In the present study, a column packed with core-shell particles was used for the separation and the quantification of 13 sulphonamides in milk by conventional high-performance liquid chromatography coupled with diode array ultraviolet detection (HPLC/UV-DAD). Preliminary experiments were carried out to investigate selectivity of different stationary phases. Best results were achieved using a C₁₈ column packed with 2.6 μm core-shell particles (diameter 4.6 mm, length 75 mm). A binary gradient elution based on acetate buffer solution at pH 4.50 and a mixture of methanol acetonitrile 50:50 (v/v) was employed at the flow rate of 1.2 mL min⁻¹ with an injection volume of 6 μL. These chromatographic conditions allowed the efficient separation of 13 sulphonamides in about 8 min. To evaluate the suitability of the method for official control analysis, the most important validation parameters were investigated according to the European Decision 657/2002/EC as established for analysis of drug residues in food. Sulphonamides were recovered from milk samples by a simple and quick preparation procedure consisting of an extraction step with chloroform/acetone and a purification step with n-hexane. Mean recoveries from raw milk ranged between 55% and 86% at the Maximum Residual Limit of 100 μg kg⁻¹, and RSDs% resulted lower than Thompson and Horwitz RSD% reference values for all sulphonamides. The LOQ value (2.7–15 μg kg⁻¹) was low enough to satisfy legal limits suggested by European Regulation 37/2010/EC.

在本研究中，使用填充有核壳颗粒的柱子通过常规高效液相色谱结合二极管阵列紫外检测（HPLC / UV-DAD）分离和定量测定牛奶中的13种磺酰胺。进行了初步实验以研究不同固定相的选择性。使用装有2.6μm核壳颗粒（直径4.6 mm，长度75 mm）的C ₁₈色谱柱可获得最佳结果。基于pH值为4.50的乙酸盐缓冲溶液和甲醇乙腈50:50（v / v）的混合物进行二元梯度洗脱，流速为1.2 mL min ^-1进样量为6μL。这些色谱条件允许在约8分钟内有效分离13种磺酰胺。为了评估该方法用于官方对照分析的适用性，根据建立用于分析食品中药物残留的欧洲决定657/2002 / EC对最重要的验证参数进行了研究。磺酰胺是由选自由提取步骤，用氯仿/丙酮中，用纯化步骤的简单且快速的制备程序从牛奶样品中回收Ñ正己烷。在最大残留限量为100μgkg ^-1时，从生乳中的平均回收率在55％至86％之间，并且RSDs％的结果低于所有磺胺类药物的Thompson和Horwitz RSD％参考值。LOQ值（2.7–15μg千克^-1）低到足以满足欧洲法规37/2010 / EC建议的法律限制。