固相萃取-高效液相色谱法同时检测畜禽粪便中14种兽药抗生素

研究并优化了同时分析畜禽粪便中14种抗生素(四环素、磺胺、氟喹诺酮和大环内酯类)的加速溶剂萃取参数、固相富集净化程序、以及高效液相色谱分离和检测条件。结果表明,以1%乙酸(pH 2.6)作为流动相,在270 nm的检测波长下,14种抗生素能达到基线分离。3倍信噪比下,四环素、磺胺、氟喹诺酮和大环内酯类抗生素的检出限分别为35～90μg/kg,12～28μg/kg,9～17μg/kg及19μg/kg。加标浓度在1和10μg/g时,畜禽粪便样品经过50%甲醇的柠檬酸盐缓冲溶液提取,HLB固相萃取柱富集净化后,四环素、磺胺、氟喹诺酮和大环内酯类抗生素的回收率分别达到了58%～75%和66%～83%,74%～93%和91%～101%,74%～80%和80%～88%,85%和68%,相对标准偏差分别为6.2%～10.7%和7.8%～13.6,2.6%～10.2%和4.4%～13.2%,6.1%～12.5%和8.3%～14.6%,10.6%和12.3%。采用此方法对辽宁省部分规模化养殖场的猪粪、牛粪和鸡粪样品进行了检测。4类抗生素都有检出,浓度范围分别为0.75～22.34 mg/kg,0.10～1.71 mg/kg,0.38～4.46 mg/kg和0.23～0.35 mg/kg。

Simultaneous Determination of Fourteen Verterinary Antibiotics in Animal Manure Using Solid Phase Extraction and Liquid Chromatography

A method for the simultaneous determination of fourteen antibiotics in animal manure was studied and the parameters of accelerated solvent extraction(ACE),programs of solid phase extraction(SPE) and HPLC detection conditions were optimized.Fourteen antibiotics had been separated at the baseline on a C18 column at the wavelength of 270 nm after eluted by 1% acetate solution(pH=2.6) and acetonitrile.The limits of detection for tetracyclines(TCs),sulfonamides(SAs),fluoroquinolones(FQs) and tylosin(TYL) were 35-90 μg/kg,12-28 μg/kg,9-17μg/kg and 19 μg/kg,respectively.After extracted by buffer solution of 50% methanol,then enriched and cleaned-up by HLB,the recoveries of antibiotics(at the concentration of 1 μg/g and 10 μg/g) in manure were 58%-75% and 66%-83%,4%-93% and 91%-101%,74%-80% and 80%-88%,85% and 68% for TCs,SAs,FQs and TYL,respectively.The method was applied to determine fourteen antibiotics in animal manure samples collected from Liaoning Province.TCs,SAs,FQs and TYL were all detected in these manure samples and the concentrations were in the range of 0.75-22.34 mg/kg,0.10-1.71 mg/kg,0.38-4.46 mg/kg and 0.23-0.35 mg/kg,respectively.