Di Sabatino Marcello, Di Pietra Anna Maria, Benfenati Luigi, Di Simone Bruno
University of Bologna, Department of Pharmaceutical Sciences, via Belmeloro 6, 40126 Bologna, Italy.
J AOAC Int. 2007 Mar-Apr;90(2):598-603.
A liquid chromatography (LC) method is described for the simultaneous determination of 10 commonly used sulfonamide drug residues in meat. The 10 sulfonamide drugs of interest were sulfadiazine, sulfathiazole, sulfamerazine, sulfadimidine, sulfamethizole, sulfamonomethoxine, sulfachloropyridazine, sulfadoxine, sulfadimethoxine, and sulfaquinoxaline. The residues were extracted with acetone-chloroform (1 + 1). Sulfonamides were quantitatively retained in the extracting solution and afterwards eluted from a cation-exchanger solid-phase extraction cartridge with a solution of methanol-aqueous ammonia. The solution was dried, reconstituted with 5 mL methanol and filtered before analysis by LC-ultraviolet using a C18 column with a mobile phase gradient of potassium dihydrogen phosphate buffer, pH 2.5, and methanol-acetonitrile (30 + 70, v/v). The method was applied to cattle, swine, chicken, and sheep muscle tissues. The validation was performed with a fortified cattle meat sample at level of 100 ppb, which is the administrative maximum residue limit for sulfonamides in the European Union. The limit of quantitation for all sulfonamides was between 3 and 14 ppb. Recovery was evaluated for different meat matrixes. The mean recovery values were between 66.3% for pork meat samples and 71.5% for cattle meat samples.
本文描述了一种液相色谱（LC）方法，用于同时测定肉类中10种常用磺胺类药物残留。所关注的10种磺胺类药物为磺胺嘧啶、磺胺噻唑、磺胺甲基嘧啶、磺胺二甲嘧啶、磺胺甲噻二唑、磺胺间甲氧嘧啶、磺胺氯哒嗪、磺胺多辛、磺胺二甲氧嘧啶和磺胺喹恶啉。残留物用丙酮 - 氯仿（1 + 1）提取。磺胺类药物定量保留在提取液中，随后用甲醇 - 氨水从阳离子交换固相萃取柱上洗脱。溶液干燥后，用5 mL甲醇复溶并过滤，然后使用C18柱通过LC - 紫外进行分析，流动相为磷酸二氢钾缓冲液（pH 2.5）与甲醇 - 乙腈（30 + 70，v/v）的梯度洗脱。该方法应用于牛、猪、鸡和羊的肌肉组织。在100 ppb水平下对强化牛肉样品进行了验证，这是欧盟磺胺类药物的行政最大残留限量。所有磺胺类药物的定量限在3至14 ppb之间。评估了不同肉类基质的回收率。猪肉样品的平均回收率为66.3%，牛肉样品的平均回收率为71.5%。
