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Adsorbent phases with nanomaterials for in-tube solid-phase microextraction coupled on-line to liquid nanochromatography.

Journal of chromatography. A (2016-01-23)
R A González-Fuenzalida, E López-García, Y Moliner-Martínez, P Campíns-Falcó
ABSTRACT

Following the present trends in miniaturization, a methodology that combines on-line In-Tube Solid-Phase Microextraction (IT-SPME) with Liquid Nanochromatography (nano-LC) and UV-vis diode array detection (DAD) was developed. This coupling was achieved by using two interconnected valves (i.e. conventional and micro-automatic valves) in the system of injection. As for IT-SPME, different materials, containing in some cases nanostructures or nanoparticles and in other cases polymeric adsorbent phases immobilized on capillary columns, were tested in order to improve extraction efficiencies of organic compounds; diclofenac was selected as the target analyte. Additionally, the transfer time of the sample between the two injection valves, as well as the lengths and the internal diameters of the capillary columns, was optimized. Under the selected conditions, the resulting IT-SPME-nano-LC-DAD method showed great potential to become a powerful analytical tool as it was successfully applied to the determination of diclofenac in pharmaceutical and water samples. For comparison purposes, IT-SPME coupled to Capillary Liquid Chromatography (Cap-LC) was used. The extraction yield of diclofenac reached near 80%, a high value for techniques that involve IT-SPME. Good accuracy (recoveries near 100%) and precision (4% RSD) were obtained.

MATERIALS
Product Number
Brand
Product Description

Supelco
IonSense® PDMS/DVB SPE-it Tips, pkg of 96 ea
Supelco
SPME fiber assortment kit 5, needle size 23 ga, for use with autosampler
Supelco
SPME fiber assortment kit 2, for use with manual holder, needle size 24 ga
Supelco
SPME fiber assembly, Carbowax-Polyethylene Glycol (PEG) Coating, needle size 23 ga, df 60 μm (PEG), for use with autosampler
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
Supelco
SPME fiber assortment kit 2, for use with autosampler, needle size 23 ga
Supelco
SPME StableFlex fiber assortment kit, needle size 23 ga, for use with autosampler
Supelco
SPME fiber assortment kit 4, for use with autosampler, needle size 23 ga
Supelco
SPME fiber assortment kit 1, for use with autosampler, needle size 24 ga
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SPME Fiber Assembly Polydimethylsiloxane/Divinylbenzene (PDMS/DVB), fused silica fiber, df 65 μm (PDMS/DVB), for use with manual holder, needle size 23 ga
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SPME Fiber Assembly Polydimethylsiloxane/Divinylbenzene (PDMS/DVB), df 65 μm (PDMS/DVB), needle size 24 ga, for use with autosampler
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 assortment kit 1, for use with manual holder, needle size 24 ga
Supelco
SPME StableFlex fiber assortment kit, for use with manual holder
Supelco
SPME fiber assortment kit 4, for use with manual holder, 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
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 assortment kit 2, for use with autosampler, size 24 ga
Supelco
SPME Fiber Assembly Polydimethylsiloxane/Divinylbenzene (PDMS/DVB), df 65 μm (PDMS/DVB), for use with autosampler, needle size 23 ga
Supelco
SPME fiber assortment kit 1, for use with autosampler, needle size 23 ga
Supelco
SPME StableFlex fiber assortment kit, for use with autosampler, needle size 24 ga
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 assortment kit 4, for use with autosampler, size 24 ga
Supelco
SPME LC Tips, C18, tray of 96 ea
Supelco
SPME Fiber Assembly Polydimethylsiloxane/Divinylbenzene (PDMS/DVB), df 65 μm (PDMS/DVB), for use with autosampler, needle size 23 ga, metal alloy fiber
Supelco
SPME fiber assembly Polydimethylsiloxane (PDMS), df 100 μm (PDMS), for use with autosampler, needle size 24 ga
Supelco
SPME fiber assembly Polydimethylsiloxane (PDMS), df 7 μm (PDMS), needle size 24 ga, for use with manual holder
Supelco
SPME fiber assembly polyacrylate (PA), df 85 μm (PA), for use with autosampler, needle size 24 ga
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SPME Sampling Stand, for use with 4 mL vials
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SPME Portable Field Sampler, coating CAR/PDMS