用于同时测定养猪废水中10种抗生素的固相萃取-液相色谱串联.docVIP

固相萃取-液相色谱-串联质谱法测定养猪废水中10种抗生素 闾幸1,2，余卫娟3，兰亚琼2，李立2，叶朝霞3，刘锐2*，陈吕军2,4 ，张永明1 （1. 上海师范大学生命与环境科学学院，上海 200234；2. 浙江省水质科学与技术重点实验室，浙江清华长三角研究院生态环境研究所，嘉兴 314006；3. 嘉兴市环境保护监测站，嘉兴 314000；4.清华大学环境学院，北京 100084） 摘要：建立了一种固相萃取-液相色谱串联质谱分析技术，适用于同时检测养猪废水中的10种常见抗生素污染物，包括：3种四环素类（土霉素、四环素和金霉素）、2种磺胺类(磺胺二甲基嘧啶和磺胺甲噁唑)、3种喹诺酮类(恩诺沙星、诺氟沙星和环丙沙星)和2种大环内酯类（泰乐菌素和罗红霉素）。水样由稀盐酸调节pH值至3.0，流经200 mg/6 mL Oasis HLB固相萃取柱富集后再用甲醇洗脱、氮吹，共富集20倍。LC-MS/MS采用Aglient eclipse XDB C18色谱柱（4.6×150 mm, 5 μm）分离，用乙腈和0.1%甲酸水二元流动相梯度洗脱，流速为0.3 mL·min-1。该方法对养猪废水样品的加标回收率为53%~104%，略低于但接近去离子水的加标回收率（62%~106%），方法的检出限为0.03 μg·L-1（磺胺类）~3.5 μg·L-1（四环素），相对标准偏差（n=3）为0.5%~6.3%。 关键词：养猪废水；抗生素；四环素类；大环内酯类；喹诺酮类；磺胺类；LC-MS/MS 中图分类号： 文献标识码：A 文章编号： LC-MS/MS Determination of 10 Antibiotics in Swine Wastewater with Solid Phase Extraction Lü Xing1,2, YU Wei-juan3, LAN Ya-qiong2, LI Li2, YE Zhao-xia3, ZHANG Yong-ming1, LIU Rui2*, CHEN Lü-jun2,4 (1. College of Life and Environmental Science, Shanghai Normal University, Shanghai 200234, China; 2. Zhejiang Provincial Key Laboratory of Water Science and Technology, Department of Environment in Yangtze Delta Region Institute of Tsinghua University, Zhejiang, Jiaxing 314006, China; 3. Jiaxing Environmental Protection Monitoring Station, Jiaxing 314006, China; 4. School of Environment, Tsinghua University, Beijing 100084, China) Abstract: An analysis method, which combined liquid chromatography and tandem mass (LC-MS/MS) with solid-phase extraction (SPE), was developed for simultaneously determining commonly used veterinary antibiotics from swine wastewater, including: three kinds of tetracycline (oxytetracycline, tetracycline and chlortetracycline), two kinds of sulfa (sulfadimidine and sulfamethoxazole), three kinds of quinolones (enrofloxacin, norfloxacin and ciprofloxacin) and two kinds of macrolides (tylosin and roxithromycin). The pH of water samples were adjusted to 3.0 by HCl , eluted with methanol after enriched with Oasis HLB (200 mg/6 mL) column by twenty times and then blowed by nitrogen. Aglien