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
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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%.
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%.
引文
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[12]李强,赵炜,蔡立鹏等.气相色谱-串联质谱测定乳粉中6种雌激素[J].乳业科学与技术,2013,36(6):18-20.
[2]张彤炬,何以嘉.深井曝气工艺处理激素制药废水[J].中国给水排水,2012,28(4):72-77.
[3]吴曼莉,时艺馨,李炜,等.高效液相色谱-二极管紫外阵列/荧光串联测定雌激素的方法及污水处理厂对雌激素的去除特性[J].环境工程学报,2017,11(4):2614-2620.
[4]罗晓燕,林玉娜,刘莉治,等.固相萃取高效液相色谱法同时测定禽畜组织中雌雄性激素残留的研究[J].中国卫生检验杂志,2005,15(4):387-390.
[5]严忠雍,李佩佩,龙举,等.凝胶渗透色谱-液相色谱-串联质谱法测定水产品中性激素[J].广州化工,2014,42(23):121-124.
[6]王丽芳,李琼,姜佩华,等.高效液相色谱法同时测定化妆品中的5种性激素[J].精细化工,2008,25(5):479-481.
[7]李雪,牟光庆,陈历俊,等.固相萃取-高效液相色谱串联质谱法测定原料奶中5种环境雌激素残留量的研究[J].食品工业科技,2013,34(9):293-297.
[8]余玲,张银堂,张丹华,等.纳米金光度法快速检测水中雌激素[J].商丘师范学院学报,2014,30(9):30-33.
[9]刘美华,邱彬,陈国南,等.超声辅助离子液体分散液相微萃取-高效液相色谱法测定废水中雌激素的研究[J].分析测试技术与仪器,2009,15(3):151-157.
[10]郑永杰,靳凤龙,田景芝.高效液相色谱法测定乳粉和鸡肉中5种性激素[J].化学试剂,2013,35(6):522-526.
[11]宫玮,张培正.HPLC法测定鸭胚蛋中游离性激素的研究[J].食品与发酵工业,2007,33(5):115-119.
[12]李强,赵炜,蔡立鹏等.气相色谱-串联质谱测定乳粉中6种雌激素[J].乳业科学与技术,2013,36(6):18-20.