Huertas-Pérez José Fernando, Arroyo-Manzanares Natalia, Havlíková Lucie, Gámiz-Gracia Laura, Solich Petr, García-Campaña Ana M
Department of Analytical Chemistry, Faculty of Sciences, University of Granada Campus Fuentenueva s/n, E-18071 Granada, Spain.
Department of Analytical Chemistry, Faculty of Pharmacy, Charles University in Prague, Heyrovského 1203, 500 05 Hradec Králové, Czech Republic.
J Pharm Biomed Anal. 2016 May 30;124:261-266. doi: 10.1016/j.jpba.2016.02.040. Epub 2016 Mar 3.
A simple, effective and reliable method for the determination of eight sulfonamide antibiotics (sulfadiazine, sulfapiridine, sulfamerazine, sulfamethazine, sulfachloropiridazine, sulfamethoxazole, sulfadoxine, sulfadimethoxin) in chicken muscle and eggs by liquid chromatography and fluorescence detection has been developed and validated. Sulfonamides do not present native fluorescence, however their direct determination was achieved by on-line post-column photochemical derivatization by UV irradiation. Sample treatment was based on QuEChERS with several modifications depending on the matrix. Egg extracts were cleaned-up using PSA for the dispersive solid phase extraction step. On the other hand, a new clean-up sorbent, Supel™ QuE Z-Sep(+), has been successfully applied in chicken muscle extract and has proved to be effective for interference removal from this matrix. Under optimum conditions, recoveries from 65.9 to 88.1%, relative standard deviations lower than 10% (except for sulfachloropiridazine), and limits of quantification (LOQs) from 14 to 85 μg kg(-1) were achieved. Thus, the method complies with current European requirements.
已开发并验证了一种通过液相色谱和荧光检测测定鸡肉和鸡蛋中八种磺胺类抗生素（磺胺嘧啶、磺胺吡啶、磺胺甲基嘧啶、磺胺二甲嘧啶、磺胺氯吡嗪、磺胺甲恶唑、磺胺多辛、磺胺二甲氧嘧啶）的简单、有效且可靠的方法。磺胺类药物本身不具有荧光，但通过紫外照射在线柱后光化学衍生化实现了它们的直接测定。样品处理基于QuEChERS，并根据基质进行了一些修改。鸡蛋提取物在分散固相萃取步骤中使用PSA进行净化。另一方面，一种新型净化吸附剂Supel™ QuE Z-Sep(+)已成功应用于鸡肉提取物中，并被证明对去除该基质中的干扰有效。在最佳条件下，回收率为65.9%至88.1%，相对标准偏差低于10%（磺胺氯吡嗪除外），定量限为14至85 μg kg(-1)。因此，该方法符合当前欧洲的要求。
