Aguilera-Luiz M M, Vidal Jose Luis Martínez, Romero-González Roberto, Frenich Antonia Garrido
Group "Analytical Chemistry of Contaminants", Department of Analytical Chemistry, Almeria University, E-04071 Almería, Spain.
J Chromatogr A. 2008 Sep 26;1205(1-2):10-6. doi: 10.1016/j.chroma.2008.07.066. Epub 2008 Jul 26.
A simple, selective and fast multi-residue method was developed to determine 18 veterinary drugs in milk by ultra-high-pressure liquid chromatography coupled to tandem quadrupole mass spectrometry. The selected antibiotics include quinolones, sulphonamides, macrolides, anthelmintics and one tetracycline. An extraction procedure based on QuEChERS methodology (quick, easy, cheap, effective, rugged and safe), consisting of a liquid extraction of the milk samples with acetonitrile without sample clean up was performed. The extract was centrifuged and the supernatant was filtered prior to chromatographic analysis. Several chromatographic conditions were optimized in order to obtain a fast separation (less than 10 min). The antibiotics were detected by electrospray ionization in positive ion mode with multiple reaction monitoring (MRM) and mass spectrometric conditions were optimized in order to increase selectivity and sensitivity. The developed method was validated in terms of linearity, trueness, precision, limits of detection (LODs) and quantification. Mean recoveries ranged from 70% to 110% and interday precision was lower than 21%. LODs ranged from 1 to 4 microg/kg. Finally, the method was applied to real samples and only traces of tylosin and fenbendezol were detected in two samples.
开发了一种简单、选择性强且快速的多残留方法，用于通过超高压液相色谱-串联四极杆质谱法测定牛奶中的18种兽药。所选抗生素包括喹诺酮类、磺胺类、大环内酯类、驱虫药和一种四环素。采用基于QuEChERS方法（快速、简便、廉价、有效、耐用且安全）的提取程序，即使用乙腈对牛奶样品进行液液萃取，无需样品净化。萃取液离心后，上清液在进行色谱分析前进行过滤。优化了多种色谱条件以实现快速分离（不到10分钟）。通过电喷雾电离在正离子模式下以多反应监测（MRM）检测抗生素，并优化质谱条件以提高选择性和灵敏度。所开发的方法在线性、准确性、精密度、检测限（LOD）和定量方面进行了验证。平均回收率在70%至110%之间，日间精密度低于21%。检测限在1至4微克/千克之间。最后，该方法应用于实际样品，仅在两个样品中检测到痕量的泰乐菌素和芬苯达唑。
