The method was validated using bovine liver
fortified at levels of 4 and 20 mg kg21 with the drugs. The mean recovery ranged between 73 and 97%. The intraand inter-assay variations showed relative standard deviations typically of < 6% and < 14%, respectively. The
limit of quantitation of the method is 2 mg kg21
(ppb).