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  • Determination of phthalate esters in environmental water by magnetic Zeolitic Imidazolate Framework-8 solid-phase extraction coupled with high-performance liquid chromatography.

Determination of phthalate esters in environmental water by magnetic Zeolitic Imidazolate Framework-8 solid-phase extraction coupled with high-performance liquid chromatography.

Journal of chromatography. A (2015-08-01)
Xiaomei Liu, Zhiwei Sun, Guang Chen, Wanwan Zhang, Yiping Cai, Rongmei Kong, Xiaoyan Wang, Yourui Suo, Jinmao You
ABSTRACT

In this study, the magnetic Zeolitic Imidazolate Framework-8 (ZIF-8) microspheres were successfully synthesized and applied as an effective sorbent for preconcentration of several typical phthalate esters (PAEs) from environmental water samples. Firstly, the solvothermal treatment method was used for preparation of Fe3O4 nanoparticles. Then, mercaptoacetic acid (MAA) was served as the functionalized chemical to modify Fe3O4 nanoparticles. The Fe3O4@ZIF-8 core-shell microspheres were synthesized through coating the MAA-capped Fe3O4 nanoparticles with ZIF-8. By coupling magnetic solid-phase extraction (MSPE) with high-performance liquid chromatography (HPLC), a reliable, sensitive and cost-effective method for simultaneous determination of five main PAEs including dimethyl phthalate (DMP), diethyl phthalate (DEP), di-n-butyl phthalate (DBP), benzyl butyl phthalate (BBP), and dioctyl phthalate (DOP) was developed. Good linearity was observed in the range of 1.0-100.0μg/L. The limits of detection (S/N=3) and limits of quantification (S/N=10) were in the range of 0.08-0.24 and 0.3-0.8μg/L, respectively. The relative standard deviations were less than 5.5% and the accuracies of the method for the PAEs were in the range from 85.6% to 103.6%. Finally, the Fe3O4@ZIF-8 was successfully applied for rapid extraction of trace amounts of PAEs in environmental water samples.

MATERIALS
Product Number
Brand
Product Description

Sigma-Aldrich
Dimethyl phthalate, ≥99%
Sigma-Aldrich
Dibutyl phthalate, 99%
Sigma-Aldrich
Dimethyl phthalate, ≥99%
Sigma-Aldrich
Methanol, anhydrous, 99.8%
Sigma-Aldrich
Dess-Martin periodinane, 97%
Sigma-Aldrich
Benzyl butyl phthalate, 98%
Sigma-Aldrich
Dioctyl phthalate, ≥99.5%
Sigma-Aldrich
Methanol, suitable for NMR (reference standard)
Sigma-Aldrich
Methanol, purification grade, 99.8%
Sigma-Aldrich
Toluene, JIS special grade, ≥99.5%
Sigma-Aldrich
Methanol solution, (Methanol:Dimethyl sulfoxide 1:1 (v/v))
Sigma-Aldrich
Methanol solution, contains 0.50 % (v/v) triethylamine
Sigma-Aldrich
Acetonitrile, electronic grade, 99.999% trace metals basis
Sigma-Aldrich
Diethyl pyrocarbonate, 96% (NT)
Sigma-Aldrich
Methanol solution, suitable for NMR (reference standard), 4% in methanol-d4 (99.8 atom % D), NMR tube size 3 mm × 8 in.
Sigma-Aldrich
Acetonitrile, Preparateur, ≥99.9% (GC), One-time steel-plastic (SP) drum
Sigma-Aldrich
Diethyl phthalate, 99.5%
Sigma-Aldrich
Di-n-octyl phthalate, ≥98.0% (GC)
Sigma-Aldrich
Diethyl phthalate, ≥99%
Sigma-Aldrich
Diethyl pyrocarbonate, 96% (NT)
Sigma-Aldrich
Acetonitrile, anhydrous, 99.8%
Sigma-Aldrich
Toluene, anhydrous, 99.8%
Sigma-Aldrich
Diethyl pyrocarbonate, 96% (NT)
Sigma-Aldrich
DBP, 98% (HPLC)
Sigma-Aldrich
Sodium phosphate dibasic dodecahydrate, BioXtra, ≥99.0% (T)
Sigma-Aldrich
Diethyl pyrocarbonate, Vetec, reagent grade, ≥97%
Sigma-Aldrich
Sodium phosphate dibasic dodecahydrate, Vetec, reagent grade, 99%