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Merck
  • Development of a functionalized polymeric ionic liquid monolith for solid-phase microextraction of polar endocrine disrupting chemicals in aqueous samples coupled to high-performance liquid chromatography.

Development of a functionalized polymeric ionic liquid monolith for solid-phase microextraction of polar endocrine disrupting chemicals in aqueous samples coupled to high-performance liquid chromatography.

Analytical and bioanalytical chemistry (2015-07-30)
Juanjuan Feng, Min Sun, Yanan Bu, Chuannan Luo
RESUMEN

Ionic liquids (ILs) have been efficiently used as a "designer sorbent" in sample preparation. A novel 1-(3-aminopropyl)-3-(4-vinylbenzyl)imidazolium 4-styrenesulfonate IL monomer was synthesized and copolymerized with 1,6-di(3-vinylimidazolium) hexane bishexafluorophosphate IL as cross-linking agent to prepare a cross-linked polymeric ionic liquids (PILs) monolith. Coupled to high-performance liquid chromatography (HPLC), the PILs monolith was used as a solid-phase microextraction (SPME) sorbent to extract some polar endocrine disrupting chemical (EDCs) such as estrogens, bisphenol A, and phthalate esters in aqueous samples. Preparation and extraction conditions were investigated and optimized to obtain satisfactory extraction efficiency. Limits of detection (LODs) of the proposed method for three steroid estrogens and bisphenol A were 0.25 and 0.2 μg L(-1), respectively, which were lower than or comparable to some other sample preparation methods. Intra- and inter-day repeatability for all the analytes was 2.2-12%. The monolith-to-monolith repeatability was 7.4-15%. The extraction performance of the method for analysis of target estrogens in treated domestic wastewater was investigated and compared with a dispersive liquid-liquid microextraction (DLLME) method. The proposed SPME method provided better sensitivity and higher resistance to matrix interferences.

MATERIALES
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Sigma-Aldrich
Dess-Martin periodinane, 97%
Supelco
Bisphenol A, ≥99%
Sigma-Aldrich
4-Vinylbenzyl chloride, 90%
Sigma-Aldrich
Diethyl phthalate, 99.5%
Supelco
Filtro SPME Polidimetilsiloxano (PDMS), df 100 μm(PDMS, needle size 24 ga, for use with manual holder
Sigma-Aldrich
1-Vinylimidazole, ≥99%
Supelco
Filtro SPME Polidimetilsiloxano (PDMS), df 100 μm(PDMS, for use with autosampler, needle size 23 ga
Sigma-Aldrich
1,6-Dibromohexane, 96%
Sigma-Aldrich
Sodium 4-vinylbenzenesulfonate, technical, ≥90% (T)
Sigma-Aldrich
Bisphenol A, 97%
Supelco
Filtro SPME Polidimetilsiloxano (PDMS), df 100 μm(PDMS, for use with autosampler, needle size 24 ga
Sigma-Aldrich
Estrone, ≥99%
Sigma-Aldrich
1-(3-Aminopropyl)imidazole, ≥97%
Supelco
SPME fiber assembly Polydimethylsiloxane/Divinylbenzene (PDMS/DVB), df 65 μm(PDMS/DVB, needle size 24 ga, for use with manual holder
Supelco
SPME fiber assembly Polydimethylsiloxane/Divinylbenzene (PDMS/DVB), df 65 μm(PDMS/DVB, needle size 23 ga, PDMS/DVB StableFlex, for use with autosampler
Supelco
SPME fiber assembly Polydimethylsiloxane/Divinylbenzene (PDMS/DVB), df 65 μm(PDMS/DVB, for use with autosampler, needle size 23 ga
Supelco
SPME fiber assembly Polydimethylsiloxane/Divinylbenzene (PDMS/DVB), df 65 μm(PDMS/DVB, needle size 24 ga, StableFlex, for use with autosampler
Supelco
SPME fiber assembly polyacrylate (PA), df 85 μm(PA, for use with autosampler, needle size 23 ga
Sigma-Aldrich
Diethyl phthalate, ≥99%
Supelco
SPME fiber assembly polyacrylate (PA), df 85 μm(PA, for use with autosampler, needle size 24 ga
Supelco
SPME fiber assembly Polydimethylsiloxane/Divinylbenzene (PDMS/DVB), df 65 μm(PDMS/DVB, needle size 24 ga, StableFlex, for use with manual holder
Sigma-Aldrich
Diethylstilbestrol, ≥99% (HPLC)
Supelco
SPME fiber assembly Polydimethylsiloxane/Divinylbenzene (PDMS/DVB), df 65 μm(PDMS/DVB, needle size 24 ga, for use with autosampler