固相萃取-高效液相色谱法同时检测奶牛粪污中5种磺胺类抗生素

Simultaneous Determination of Five Sulfonamide Antibiotics in excrement and sewage of dairy farm Using Solid Phase Extraction and High Performance Liquid Chromatography

关键词:  奶牛粪污  磺胺类抗生素  固相萃取  高效液相色谱  

Key words:  Excrement and sewage of dairy farm  Sulfonamide antibiotics  Solid phage extraction  High Performance Liquid Chromatography

摘要:

建立的固相萃取-高效液相色谱法具有灵敏度高、检测限低的特点，可同时定量检测奶牛粪污中磺胺嘧啶、磺胺二甲嘧啶、磺胺间甲氧嘧啶、磺胺甲恶唑、磺胺喹噁啉的残留。采用C18色谱柱(500mm×4.6nm, 5μm)，以0.3%的乙酸-乙腈溶液为流动相，在流速1.0mL/min、检测波长270nm、柱温30℃条件下，5种抗生素均能达到基线分离；3倍信噪比下，5种抗生素的检出限均为20μg/kg。在加标浓度50μg/kg条件下，奶牛粪污样品经前处理、MCX固相萃取小柱富集净化后，五种磺胺类抗生素回收率达到75%~80%，相对标准偏差为2.8%~3.9%。此方法检测了某规模化奶牛场粪污中磺胺类抗生素残留，结果显示，磺胺嘧啶的浓度范围在45~50μg/kg，其他抗生素无检出。

Abstract:

A method for simultaneous determination of sulfadiazine (SDZ), sulfamethoxazole (SDMD), sulfamonomethoxine (SMM), sulfamethoxazole (SMZ), sulfaquinoxaline (SQ) in excrement and sewage of dairy farm using solid phase extraction and high performance liquid chromatography was established. Five antibiotics have been separated at the baseline on the C18 cloumn (500mm×4.6nm, 5μm) at the wavelength of 270 nm , 30℃ of column temperature after eluted by 0.3% acetate solution and acetonitrile. The limits of detection of five sulfonamide antibiotics was 20μg/kg. After the excrement and sewage of dairy farm samples were enriched and cleaned-up by MCX , the recovery of five antibiotics at the concentration of 50μg/kg in samples was 75%~80% and repeatability within one day (RSD) was 2.8%~3.9%. The method was applied to determined five antibiotics in samples collected from a dairy farm in Wuhan, only sulfadiazine has been detected and the concentration was in the range of 45~50μg/kg. The method has high sensitivity and low detection line, which can be used for the quantitative detection of sulfonamide antibiotics in excrement and sewage of dairy farm.