摘要
采用HLB固相萃取、超高效液相色谱-串联质谱(UPLC-MS/MS)法,在多反应监测(MRM)模式下建立污水处理厂进、出水口水样中7种雌激素(戊酸雌二醇、炔雌醇、雌三醇、雌二醇、己烷雌酚、雌酮和己烯雌酚)的快速筛查测定方法,优化了固相萃取条件(萃取柱、洗脱液、pH值以及淋洗液)和UPLC-MS/MS分析条件(流动相及梯度、毛细管电压、锥孔电压、射频透镜电压、碰撞能量、离子源温度、脱溶剂气流量和锥孔气流量)。当7种雌激素质量浓度在1～100μg.L-1线性范围内时,所得回归方程的决定系数r2均大于0.997 2,方法检测限为4.40～10.27 ng.L-1,在20～100 ng.L-1雌激素添加水平范围内,进、出水口水样中目标物平均回收率分别为70.3%～95.1%和72.6%～96.7%,相对标准偏差(RSD)分别小于10.4%和9.5%。将该方法应用于南京地区4个综合污水处理厂进、出水口水样中雌激素的测定,4个污水处理厂进水中均含有高达几十、甚至上百ng.L-1的戊酸雌二醇、雌三醇和雌酮,出水中也含有几到几十ng.L-1的某几种雌激素。
An instant estrogen screening and determination method,using the HLB solid-phase extraction and ultra-performance liquid chromatography-electrospray tandem mass spectrometry technology（UPLC-MS/MS） in a multiple reaction monitoring（MRM） mode,was established for determination of seven estrogens（estradiol valerate,ethynylestradiol,estriol,estradiol,hexestrol,estrone and diethylstilbestrol） in the influent and final effluent of a wastewater treatment plant.Conditions for performances of solid-phase extraction（selection of extraction cartridge,eluate and its volume used for elution,pH adjustment of the water sample,and rinsing solution） and for UPLC-MS/MS analysis（mobile phase and gradient,capillary voltage,cone voltage,RF lens voltage,collision energy,ion source temperature,desolvation gas flow and cone gas flow） were optimized.In the case that all the seven estrogens were in the linear range of 1-100 μg·L-1,in mass concentration,all the determination coefficients（r2） of the regression equation were over 0.997 2,and the detection limit of the method ranged from 4.40 to 10.27 ng·L-1 for estrogens.When the mass concentration of estrogens was raised to the range of 20-100 ng·L-1,the recovery rates of the target substances in the influent and effluent water samples were in the range from 70.3% to 95.1% and from 72.6% to 96.7%,separately,with relative standard deviation（RSD） below 10.4% and 9.5%,separately.This method was applied to determine estrogens in influents and effluents of four major integrated wastewater treatment plants in Nanjing.It was found that concentrations of estradiol valerate,estriol and estrone reached as high as dozens and even hundred of ng·L-1 in the influents and several or dozens in the final effluents.
出处
《生态与农村环境学报》
CAS
CSSCI
CSCD
北大核心
2011年第5期86-92,共7页
Journal of Ecology and Rural Environment
基金
环境保护部公益性项目(200809094)
