基质固相分散-高效液相色谱法测定蜂蜜中10种磺胺类药物  

Determination of ten sulfonamide residues in honey with matrix solid phase dispersion-high performance liquid chromatography

作　　者：余辉菊[1] 杨晓松[1] 杨胜利[2] 

机构地区：[1]成都市疾病预防控制中心,四川成都610041 [2]成都市武侯区疾病预防控制中心,四川成都610041

出　　处：《中国食品卫生杂志》2011年第2期147-150,共4页Chinese Journal of Food Hygiene

基　　金：成都市卫生局重大医学联合攻关项目(080808);成都市疾病预防控制中心重点科研项目(080102)

摘　　要：目的建立基质固相分散-高效液相色谱法测定蜂蜜中10种磺胺类药物残留量的方法,包括磺胺、磺胺嘧啶、磺胺吡啶、磺胺甲基嘧啶、磺胺二甲基嘧啶、磺胺甲氧嘧啶、磺胺间甲氧嘧啶、磺胺氯哒嗪、磺胺甲唑和磺胺二甲异唑。方法蜂蜜样品与C18固相吸附剂于玻璃研钵中研磨均匀,得半干状混合物,装入空的固相萃取管中,盖上一层滤纸,以1+3二氯甲烷-乙酸乙酯(V/V)为洗脱剂洗脱,洗脱液经氮气吹干,用流动相溶解残渣,经0.45μm滤膜过滤,Agilent TC-C18(4.6 mm×250 mm,5μm)色谱柱分离,高效液相色谱法测定。结果 10种磺胺类药物的线性范围为0.10～10.00 mg/L,相关系数r>0.999,样品加标回收率60.0%～109.3%,相对标准偏差小于10%,方法检出限0.016～0.025 mg/L,样品中磺胺类检出限为0.050～0.079 mg/kg。Objective To establish a method for the determination of 10 sulfonamides in honey,including sulfanilamide,sulfadiazine,sulfapyridine,sulfamerazine,sulfamethazine,sulfameter,sulfamonomethoxine,sulfachloropyridazine,sulfamethoxazole and sulfisoxazole,with matrix solid phase dispersion and high performance liquid chromatography.Methods Honey sample was grinded and well-distributed with a solid-phase sorbent C18 in a glass mortar to form a semi-solid mixture.The mixture was packed as a solid phase extraction（SPE） cartridge,covered with a piece of paper on the top of the mixture to produce a sample/column material;and then eluted with 20ml 1 ＋ 3 methylene-ethyl acetate（V/V）.The eluted materials were collected and evaporated to dry at 40 ℃ by nitrogen gas.The residues were dissolved in 0.5ml of mobile phase solvent and passed through a 0.45 μm filter membrane,and then were separated by an Agilent TC-C18 column（4.6 mm × 250 mm,5 μm） and determined by HPLC.Results The linear ranges of 10 sulfonamides were 0.10-10.00 mg/L,r 0.999.The recovery ranges were 60.0%-109.3% and RSD 10%.The detection limits were 0.016-0.025 mg/L and the quantification limits were 0.050-0.079 mg/kg.

关 键 词：高效液相色谱 基质固相分散 蜂蜜 磺胺 

分 类 号：S896.1[农业科学—特种经济动物饲养]