高效液相色谱法测定城市污泥堆肥中的三氯生  

Monitoring of Triclosan in Municipal Sewage Sludge Composting by High Performance Liquid Chromatography

作　　者：汪敏[1,2] 郑国砥[2,3] 王学东[1] 牛明杰[2] 刘长利[2,3] 

机构地区：[1]首都师范大学资源环境与旅游学院,北京100048 [2]中国科学院地理科学与资源研究所环境修复中心,北京100101 [3]中国科学院大学资源与环境学院,北京100049

出　　处：《中国给水排水》2017年第16期121-126,共6页China Water & Wastewater

基　　金：国家自然科学基金面上项目(41371455)

摘　　要：采用加速溶剂萃取法(ASE)-固相萃取净化法(SPE),联合高效液相色谱法(HPLC-UV)测定城市污泥堆肥中三氯生。通过对加速溶剂萃取条件、固相萃取净化和高效液相色谱条件的优化,最后确定ASE萃取溶剂为二氯甲烷,SPE净化采用HLB固相萃取柱,甲醇/丙酮(V∶V=1∶1)为洗脱溶剂,流动相为甲醇/水(V∶V=80∶20),检测波长λ=280 nm。当三氯生浓度在1~20μg/m L时,其HPLC峰面积与其浓度呈良好的线性关系,相关系数r^2=0.997 4,加标回收率在79.7%~104.1%之间,检出限(S/N=3)为0.16μg/g,RSD<13%。该方法简便、快速、准确、重复性较好,能满足城市污泥堆肥中三氯生定量分析要求。An accelerated solvent and high performance liquid chromatograp extraction （ASE） - solid phase extraction purification （SPE） hy-uhraviolet detector （HPLC-UV） method were used for monitoring of triclosan （TCS） in sewage sludge compost. Optimal conditions were determined as： dichlo- romethane was as extractant ; HLB column was used as separation column ; methanol/acetone （ V ： V = 1 ： 1 ） was adopted as eluate, while methanol/H20 （ V ： V = 80 ： 20） was employed as mobile phase ; and finally , the wavelength of ultraviolet detector was set as 280 nm. When triclosan concentration was 1 - 20 μg/mL, the satisfactory linearities with the area of HPLC and concentration （ r2 = 0. 997 4） was obtained. The average recoveries were from 79.7% to 104.1%. The limit of detection （S/N = 3 ） was 0.16 μg/g, while the RSD was less than 13%. It has been demonstrated that the method was conven- ient, repeatable and suitable for determination of triclosan in sewage sludge compost.

关 键 词：城市污泥 堆肥 三氯生 高效液相色谱法 加速溶剂萃取 

分 类 号：O657.72[理学—分析化学] X703[理学—化学]