【作者】 余胜兵； 鲁琳； 苏广宁； 钟秀华； 朱杰民； 黄伟雄； 朱炳辉；

【Author】 Yu Shengbing;Lu Lin;Su Guangning;Zhong Xiuhua;Zhu Jiemin;Huang Weixiong;Zhu Binghui;Center for Disease Prevention and Control of Guangdong Province;

【机构】 广东省疾病预防控制中心；

【摘要】 水体中抗生素污染具有污染浓度低、种类多的特点,因而低检出限、多组分同时快速检测是饮用水中抗生素检测的热点之一[1]。现有报道的检测方法大多不能实现多种类型抗生素的同时检测,导致实验耗时较长、操作繁琐。本文通过对样品萃取条件的优化和色谱质谱条件的优化,建立了饮用水中磺胺类、喹诺酮类、β-内酰胺类、大环内酯类、抗菌增效剂和精神类等60种抗生素的超高效液相色谱-串联质谱的检测方法。水样调节pH至2.0后,加入同位素内标和金属螯合剂Na₂EDTA充分混匀。用HLB固相萃取小柱进行富集净化浓缩,超高效液相色谱-串联质谱测定分析,内标法定量。抗生素的检出限在0.001-0.6ng/L,定量限在0.004-1.9 ng/L。大部分抗生素在0.2-40 ng/L范围内,相关系数良好（R2>0.99）。低、中、高三种浓度抗生素水样的加标回收率在58.3%-127.7%。精密度在1.6-13.9%。采用所建立的方法对水源水、出厂水和管网末梢水进行分析,获得了满意的结果。本文建立的方法具有操作简单、灵敏、快速、准确的优点,适用于饮用水中抗生素的多残留同时测定。更多还原

【Abstract】 A method for simultaneous determination of 60 kinds of antibiotics in water samples was developed. The pH of 1 L of water sample was adjusted to 2.0 by phosphate buffer. The water sample was then concentrated and purified by the oasis HLB solid phase extraction column. The purified antibiotics was eluted by 10 m L of methanol and concentrated to 1.0 m L for ultra-performance liquid chromatography-tandem mass spectrometry analysis. Good linearity for major antibiotics in the range from 0.2 to 40 ng/L was obtained, with correlation coefficient(R2) ≥0.99 and the limits of determination within 0.001-0.6 ng/L and the limits of quantification within 0.004-1.9 ng/L, respectively.The recoveries of the spiked samples were 58.3%-127.7% at 3 spike levels( 1 ng/L,4 ng/L and 20 ng/L).The relative standard deviations were ranged from 1.6% to 13.9%. The established method is simple, rapid and accuracy, which can be applied to the determination and quantification of antibiotics residues in water samples.更多还原