食品科学 ›› 2007, Vol. 28 ›› Issue (6): 256-259.

• 分析检测 • 上一篇    下一篇

牛奶中多种磺胺类抗生素残留的HPLC快速分析

 孙晶玮, 赵新淮   

  1. 东北农业大学乳品科学教育部重点实验室; 东北农业大学乳品科学教育部重点实验室 黑龙江哈尔滨150030; 黑龙江哈尔滨150030;
  • 出版日期:2007-06-15 发布日期:2011-12-31

Analysis of Sulfonamide Residues in Milk with Rapid HPLC Method

 SUN  Jing-Wei, ZHAO  Xin-Huai   

  1. Key Laboratory of Dairy Science, Ministry of Education, Northeast Agricultural University, Harbin 150030, China
  • Online:2007-06-15 Published:2011-12-31

摘要: 研究了牛奶中磺胺嘧啶、磺胺甲基嘧啶、磺胺二甲基嘧啶、磺胺甲噁唑、磺胺间甲氧嘧啶、磺胺二甲氧嘧啶六种磺胺类抗生素的多残留高效液相色谱(HPLC)分析方法。样品经氯仿-丙酮(2:1,V/V)提取两次,提取液浓缩至干。残渣用流动相甲醇-0.08%乙酸(60:40,V/V)溶解,净化后以反相C18柱,甲醇-0.08%乙酸等度洗脱,紫外检测器检测、外标法定量。结果表明,这六种抗生素在0.01~1.0mg/L浓度范围内呈线性关系,磺胺嘧啶、磺胺甲基嘧啶、磺胺二甲基嘧啶检的检出限为0.010mg/L、磺胺甲噁唑、磺胺间甲氧嘧啶、磺胺间二甲氧嘧啶检出限分别为0.015mg/L。分析的添加回收率为69.4%~123.5%,变异系数为<8%,整体分析时间小于3h。方法具有处理简单、检测快速、准确的特点。

关键词: 磺胺, 牛奶, 分析, 反相高效液相色谱

Abstract: The analysis method on six sulfonamides in milk, namely sulfamerazine, sulfamethazine, sulfamethoxazole, sulfamonomethoxine, sulfadimethoxine and sulfadiazine was studied. Milk containing sulfonamides was extracted with chloroform -acetone mixture (2:1, V/V) twice. The extract was combined and evaporated to dry, then dissolved in methanol-0.08% acetic acid (60:40, V/V). Purified by hexane, the extract was analyzed in HPLC in a C18 column with methanol-acetic acid-H2O as eluent. Sulfonamide residues were detected by a UV detector and their concentrations were determined with calibrated curves. A good linear relationship exists for all residues in concentration range of 0.01~1.0 mg/L, while the detection limit for sulfadiazine and sulfamerazine and sulfamethazine is 0.010 mg/L and for sulfadimethoxine and sulfamonomethoxine and sulfadimethoxine 0.015 mg/L. The analysis procedure needs total time less than 3 h with an addition recovery for sulfonamides about 69.4%~ 123.5% and coefficient of variation less than 8%. The method is rapid, simple and accurate.

Key words: sulfonamide, milk, analysis, RP-HPLC