Paula Berton1,2,3,4, Noureen Siraj1,5, Susmita Das1,6, Sergio de Rooy1,7, Rodolfo G Wuilloud2,3, Isiah M Warner1. 1. Department of Chemistry, Louisiana State University, Baton Rouge, LA 70803, USA. 2. Laboratorio de Química Analítica para Investigación y Desarrollo (QUIANID), Facultad de Ciencias Exactas y Naturales, Universidad Nacional de Cuyo/Instituto Interdisciplinario de Ciencias Básicas (ICB), CONICET UNCUYO, Padre J. Contreras 1300, Mendoza 5500, Argentina. 3. Consejo Nacional de Investigaciones Científicas y Técnicas (CONICET), Autonomous City of Buenos Aires C1425FQB, Argentina. 4. Chemical and Petroleum Engineering Department, University of Calgary, 2500 University Drive NW, Calgary, AB T2N 1N4, Canada. 5. Department of Chemistry, University of Arkansas at Little Rock, Little Rock, AR 72204, USA. 6. Department of Chemistry, Amity University Kolkata, Major Arterial Road, Action Area II, Kadampukur Village, Rajarhat, Newtown, West Bengal 700135, India. 7. Shell Oil Products US, 150 N Dairy Ashford Rd, Houston, TX 77079, USA.
Abstract
In this study, three magnetic ionic liquids (MILs) were investigated for extraction of four estrogens, i.e., estrone (E1), estradiol (E2), estriol (E3), and ethinylestradiol (EE2), from environmental water. The cation trihexyl(tetradecyl)phosphonium ([P66614]+), selected to confer hydrophobicity to the resulting MIL, was combined with tetrachloroferrate(III), ferricyanide, and dysprosium thiocyanate to yield ([P66614][FeCl4]), ([P66614]3[Fe(CN)6]), and ([P66614]5[Dy(SCN)8]), respectively. After evaluation of various strategies to develop a liquid-liquid microextraction technique based on synthesized MILs, we placed the MILs onto a magnetic stir bar and used them as extracting solvents. After extraction, the MIL-enriched phase was dissolved in methanol and injected into an HPLC-UV for qualitative and quantitative analysis. An experimental design was used to simultaneously evaluate the effect of select variables and optimization of extraction conditions to maximize the recovery of the analytes. Under optimum conditions, limits of detection were in the range of 0.2 (for E3 and E2) and 0.5 μg L-1 (for E1), and calibration curves exhibited linearity in the range of 1-1000 μg L-1 with correlation coefficients higher than 0.998. The percent relative standard deviation (RSD) was below 5.0%. Finally, this method was used to determine concentration of estrogens in real lake and sewage water samples.
In this stunclass="Chemical">dy, three class="Chemical">n class="Chemical">magnetic ionic liquids (MILs) were investigated for extraction of four estrogens, i.e., estrone (E1), estradiol (E2), estriol (E3), and ethinylestradiol (EE2), from environmentalwater. The cation trihexyl(tetradecyl)phosphonium ([P66614]+), selected to confer hydrophobicity to the resulting MIL, was combined with tetrachloroferrate(III), ferricyanide, and dysprosium thiocyanate to yield ([P66614][FeCl4]), ([P66614]3[Fe(CN)6]), and ([P66614]5[Dy(SCN)8]), respectively. After evaluation of various strategies to develop a liquid-liquid microextraction technique based on synthesized MILs, we placed the MILs onto a magnetic stir bar and used them as extracting solvents. After extraction, the MIL-enriched phase was dissolved in methanol and injected into an HPLC-UV for qualitative and quantitative analysis. An experimental design was used to simultaneously evaluate the effect of select variables and optimization of extraction conditions to maximize the recovery of the analytes. Under optimum conditions, limits of detection were in the range of 0.2 (for E3 and E2) and 0.5 μg L-1 (for E1), and calibration curves exhibited linearity in the range of 1-1000 μg L-1 with correlation coefficients higher than 0.998. The percent relative standard deviation (RSD) was below 5.0%. Finally, this method was used to determine concentration of estrogens in real lake and sewage water samples.
Entities:
Keywords:
estrogens; magnetic ionic liquids; microextraction; wastewater samples
Authors: Kevin D Clark; Omprakash Nacham; Jeffrey A Purslow; Stephen A Pierson; Jared L Anderson Journal: Anal Chim Acta Date: 2016-06-13 Impact factor: 6.558
Authors: Samantha Macchi; Mohd Zubair; Robert Hill; Nabeel Alwan; Yusuf Khan; Nawab Ali; Grégory Guisbiers; Brian Berry; Noureen Siraj Journal: ACS Appl Bio Mater Date: 2021-09-24