生态与农村环境学报 ›› 2013, Vol. 29 ›› Issue (3): 380-385.doi:

• 研究方法 • 上一篇    下一篇

水和土壤中磺胺和激素类药物的同时分析方法

陈传斌, 王娜, 孔德洋, 单正军, 高士祥   

  1. 南京大学环境学院
  • 收稿日期:2013-01-27 修回日期:2013-04-27 出版日期:2013-05-25 发布日期:2013-06-07
  • 通讯作者: 高士祥 南京大学环境学院 E-mail:ecsxg@nju.edu.cn
  • 作者简介:陈传斌(1989-),男,安徽六安人,硕士生,主要从事化学物质对生态环境和人体健康的安全性评价研究。E-mail:dalian19891104@163.com
  • 基金资助:

    环保公益性行业科研专项(201109038);中央级公益性科研院所2011年基本科研业务专项

Method for Simultaneous Determination of Sulfonamides and Hormone-Type Drugs in Water and Soil

CHEN  Chuan-Bin, WANG  Na, KONG  De-Yang, SHAN  Zheng-Jun, GAO  Shi-Xiang   

  1. School of the Environment,Nanjing University
  • Received:2013-01-27 Revised:2013-04-27 Online:2013-05-25 Published:2013-06-07
  • Contact: GAO Shi-Xiang School of the Environment,Nanjing University E-mail:ecsxg@nju.edu.cn

摘要: 建立了一种水和土壤中磺胺嘧啶、磺胺甲嘧啶、磺胺噻唑、磺胺二甲嘧啶、磺胺二甲氧嘧啶、磺胺甲恶唑6种磺胺类药物和17α-雌二醇、17β-雌二醇、雌酮、雌三醇、炔雌醇、乙烷雌酚6种激素类药物同时分析的方法。具体步骤:水样过滤后使用Oasis HLB 固相萃取小柱进行净化富集;土壤样品经加速溶剂提取(ASE)之后过Oasis HLB小柱净化富集;采用超高效液相色谱-串联质谱(UPLC-MS/MS)进行检测,分别以乙腈和1 mL•L-1甲酸溶液、乙腈和1 mL•L-1氨水溶液作为流动相。磺胺在水和土壤中的回收率分别为87.4%~103.6%和58.2%~80.0%,激素在水和土壤中的回收率分别为84.8%~101.8%和62.8%~79.3%,相对标准偏差均小于10.3%。水和土壤中磺胺的检测限分别为0.11~0.24 ng•L-1和0.01~0.02 ng•g-1,激素的检测限分别为0.31~2.14 ng•L-1和0.03~0.21 ng•g-1。用上述方法检测宿迁某典型养殖场周边的地表水和土壤,结果表明采用该方法检测环境样品中的磺胺和激素类药物是可行的。

关键词: 磺胺, 激素, 水, 土壤, 液相色谱-串联质谱, 分析方法

Abstract: A new method has been established for simultaneous determination of 6 sulfonamides, i.e. sulfadiazine, sulfamerazine, sulfathiazole, sulfamethazine, sulfadimethazine, sulfamethoxazole, and 6 hormone-type drugs, i.e. 17α-estradiol, 17β-estradiol, estrone, estriol, 17α-ethinyl-estradiol and hexestrol. Specific steps of the method are as following: After being filtered, water samples get purified and concentrated through Oasis HLB solid-phase extraction (SPE) cartridges. After accelerated solvent extraction (ASE), soil samples get purified and concentrated through Oasis HLB cartridges. Then the water and soil samples are analyzed by UPLC-MS/MS, which uses solvent of acetonitrile-and-methanoic acid (1 mL•L-1) and acetonitrile-and-ammonia (1 mL•L-1) as mobile phase respectively. The mean recovery rate of sulfonamides in water and soil samples varied in the range of 87.4-103.6% and 58.2-80.0%, respectively, and that of the hormones in the range of 84.8%-101.8% and 62.8%-79.3%, respectively, with relative standard deviation all below 10.3%. Detection limit of the method (MDL) for sulfonamides in water and soil ranged from 0.11 to 0.24ng•L-1 and from 0.01 to 0.02ng.g-1, respectively, and for the hormones did from 0.31 to 2.14 ng•L-1 and from 0.03 to 0.21 ng•L-1, respectively. This method was applied for determination of sulfonamides and hormones in the soil and surface water around a swine farm typical in Suqian area, with results demonstrating that this method is applicable to the determination of sulfonamides and hormone-type drugs in the environment.

Key words: sulfonamides, hormone, water, soil, LC-MS/MS, determination method

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