邵天华,贲伟伟,苏都,张欢欢,侯嫔,强志民,张昱.城市污水处理厂污水及污泥中典型药物及其代谢产物的定量检测[J].环境科学学报,2020,40(6):2136-2141
城市污水处理厂污水及污泥中典型药物及其代谢产物的定量检测
- Quantitative determination of typical pharmaceuticals and their metabolites in municipal wastewater treatment plants
- 基金项目：国家自然科学基金（No.51678559）；国家重大科技专项（No.2017ZX07106005-01）
- 邵天华
- 1. 中国矿业大学(北京), 化学与环境工程学院, 北京 100083;2. 中国科学院生态环境研究中心, 饮用水科学与技术重点实验室, 北京 100085
- 贲伟伟
- 中国科学院生态环境研究中心, 饮用水科学与技术重点实验室, 北京 100085
- 苏都
- 中国科学院生态环境研究中心, 饮用水科学与技术重点实验室, 北京 100085
- 张欢欢
- 1. 中国矿业大学(北京), 化学与环境工程学院, 北京 100083;2. 中国科学院生态环境研究中心, 饮用水科学与技术重点实验室, 北京 100085
- 侯嫔
- 中国矿业大学(北京), 化学与环境工程学院, 北京 100083
- 强志民
- 中国科学院生态环境研究中心, 饮用水科学与技术重点实验室, 北京 100085
- 张昱
- 中国科学院生态环境研究中心, 饮用水科学与技术重点实验室, 北京 100085
- 摘要：基于超声溶剂萃取、固相萃取和超高效液相色谱-质谱联用技术（UPLC-MS/MS），建立了一种适用于城市污水处理厂污水和污泥中2种典型药物（磺胺甲恶唑和卡马西平）及其5种代谢产物的同步分析方法.污水样品添加硫酸酸化、Na2EDTA络合金属离子后经固相萃取富集净化；污泥样品通过甲醇/0.2 mol·L-1柠檬酸溶液（1：1，体积比）超声萃取后经固相萃取富集净化.采用UPLC-MS/MS电喷雾电离源在多反应监测模式下进行目标物的定量分析.结果表明，在优化条件下，7种目标物标准曲线的线性可决系数（R2）均大于0.99，方法回收率为74%~217%，日内与日间相对标准偏差稳定（RSD<20%），污水定量限为0.17~2.42 ng·L-1，污泥定量限为0.20~2.85 μg·kg-1.将该方法成功应用于两家城市污水处理厂样品中，除N-AcSMX外其余6种目标物被检出，其在污水和污泥中的浓度分别为3.92（SMX-DG）~667（LCBZ）ng·L-1和0.41（2OH-CBZ）~2.74（CBZ）μg·kg-1.
- Abstract：The study herein developed an analytical method for simultaneously determining two commonly-used pharmaceuticals and their five metabolites in the wastewater and sludge phases from wastewater treatment plants, by applying ultrasonic solvent extraction (USE), solid phase extraction (SPE) and ultra-performance liquid chromatography-mass spectrometry (UPLC-MS/MS). The wastewater samples were firstly acidified by sulfuric acid and added with Na2EDTA to chelate metal ions, and then went through SPE to enrich compounds and purify the background interference. The sludge samples were firstly extracted by USE with a mixture of methanol and 0.2 mol·L-1 citric acid (1:1, V:V), and then followed by SPE process. Thereafter, the target compounds were analyzed by UPLC-MS/MS equipped with an electrospray ionization source under multi-reaction monitor (MRM) mode. After optimization, the linear relationship coefficients (R2) of all target compounds were higher than 0.99, the method recoveries were in the range of 74%~217%, the method quantitative limits for the wastewater and sludge samples were in the range of 0.17~2.42 ng·L-1 and 0.20~2.85 μg·kg-1, respectively. This method has been successfully applied in determining samples from two municipal wastewater treatment plants. Six target compounds could be detected except for N-AcSMX, with the concentration ranges of 3.92~667 ng·L-1 and 0.41~2.74 μg·kg-1 in wastewater and sludge samples, respectively.
