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Solid-phase microextraction and gas chromatography-mass spectrometry for analysis of phenols and nitrophenols in rainwater, as their t-butyldimethylsilyl derivatives.

Analytical and bioanalytical chemistry (2007-01-30)
Farouk Jaber, Claude Schummer, Jamal Al Chami, Philippe Mirabel, Maurice Millet
ABSTRACT

Solid-phase microextraction (SPME) coupled with gas chromatography-mass spectrometry has been used for analysis of four phenols and sixteen nitrophenols in rainwater samples. Analytes were extracted from the water in the immersion mode and derivatised for 5 min during direct desorption in the GC injector. Before desorption, 2 microL N-(t-butyldimethylsilyl)-N-methyltrifluoroacetamide (MDBSTFA) was introduced into the injector, which was maintained at 280 degrees C. Different conditions affecting extraction efficiency were studied, including temperature, type of microextraction fibre, and effect of pH and ionic strength. Five different fibre coatings were tested: 85-mum polyacrylate (PA), 100-microm polydimethylsiloxane (PDMS), 65-mum Carbowax-divinylbenzene (CW-DVB), 75-microm Carboxen-polydimethylsiloxane (CAR-PDMS), and 65-microm polydimethylsiloxane-divinylbenzene (PDMS-DVB). The best conditions were use of PA fibres for 40 min at ambient temperature (75 g NaCl per 100 mL, pH 3.0). MDBSTFA was used as derivatising agent because it enables analysis of phenols derivatives with high confidence in identification, because in electron-impact mode TBDMS-phenol derivatives produce the specific M-57 ion. Quantification was achieved by using 4-nitrophenol-d4, at 1 mg L(-1), as internal standard. Linearity was good, with correlation coefficients in the range 0.9888 (o-cresol) to 0.9987 (dinitro-o-cresol, DNOC). Detection limits varied between 0.208 and 99.3 microg L(-1) and quantification limits between 0.693 and 331 microg L(-1). Uncertainties varied between 8.7% (phenol) and 17.9% (4-methyl-2-nitrophenol). The method was successfully applied to the analysis of rainwater collected at urban and rural sites in Alsace (East of France). Because of derivatisation in the injector and the associated high temperature, the lifetime of the fibre is severely reduced.

MATERIALS
Product Number
Brand
Product Description

Supelco
Carboxen®-1010 PLOT Capillary GC Column, L × I.D. 30 m × 0.53 mm, average thickness 30 μm
Supelco
ORBO 78 HBr on Carboxen® 564 specially cleaned (20/45), 400/200 mg, W,W,W separators, O.D. × L 6 mm × 110 mm, pkg of 25 ea
Supelco
ORBO 90 Carboxen® 564 (20/45), 160/80 mg, W,F,F separators, O.D. × L 6 mm × 75 mm, pkg of 25 ea, for analyte group MEK (methylethyl ketone)
Supelco
Carboxen® Adsorbent, matrix Carboxen® 1000, 60-80 mesh, bottle of 10 g
Supelco
Carboxen®-1006 PLOT Capillary GC Column, L × I.D. 30 m × 0.53 mm, average thickness 30 μm
Supelco
Carboxen®-1010 PLOT Capillary GC Column, L × I.D. 30 m × 0.32 mm, average thickness 15 μm
Supelco
Carboxen® Adsorbent, matrix Carboxen® 569, 20-45 mesh, bottle of 10 g
Supelco
Carboxen®-1006 PLOT Capillary GC Column, L × I.D. 30 m × 0.32 mm, average thickness 15 μm
Supelco
Carboxen® Adsorbent, matrix Carboxen® 569, 20-45 mesh, bottle of 500 g
Supelco
Carboxen® Adsorbent, matrix Carboxen® 1003, 40-60 mesh, bottle of 10 g
Supelco
Carboxen® Adsorbent, matrix Carboxen® 563, 20-45 mesh, bottle of 10 g
Supelco
Carboxen® Adsorbent, matrix Carboxen® 564, 20-45 mesh, bottle of 10 g
Supelco
Carboxen® Adsorbent, matrix Carboxen® 1000, 40-60 mesh, bottle of 50 g
Supelco
Carboxen® 1000 Reversible SPE Tube, 200 mg/mL, pk 30
Supelco
Carboxen® 572 for Tobacco Smoke, Adsorbent Bed Wt: (300 mg), cartridge volume 3 mL, pkg of 10 ea
Supelco
ORBO-93 Sorbent Tube, matrix Carboxen® 1000, ORBO tube I.D. × L 6 mm × 95 mm, Bed B 90 mg, Bed A 180 mg, 60/80 mesh, pkg of 25 ea
Supelco
SPME fiber assembly Carboxen/Polydimethylsiloxane (CAR/PDMS), df 75 μm (CAR/PDMS), for use with manual holder, needle size 24 ga
Supelco
SPME fiber assembly Divinylbenzene/Carboxen/Polydimethylsiloxane (DVB/CAR/PDMS), needle size 24 ga, for use with manual holder
Supelco
Carboxen® 569, O.D. × L 1/4 in. × 3 1/2, glass TD tube, fritted, Sealed with Brass Endcaps, preconditioned, pkg of 10 ea
Supelco
Carboxen® 572 for Tobacco Smoke, Adsorbent Bed Wt: 300 mg, cartridge size 3 mL, pkg of 50 ea
Supelco
SPME fiber assembly Carboxen/Polydimethylsiloxane (CAR/PDMS), df 75 μm (CAR/PDMS), needle size 23 ga, for use with manual holder
Supelco
SPME fiber assembly Divinylbenzene/Carboxen/Polydimethylsiloxane (DVB/CAR/PDMS), needle size 24 ga, StableFlex, for use with manual holder/autosampler
Supelco
Carboxen® 569, glass TD tube, fritted, O.D. × L 1/4 in. × 3 1/2 in., preconditioned, pkg of 10 ea
Supelco
Carboxen® Adsorbent, matrix Carboxen® 564, 20-45 mesh, pack of 144 × 290 mg
Supelco
SPME fiber assembly Carboxen/Polydimethylsiloxane (CAR/PDMS), df 75 μm (CAR/PDMS), needle size 24 ga, for use with autosampler
Supelco
SPME fiber assembly Divinylbenzene/Carboxen/Polydimethylsiloxane (DVB/CAR/PDMS), needle size 24 ga, StableFlex, for use with autosampler
Supelco
SPME fiber assembly Carboxen/Polydimethylsiloxane (CAR/PDMS), df 75 μm (CAR/PDMS), needle size 23 ga, for use with autosampler
Supelco
SPME fiber assembly Divinylbenzene/Carboxen/Polydimethylsiloxane (DVB/CAR/PDMS), needle size 23 ga, StableFlex, for use with manual holder/autosampler, fiber L 2 cm
Supelco
SPME fiber assembly Carboxen/Polydimethylsiloxane (CAR/PDMS), df 85 μm (CAR/PDMS), needle size 24 ga, for use with manual holder, StableFlex fiber
Supelco
SPME fiber assembly Divinylbenzene/Carboxen/Polydimethylsiloxane (DVB/CAR/PDMS), needle size 23 ga, StableFlex, for use with autosampler