固相萃取-高效液相色谱法测定畜牧粪便中13种抗生素药物残留

建立了固相萃取-反相高效液相色谱法测定畜牧粪便中5种磺胺类、4种四环素类、2种喹诺酮类以及氯霉素和呋喃唑酮的检测方法.采用乙腈和0.01 mol/L草酸作为流动相分离4种四环素类和氯霉素,乙腈和0.025 mol/L醋酸铵作为流动相分离5种磺胺类和其它3种抗生素.结果表明,检测的13种抗生素出峰时间稳定,峰形较好,检出限0.01～0.05 mg/L,定量下限0.03～0.167 mg/L,采用柠檬酸缓冲液酸化的乙腈对猪粪便样品前处理,采用EDTA-McIlvaine提取液对鸡粪便样品前处理,两类样品均通过HLB固相萃取小柱纯化富集,回收率为54%～103%.该方法成功用于天津市4个畜牧养殖基地的20个畜牧粪便样品中抗生素的检测.结果表明,均有不同浓度的抗生素检出,浓度范围0.3～173 mg/kg.

Determination of Thirteen Antibiotics Residues in Manure by Solid Phase Extraction and High Performance Liquid Chromatography

A method was developed for the determination of five sulfonamides,four tetracyclines,two quinolones,furazolidone and chloramphenicol in liquid manure and chicken dung using solid phase extraction with high performance liquid chromatographic detection.Acetonitrile and 0.01 molL oxalic acid were used as the mobile phase to seperate four tetracyclines and chloramphenicol.Five sulfonamides,two quinolones and furazolidone were separated by acetonitrile and 0.025 molL NH4OAc.Limit of detection and quantization fall into the range of 0.01-0.05 mgL and 0.03-0.167 mgL respectively.Thirteen antibiotics in liquid manure and chicken dung were extracted using a mixture of ACN acidified with acetate buffer and EDTA and McIlvaine buffer respectively,then they were cleaned-up and pre-concentrated by hydrophilic-liphophilic balance(HLB) cartridge.The recoveries are 54%-103%.This method was successfully used in the detection of 13 antibiotics in 4 livestock husbandries in Tianjin.Results showed the above all antibiotics were detected,with concentrations of 0.3-173.2 mgkg.