Department of Analytical Chemistry, Faculty of Sciences, Campus Fuentenueva, s/n, E-18071 Granada, Spain.
J Chromatogr A. 2009 Nov 20;1216(47):8355-61. doi: 10.1016/j.chroma.2009.09.042. Epub 2009 Sep 23.
A sensitive and reliable method using capillary HPLC with UV-diode array detection (DAD) has been developed and validated for the trace determination of residues of 10 beta-lactam antibiotics of human and veterinary use, in milk, chicken meat and environmental water samples. The analytes included ampicillin, amoxicillin, penicillin V, penicillin G, cloxacillin, oxacillin, dicloxacillin, nafcillin, piperacillin and clavulanic acid. Legal levels are regulated by the EU Council regulation 2377/90 in animal edible tissues for these compounds. For food analysis, a solid-phase extraction (SPE) procedure consisting in a tandem of Oasis HLB and Alumina N cartridges was applied for off-line preconcentration and cleanup. For water analysis, the first step was only necessary. The limits of detection for the studied compounds were between 0.04-0.06 microg l(-1) for water samples and 0.80-1.40 microg l(-1) (or microg kg(-1)) in the case of foods derived from animals. Average recoveries for fortified samples at different concentration levels ranged between 82.9% and 98.2%, with relative standard deviations (RSDs) lower than 9%. The method showed the advantages of capillary HPLC for the detection of these widely applied antibiotics in different samples at very low concentration levels.
已开发并验证了一种使用毛细管 HPLC 与紫外-二极管阵列检测(DAD)的灵敏可靠方法,用于痕量测定牛奶、鸡肉和环境水样中 10 种人用和兽用β-内酰胺抗生素的残留。分析物包括氨苄西林、阿莫西林、青霉素 V、青霉素 G、氯唑西林、苯唑西林、双氯西林、萘夫西林、哌拉西林和克拉维酸。这些化合物在动物可食用组织中的欧盟理事会法规 2377/90 对其进行了法定管制。对于食品分析,采用了固相萃取(SPE)程序,由 Oasis HLB 和 Alumina N 柱串联组成,用于离线预浓缩和净化。对于水样,仅需进行第一步即可用于水分析。所研究化合物的检测限为 0.04-0.06μg l(-1),而动物源性食品中的检测限为 0.80-1.40μg l(-1)(或μg kg(-1))。在不同浓度水平下添加的样品的平均回收率在 82.9%至 98.2%之间,相对标准偏差(RSD)低于 9%。该方法显示了毛细管 HPLC 在检测不同样品中这些广泛应用的抗生素方面的优势,即使在非常低的浓度水平下也能进行检测。