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Analysis of aldehydes in human exhaled breath condensates by in-tube SPME-HPLC.

Analytica chimica acta (2015-11-18)
ShuLing Wang, Sheng Hu, Hui Xu
ZUSAMMENFASSUNG

In this paper, polypyrrole/graphene (PPy/G) composite coating was prepared by a facile electrochemical polymerization strategy on the inner surface of a stainless steel (SS) tube. Based on the coating tube, a novel online in-tube solid-phase microextraction -high performance liquid chromatography (IT-SPME-HPLC) was developed and applied for the extraction of aldehydes in the human exhaled breath condensates (EBC). The hybrid PPy/G nanocomposite exhibits remarkable chemical and mechanical stability, high selectivity, and satisfactory extraction performance toward aldehyde compounds. Moreover, the proposed online IT-SPME-HPLC method possesses numerous superiorities, such as time and cost saving, process simplicity, high precision and sensitivity. Some parameters related to extraction efficiency were optimized systematically. Under the optimal conditions, the recoveries of the aldehyde compounds at three spiked concentration levels varied in the range of 85%-117%. Good linearity was obtained with excellent correlation coefficients (R(2)) being larger than 0.994. The relative standard deviations (n = 5) of the method ranged from 1.8% to 11.3% and the limits of detection were between 2.3 and 3.3 nmol L(-1). The successful application of the proposed method in human EBC indicated that it is a promising approach for the determination of trace aldehyde metabolites in complex EBC samples.

MATERIALIEN
Produktnummer
Marke
Produktbeschreibung

Sigma-Aldrich
Methanol, ACS reagent, ≥99.8%
Sigma-Aldrich
Ameisensäure, reagent grade, ≥95%
Sigma-Aldrich
Ameisensäure, ACS reagent, ≥96%
Sigma-Aldrich
Methanol, anhydrous, 99.8%
Sigma-Aldrich
Methanol, Laboratory Reagent, ≥99.6%
Sigma-Aldrich
Ameisensäure, ACS reagent, ≥88%
Sigma-Aldrich
Methanol, ACS spectrophotometric grade, ≥99.9%
Sigma-Aldrich
Pyrrol, reagent grade, 98%
Sigma-Aldrich
Methanol, ACS reagent, ≥99.8%
Supelco
SPME-Faseranordnung, 50/30µm DVB/CAR/PDMS, StableFlex (1 cm), needle size 23 ga, Autosampler, pk of 3, plain gray hub
Supelco
SPME-Faseranordnung, 50/30µm DVB/CAR/PDMS, StableFlex (2cm), needle size 24 ga, Autosampler, pk of 3, notched gray hub
Sigma-Aldrich
Methanol, Absolute - Acetone free
Supelco
SPME-Faseranordnung, 50/30µm DVB/CAR/PDMS, StableFlex (1cm), needle size 24 ga, Manual Holder, pk of 3, plain gray hub
Sigma-Aldrich
Methanol, BioReagent, ≥99.93%
Sigma-Aldrich
Capronaldehyd, 98%
Supelco
SPME-Faseranordnung, 50/30µm DVB/CAR/PDMS, StableFlex (2cm), needle size 23 ga, Autosampler, pk of 3, notched gray hub
Supelco
SPME-Faseranordnung Polydimethylsiloxan (PDMS), 100 μm PDMS, Fused Silica (1 cm), needle size 23 ga, Autosampler, pk of 3, red hub
Supelco
SPME-Faseranordnung, 50/30µm DVB/CAR/PDMS, StableFlex (1 cm), needle size 24 ga, Autosampler, pk of 3, plain gray hub
Sigma-Aldrich
Methanol, ACS reagent, ≥99.8%
Supelco
SPME-Faseranordnung Polydimethylsiloxan (PDMS), 100 μm PDMS, Fused Silica (1 cm), needle size 24 ga, Manual Holder, pk of 3, red hub
Sigma-Aldrich
Butyraldehyd, purified by redistillation, ≥99.5%
Supelco
SPME-Faseranordnung Carboxen/Polydimethylsiloxan (CAR/PDMS), 75 μm CAR/PDMS, Fused Silica (1 cm), needle size 24 ga, Manual Holder, pk of 3, black hub
Sigma-Aldrich
Heptanal, ≥95%, FCC, FG
Sigma-Aldrich
Ameisensäure, ≥95%, FCC, FG
Sigma-Aldrich
Octanal, 99%
Supelco
SPME-Faseranordnung Polydimethylsiloxan (PDMS), 100 μm PDMS, Fused Silica (1 cm), needle size 24 ga, Autosampler, pk of 3, red hub
Supelco
SPME-Faseranordnung Polydimethylsiloxan/Divinylbenzen (PDMS/DVB), 65 μm PDMS/DVB, Fused Silica (1 cm), needle size 24 ga, Manual Holder, pk of 3, blue hub
Sigma-Aldrich
Valeraldehyd, 97%
Sigma-Aldrich
Pyrrol, ≥98%, FCC, FG
Supelco
SPME-Faseranordnung Carboxen/Polydimethylsiloxan (CAR/PDMS), 85 μm CAR/PDMS, StableFlex (1 cm), needle size 23 ga, Autosampler, pk of 3, light blue hub