SPE-UFLC-MS/MS法测定制药废水中四环素类抗生素  

Determination of Tetracyclines in Pharmaceutical Wastewater by Solid Phase Extraction-Ultra Fast Liquid Chromatography-Tandem Mass Spectrometry

作　　者：李再兴[1,2] 张非非[1] 左剑恶[2] 张敬轩[3] 李挥[3] 余忻[2] 剧盼盼[1] 

机构地区：[1]河北科技大学环境科学与工程学院,河北石家庄050018 [2]清华大学环境学院,北京100084 [3]国家环保产品质量监督检验中心,河北石家庄050051

出　　处：《环境科学与技术》2013年第7期139-142,共4页Environmental Science & Technology

基　　金：十一五"国家水体污染控制与治理科技重大专项(2008ZX07529-006);河北省重大技术创新项目(12276703Z)

摘　　要：文章建立了利用固相萃取-超快速液相色谱-串联质谱（SPE-UFLC-MS/MS）测定制药废水中四环素类抗生素（土霉素、四环素和金霉素）残留的方法。水样经（30%硫酸锌＋20%亚铁氰化钾）溶液作为沉淀剂沉淀蛋白质后,上清液采用Oasis HLB固相萃取柱富集和净化,以（0.1%甲酸溶液＋乙腈）为流动相进行梯度洗脱,经Agilent ZORBAX SB C18柱分离后,在串联质谱ES（I＋）模式下进行MRM检测。该方法四环素类抗生素检出限（S/N=3时）0.02μg/L,3种目标物在0.010~1.0 mg/L范围内线性关系良好,线性相关系数在0.998 2~0.999 8之间。在0.20、0.40和0.60μg/L添加水平,各组分的回收率在80.8%~97.2%之间,相对标准偏差在5.31%~9.92%之间。该方法可满足制药废水中四环素类抗生素残留检测的要求。A method based on solid phase extraction-ultra fast liquid chromatography-tandem mass spectrometry（SPEUFLC-MS/MS）was developed to determine tetracyclines such as xoytetracycline,tetracycline,chlortetracycline in pharmaceutical wastewater.Water samples were firstly purified through protein precipitation process with 30% zinc sulfate and 20% potassium ferrocyanide,and the tetracyclines was enriched and purified with Oasis HLB SPE,separated through Agilent ZORBAX SB C18 UFLC using 0.1% formic acid solution and acetonitrile as mobile phase,and detected by mass spectrometry in positive ion mode with multiple reaction monitoring using an electrospray ionization interface.The detection limit was 0.02 μg/L.The linear range was 0.010 to 1.0 mg/L,with a correlation coefficient of 0.998 2~0.999 8.The recoveries at the spiked concentration of 0.20,0.40 and 0.60 μg/L ranged from 80.8% to 97.2%,with a relative standard deviation from 5.31% to 9.92%.The procedure would provide a method for determination of tetracyclines in pharmaceutical wastewater.

关 键 词：四环素类抗生素 超快速液相色谱-串联质谱 固相萃取 制药废水 

分 类 号：X832[环境科学与工程—环境工程]