Group Analytical Chemistry of Contaminants, Department of Analytical Chemistry, Almeria University, E-04071 Almería, Spain.
Anal Chim Acta. 2010 Feb 28;661(2):150-60. doi: 10.1016/j.aca.2009.12.016. Epub 2009 Dec 21.
This study compared four extraction methods for the simultaneous determination of tetracyclines, macrolides, quinolones, sulphonamides and anthelmintics (including benzimidazoles and avermectins) in eggs by ultra-high pressure liquid chromatography coupled to tandem mass spectrometry (UHPLC-MS/MS). Solvent extraction, solid-phase extraction (SPE), matrix solid-phase dispersion (MSPD) and modified QuEChERS procedure were compared in terms of recovery and number of veterinary drugs extracted. The solvent extraction procedure with a clean-up step provided better results than the other tested procedures. The QuEChERS procedure was simpler and faster, but extracted fewer compounds than solvent extraction. MSPD did not extract tetracyclines and quinolones, whereas macrolides and tetracyclines were not extracted when SPE was applied. The solvent extraction procedure was validated, obtaining recoveries ranging from 60% (sulfaquinoxaline) to 119% (levamisole) with repeatability values (expressed as relative standard deviations, RSDs) lower than 20% at two concentration levels (10 and 100 microg kg(-1)), except for erythromycin, emamectin and ivermectin that showed RSD values close to 25% at 10 microg kg(-1). Limits of quantification (LOQs) were always equal or lower than 5 microg kg(-1). Finally the method was applied to egg samples, and erythromycin, enrofloxacin, difloxacin, thiabendazole, emamectin and fenbendazole were detected in four samples.
本研究比较了四种提取方法，用于通过超高效液相色谱串联质谱法（UHPLC-MS/MS）同时测定鸡蛋中的四环素、大环内酯类、喹诺酮类、磺胺类和驱虫药（包括苯并咪唑类和阿维菌素类）。在提取回收率和提取的兽药数量方面，比较了溶剂萃取、固相萃取（SPE）、基质固相分散（MSPD）和改良 QuEChERS 方法。具有净化步骤的溶剂萃取程序比其他测试程序提供了更好的结果。QuEChERS 方法更简单、更快，但提取的化合物少于溶剂萃取。MSPD 未提取四环素和喹诺酮类，而 SPE 应用时未提取大环内酯类和四环素。溶剂萃取程序经过验证，在两个浓度水平（10 和 100μgkg-1）下，回收率范围为 60%（磺胺喹噁啉）至 119%（左旋咪唑），重复性值（表示为相对标准偏差，RSD）低于 20%，除了红霉素、埃玛菌素和伊维菌素，它们在 10μgkg-1 时的 RSD 值接近 25%。定量限（LOQ）始终等于或低于 5μgkg-1。最后，该方法应用于鸡蛋样品中，在四个样品中检测到红霉素、恩诺沙星、二氟沙星、噻苯达唑、埃玛菌素和芬苯达唑。
