全自动固相萃取-高效液相色谱法测定养殖场废水中6种常见环境雌激素的残留量  

HPLC Determination the Residual Amounts of 6 Common Environmental Estrogens in Wastewater from Farms with Separation by Automatic Solid Phase Extraction

作　　者：罗书 LUO Shu(Luzhou Environmental Monitoring Center Station,Luzhou 646000,China)

机构地区：[1]泸州市环境监测中心站,泸州646000

出　　处：《理化检验（化学分册）》2019年第4期379-382,共4页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

摘　　要：取废水样品(1 000mL)静置约1h,取500mL上清液经过0.45μm滤膜过滤,滤液以10mL·min-1流量通过固相萃取柱,用甲醇-水(80+20)混合液将吸附富集在固相萃取柱上的6种环境雌激素洗脱并净化。收集洗脱液,将其吹氮至近干,用1.0mL甲醇溶解残渣,经过0.45μm滤膜过滤,用高效液相色谱法二极管阵列检测器在波长225nm处测定其中6种常见环境雌激素的含量。结果表明:6种常见环境雌激素的质量浓度均在0.10～5.0mg·L-1内与其信号强度之间呈线性关系,检出限(3S/N)在0.03～0.05mg·L-1之间。按照标准加入法进行加标回收试验,测得回收率在90.7%～108%之间;重复性试验的测定值相对标准偏差(n=6)在3.0%～4.8%之间。The wastewater sample(1 000 mL)was stood for about 1 h,and the supernatant(500 mL)was taken and filtered through 0.45μm filter membrane.The filtrate was passed through solid phase extraction column at a flow rate of 10 mL·min^-1.The extraction column was eluted with CH3 OH-H2 O(80+20)mixture to desorb the 6 common environmental estrogens from the column,and the eluate was blown to near dryness with nitrogen.The residue was dissolved in 1.0 mL of methanol and the solution was filtered with 0.45μm filter membrane.6 common environmental estrogens in the filtrate were determined by high performance liquid chromatography with diode array detector at the wavelength of 225 nm.As shown by the results,linear relationships between values of response signals and mass concentration of the 6 common environmental estrogens were found in the range of 0.10-5.0 mg·L^-1,with detection limits(3 S/N)in the range of 0.03-0.05 mg·L^-1.Test for recovery was made by standard addition method,giving results in the range of 90.7%-108%.Values of RSDs(n=6)found by repeatability test were in the range of 3.0%-4.8%.

关 键 词：高效液相色谱法 二极管阵列检测器 全自动固相萃取 环境雌激素 养殖场废水 

分 类 号：O657.7[理学—分析化学]