Analysis of estrogens in environmental waters using polymer monolith in-polyether ether ketone tube solid-phase microextraction combined with high-performance liquid chromatography.
A simple, rapid and sensitive on-line method for simultaneous determination of four endocrine disruptors (17beta-estradiol, estriol, bisphenol A and 17alpha-ethinylestradiol) in environmental waters was developed by coupling in-tube solid-phase microextraction (SPME) to high-performance liquid chromatography (HPLC) with fluorescence detection (FLD). A poly(acrylamide-vinylpyridine-N,N'-methylene bisacrylamide) monolith, synthesized inside a polyether ether ketone (PEEK) tube, was selected as the extraction medium. To achieve optimum extraction performance, several parameters were investigated, including extraction flow-rate, extraction time, and pH value, inorganic salt and organic solvent content of the sample matrix. By simply filtered with nylon membrane filter and adjusting the pH of samples to 6.0 with phosphoric acid, the sample solution then could be directly injected into the device for extraction. Low detection limits (S/N=3) and quantification limits (S/N=10) of the proposed method were achieved in the range of 0.006-0.10 ng/mL and 0.02-0.35 ng/mL from spiked lake waters, respectively. The calibration curves of four endocrine disruptors showed good linearity ranging from quantification limits to 50 ng/mL with a linear coefficient R(2) value above 0.9913. Good method reproducibility was also found by intra- and inter-day precisions, yielding the RSDs less than 12 and 9.8%, respectively. Finally, the proposed method was successfully applied to the determination of these compounds in several environmental waters.
Wen
Yi
Y
Department of Chemistry, Wuhan University, Wuhan 430072, PR China.
Zhou
Bing-Sheng
BS
Xu
Ying
Y
Jin
Shi-Wei
SW
Feng
Yu-Qi
YQ
D001577:Benzophenones; D005591:Chemical Fractionation / Q000379:methods; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D052244:Endocrine Disruptors / Q000032:analysis* / Q000737:chemistry; D007659:Ketones / Q000737:chemistry*; D008855:Microscopy, Electron, Scanning / Q000379:methods; D011092:Polyethylene Glycols / Q000737:chemistry*; D011108:Polymers; D015203:Reproducibility of Results; D014867:Water / Q000032:analysis*; D014874:Water Pollutants, Chemical / Q000032:analysis* / Q000737:chemistry
D001577:Benzophenones; D052244:Endocrine Disruptors; D007659:Ketones; D011108:Polymers; D014874:Water Pollutants, Chemical; D014867:Water; C063834:polyetheretherketone; D011092:Polyethylene Glycols