建立了固相萃取-超高效液相色谱-串联质谱同时测定畜禽饮用水中 4类 23种抗生素(磺胺类、喹诺酮类、四环素类、氯霉素类)和3种 β-受体激动剂(克伦特罗、莱克多巴胺、沙丁胺醇)的分析方法.样品经高氯酸调节 pH至5. 0,加入乙二胺四乙酸二钠( Na2 EDTA),HLB固相萃取柱富集,用超高效液相色谱-质谱联用仪分时段多反应监测离子模式分析,外标法定量抗生素,内标法定量 β-受体激动剂.23 种抗生素和 3 种 β-受体激动剂的空白基质加标回收率为50. 7%~104. 6%,相对标准偏差( n=3)为2. 6%~8. 8%.23种抗生素和 3种 β-受体激动剂的线性关系良好,相关系数均大于0. 994,检出限为0. 01~0. 20 ng/L.通过该方法分析了北京地区 36家规模化畜禽养殖场畜禽饮用水中的抗生素和 β-受体激动剂,检出了多种抗生素,并对含量进行了定量计算.
A method has been developed for the simultaneous determination of 23 antibiotics ( four categories)and 3 β-agonists in livestock drinking water using solid-phase extraction and ultra performance liquid chromatography coupled with electrospray ionization tandem mass spectrometry(UPLC-ESI MS/MS). The samples were adjusted pH to 5. 0,added Na2EDTA, enriched and cleaned-up by an HLB solid-phase extraction cartridge. The target compounds were confirmed and quantified by UPLC-ESI MS/MS with external standard method for the anti-biotics and internal standard method for the β-agonists. The recoveries were assessed by using lab tap water as matrix. The average recoveries of the 23 antibiotics and the 3 β-agonists were in the range of 50. 7%-104. 6% and the relative standard deviations( RSDs)were 2. 6%-8. 8%( n=3). Under the optimal conditions,the calibration curves of the 23 antibiotics and the 3 β-agonists showed good linearity with the correlation coefficients better than 0. 994. The limits of detection( LODs,S/N≥3)ranged from 0. 01-0. 20 ng/L. The developed method was applied to analyze the livestock drinking waters in 36 Beijing intensive livestock farms. The results showed that some antibiotics were detected.