LC-MS/MS法分析生猪异位发酵床垫料中5大类兽用抗菌药物残留及蓄积趋势

建立了生猪异位发酵床垫料中四环素类、喹诺酮类、磺胺类、酰胺醇类和大环内酯类共54种抗菌药物残留量的LC-MS/MS检测方法，经超低温冷冻粉碎后的垫料样本，以费休氏-库仑滴定法测定水分，用Mcllvaine-Na2EDTA缓冲液和乙腈提取，经亲水亲脂平衡固相萃取小柱净化，用LC-MS/MS法测定抗菌药物残留量，最终结果以折水后含量表示。方法具有简便、高通量、抗干扰的特点，可以满足生猪异位发酵床垫料中主要兽用抗菌药物残留检测的要求。利用该方法，对12家养殖场垫料样本中5大类兽用抗菌药物的残留量进行了检测。12家养殖场垫料样本中共检出25种抗菌药物，各场垫料样本抗菌药物总残留量在0.7 g/t~28 g/t之间，其中四环素类药物对总残留量的贡献率在91.3%～98.8%之间。

Analysis of Residues of 5 Kinds of Antibiotics in Litters from Ectopic Pig Manure Fermentation Beds by LC-MS/MS

A High performance liquid chromatography tandem mass spectrometry (LC-MS/MS) method for the determination of five kinds of antibiotics residues in litters from ectopic pig manure fermentation bed was developed, which was used for the analysis of tetracyclines (TETs), quinolones (FLQs), sulpha (SAs), amphenicols (AMPs) and macrolides (MIs) levels in litters from 12 ectopic pig manure fermentation beds. After superfreezed crushing, the moisture of litters was measured by Fischer coulometric titration. The target compounds were extracted by Mcllvaine-Na2EDTA and acetonitrile, and Solid phase extraction (HLB) clean-up step was followed. Finally, the antibiotics levels were detected by LC-MS/MS, and the results were expressed as moisture-free. The data shows 25 kinds antibiotics were found in 12 ectopic pig manure fermentation beds, the total residual levels in each pig manure fermentation beds were between 0.7 and 28 g/t, TETs residues were the highest, and its contribution rates of the total residual levels were between 91.3% and 98.8% in the 12 ectopic pig manure fermentation beds.