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  • [PMIM]Br@TiO2 nanocomposite reinforced hollow fiber solid/liquid phase microextraction: an effective extraction technique for measurement of benzodiazepines in hair, urine and wastewater samples combined with high-performance liquid chromatography.

[PMIM]Br@TiO2 nanocomposite reinforced hollow fiber solid/liquid phase microextraction: an effective extraction technique for measurement of benzodiazepines in hair, urine and wastewater samples combined with high-performance liquid chromatography.

Journal of chromatography. B, Analytical technologies in the biomedical and life sciences (2015-01-16)
Zarrin Es'haghi, Azizollah Nezhadali, Shahriyar Bahar, Shahab Bohlooli, Alireza Banaei
ABSTRACT

A new design of hollow fiber solid-liquid phase microextraction (HF-SLPME) was developed for the determination of benzodiazepines (BZPs) in hair, urine and wastewater. The membrane extraction with 1-pentyl-3-methylimidazolium bromide coated titanium dioxide ([PMIM]Br@TiO2) sorbent used in this research is a two-phase supported membrane extraction consisting of an aqueous (donor phase), and n-octanol/nano [PMIM]Br@TiO2 (acceptor phase) system operated in direct immersion sampling mode. The 1-pentyl-3-methylimidazolium bromide (ionic liquid) coated nano TiO2 dispersed in the organic solvent (n-octanol) is held into a porous membrane supported by capillary forces and sonification. It is in contact with the feed phase, which is the aqueous sample. The experimental setup is very simple and highly affordable. The hollow fiber is disposable, so single use of the fiber reduces the risk of cross-contamination and carry-over problems. The proposed method allows the very effective and enriched recuperation of BZPs into one single extract. In order to obtain high extraction efficiency of the analytes using this novel sorbent, the main parameters were optimized. Under the optimized extraction conditions, the method showed good linearity (0.05-6000ngmL(-1)), low limits of detection (0.08-0.5ngmL(-1)) and good enrichment (533-1190).

MATERIALS
Product Number
Brand
Product Description

Sigma-Aldrich
1-Bromopentane, 98%
Sigma-Aldrich
Methanol, anhydrous, 99.8%
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Titanium(IV) isopropoxide, 97%
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1-Methylimidazole, ReagentPlus®, 99%
Sigma-Aldrich
Titanium(IV) isopropoxide, ≥97.0%
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Acetonitrile solution, contains 0.1 % (v/v) trifluoroacetic acid, suitable for HPLC
Supelco
SPME Portable Field Sampler, coating PDMS/DVB
Supelco
SPME fiber assembly Polydimethylsiloxane (PDMS), df 30 μm(PDMS, needle size 24 ga, for use with autosampler
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SPME Fiber Assembly Polydimethylsiloxane/Divinylbenzene (PDMS/DVB), df 65 μm(PDMS/DVB, for use with autosampler, needle size 23 ga
Supelco
SPME Sampling Stand, for use with 15 mL vials
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), fused silica fiber, df 65 μm(PDMS/DVB, for use with manual holder, needle size 23 ga
Supelco
SPME fiber assembly Polydimethylsiloxane (PDMS), df 7 μm(PDMS, needle size 24 ga, for use with manual holder
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 manual holder, needle size 24 ga
Supelco
SPME fiber assembly polyacrylate (PA), df 85 μm(PA, for use with autosampler, needle size 24 ga
Supelco
SPME fiber assembly Polydimethylsiloxane (PDMS), df 100 μm(PDMS, for use with autosampler, needle size 24 ga
Sigma-Aldrich
Acetonitrile solution, contains 0.1 % (v/v) formic acid, suitable for HPLC
Sigma-Aldrich
1-Methylimidazole, ≥99%, purified by redistillation
Sigma-Aldrich
1-Octanol, anhydrous, ≥99%
Supelco
SPME fiber assembly Polydimethylsiloxane (PDMS), metal alloy fiber, df 100 μm(PDMS, needle size 23 ga, for use with autosampler
Sigma-Aldrich
Acetonitrile solution, contains 10.0% acetone, 0.05% formic acid, 40.0% 2-propanol
Supelco
SPME fiber assembly, Carbowax-Polyethylene Glycol (PEG) Coating, needle size 23 ga, df 60 μm(PEG, for use with autosampler
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SPME fiber assembly polyacrylate (PA), df 85 μm(PA, for use with autosampler, needle size 23 ga
Supelco
SPME fiber assembly Polydimethylsiloxane (PDMS), df 7 μm(PDMS, needle size 23 ga, for use with autosampler
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 Portable Field Sampler, coating CAR/PDMS
Sigma-Aldrich
Acetonitrile solution, contains 0.05 % (v/v) trifluoroacetic acid
Supelco
SPME fiber assembly Polydimethylsiloxane (PDMS), df 100 μm(PDMS, for use with manual holder, needle size 23 ga
Supelco
SPME fiber assembly, Carbowax-Polyethylene Glycol (PEG) Coating, needle size 23 ga, df 60 μm(PEG, metal alloy fiber, for use with manual holder