Trace analysis of endectocides in milk by high performance liquid chromatography with fluorescence detection
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- 作者：Vesna Cerkvenik-Flajs ; Luka Milč ; inski ; Adica Sü ; ssinger ; Lena Hodoš ; č ; ek ; Martin Danaher ; Jan Antonić
- 关键词：Endectocides ; Avermectins ; Milk ; Analysis ; HPLC-fluorescence
- 刊名：Analytica Chimica Acta
- 出版年：2010
- 出版时间：24 March 2010
- 年：2010
- 卷：663
- 期：2
- 页码：165-171
- 全文大小：559 K
文摘
An analytical method has been developed for the simultaneous determination of the following endectocide drugs in milk: ivermectin, abamectin, doramectin, moxidectin, eprinomectin, emamectin and nemadectin. Samples were extracted with acetonitrile, purified with solid-phase extraction on a reversed phase C8, derivatised with N-methylimidazole, trifluoroacetic anhydride and acetic acid to a stable fluorescent derivative, and were further analysed by gradient high performance liquid chromatography (HPLC) on an endcapped reversed phase Supelcosil LC-8-DB. The derivatisation step was mathematically optimised and the method was validated according to the requirements of Commission Decision 2002/657/EC, using fortified raw bovine milk. Mean recovery was between 78 and 98 % . The repeatability (CVr) and within-laboratory reproducibility (CVW) ranged from 4.6 to 13.4 % and from 6.6 to 14.5 % , respectively. Decision limits (CCα) for analytes with MRL values, namely eprinomectin and moxidectin, were determined to be 24.8 and 50.6 μg kg−1, respectively. CCα values for unauthorised endectocides ranged from 0.1 to 0.2 μg kg−1. Due to high acceptability regarding the required criteria and applicability to ovine and caprine milk, giving similar results, this multi-analyte method has been successfully implemented in pharmacokinetic research studies as well as statutory residue monitoring in Slovenia.