Departament de Quimica Analitica, Universitat de Barcelona, Spain.
Food Addit Contam Part A Chem Anal Control Expo Risk Assess. 2009 Jul;26(7):969-77. doi: 10.1080/02652030902810476.
A feasibility study of the preparation of quality control materials for the analysis of medicated feeds has been carried out. Two analytical methodologies for the analysis of sulfonamides in feeds were developed, validated and applied to homogeneity and stability studies. Pig feeds spiked with sulfadiazine and sulfadimidine were prepared. The drugs were spiked at 500 microg g(-1), representing what can be expected in a commercial medicated feed, and at 2 and 5 microg g(-1), which roughly correspond to drug-free feeds cross-contaminated during the fabrication process. The homogeneity of both the bulk and the bottled materials was verified. A stability study of the materials containing 2 and 5 microg g(-1) of sulfonamides was carried out over an 18-month period at room temperature, at 4 degrees C and -20 degrees C. The determination of sulfadiazine and sulfadimidine in samples coming from these homogeneity and stability studies of the quality control materials was carried out by high-performance liquid chromatography (HPLC) with either ultraviolet light or fluorimetric detection, depending on the concentration of the analytes in the samples.
已经开展了一项关于制备药用饲料分析用质控材料的可行性研究。开发、验证了两种用于饲料中磺胺类药物分析的分析方法，并将其应用于均匀性和稳定性研究。用磺胺嘧啶和磺胺二甲嘧啶对猪饲料进行了加标，添加浓度为 500μg g(-1)，这代表了商业药用饲料中的预期浓度，以及 2μg g(-1)和 5μg g(-1)，这大致对应于在制造过程中受到污染的无药饲料。验证了散装和瓶装材料的均匀性。在室温、4°C 和-20°C 条件下，对含有 2μg g(-1)和 5μg g(-1)磺胺类药物的材料进行了为期 18 个月的稳定性研究。通过高效液相色谱法（HPLC），根据样品中分析物的浓度，使用紫外光或荧光检测，对来自这些质控材料均匀性和稳定性研究的样品中的磺胺嘧啶和磺胺二甲嘧啶进行了测定。
