Quantitative analysis of 2-furfural and 5-methylfurfural in different Italian vinegars by headspace solid-phase microextraction coupled to gas chromatography-mass spectrometry using isotope dilution.

Quantitative analysis of 2-furfural and 5-methylfurfural in different Italian vinegars by headspace solid-phase microextraction coupled to gas chromatography-mass spectrometry using isotope dilution.

Journal of chromatography. A (2003-10-31)

Lucia Giordano, Roberto Calabrese, Enrico Davoli, Domenico Rotilio

ABSTRACT

A new method was developed for the determination of 2-furfural (2-F) and 5-methylfurfural (5-MF), two products of Maillard reaction in vinegar, with head-space solid-phase microextraction (HS-SPME) coupled to gas chromatography-mass spectrometry (GC-MS). A divinylbenzene (DVB)/carboxen (CAR)/polydimethylsiloxane (PDMS) fibre was used and SPME conditions were optimised, studying ionic strength effect, temperature effect and adsorption time. Both analytes were determined by calibration established on 2-furfural-d4 (2-F-d4). The method showed good linearity in the range studied (from 16 to 0.12 mg/l), with a regression coefficient r2 of 0.9999. Inter-batch precision and accuracy were found between 14.9 and 6.0% and between -11.7 and 0.2%, respectively. Detection limit was 15 microg/l. The method is simple and accurate and it has been applied to a series of balsamic and non-balsamic vinegars.

MATERIALS

Product Number

Brand

Product Description

23446-U

Supelco

ORBO^™-93 Sorbent Tube, ORBO tube I.D. × L 6 mm × 95 mm, Bed A 180 mg, Bed B 90 mg, 60/80 mesh, pkg of 25 ea

57912-U

Supelco

SPME fiber assembly Divinylbenzene/Carboxen/Polydimethylsiloxane (DVB/CAR/PDMS), for use with autosampler, needle size 23 ga, metal alloy fiber, fiber L 1 cm

57914-U

Supelco

SPME fiber assembly Divinylbenzene/Carboxen/Polydimethylsiloxane (DVB/CAR/PDMS), for use with autosampler, needle size 23 ga, metal alloy fiber, fiber L 2 cm

57295-U

Supelco

SPME fiber assembly Carboxen/Polydimethylsiloxane (CAR/PDMS), d_f 85 μm(CAR/PDMS, needle size 23 ga, StableFlex, for use with autosampler

W270202

Sigma-Aldrich

5-Methylfurfural, ≥98%, FG

57318

Supelco

SPME fiber assembly Carboxen/Polydimethylsiloxane (CAR/PDMS), d_f 75 μm(CAR/PDMS, for use with manual holder, needle size 24 ga

57319

Supelco

SPME fiber assembly Carboxen/Polydimethylsiloxane (CAR/PDMS), d_f 75 μm(CAR/PDMS, needle size 24 ga, for use with autosampler

57343-U

Supelco

SPME fiber assembly Carboxen/Polydimethylsiloxane (CAR/PDMS), d_f 75 μm(CAR/PDMS, needle size 23 ga, for use with autosampler

57328-U

Supelco

SPME fiber assembly Divinylbenzene/Carboxen/Polydimethylsiloxane (DVB/CAR/PDMS), needle size 24 ga, for use with manual holder

25461

Supelco

Carboxen^®-1006 PLOT Capillary GC Column, L × I.D. 30 m × 0.53 mm, average thickness 30 μm

10263

Supelco

Carboxen^® Adsorbent, matrix Carboxen^® 563, 20-45 mesh, bottle of 10 g

10264

Supelco

Carboxen^® Adsorbent, matrix Carboxen^® 564, 20-45 mesh, bottle of 10 g

25467

Supelco

Carboxen^®-1010 PLOT Capillary GC Column, L × I.D. 30 m × 0.53 mm, average thickness 30 μm

10269

Supelco

Carboxen^® Adsorbent, matrix Carboxen^® 569, 20-45 mesh, bottle of 10 g

10471

Supelco

Carboxen^® Adsorbent, matrix Carboxen^® 1003, 40-60 mesh, bottle of 10 g

10478-U

Supelco

Carboxen^® Adsorbent, matrix Carboxen^® 1000, 60-80 mesh, bottle of 10 g

57334-U

Supelco

SPME fiber assembly Carboxen/Polydimethylsiloxane (CAR/PDMS), d_f 85 μm(CAR/PDMS, needle size 24 ga, for use with manual holder, StableFlex fiber

57329-U

Supelco

SPME fiber assembly Divinylbenzene/Carboxen/Polydimethylsiloxane (DVB/CAR/PDMS), needle size 24 ga, StableFlex, for use with autosampler

24246

Supelco

Carboxen^®-1010 PLOT Capillary GC Column, L × I.D. 30 m × 0.32 mm, average thickness 15 μm

24241-U

Supelco

Carboxen^®-1006 PLOT Capillary GC Column, L × I.D. 30 m × 0.32 mm, average thickness 15 μm

57335-U

Supelco

SPME fiber assembly Carboxen/Polydimethylsiloxane (CAR/PDMS), d_f 85 μm(CAR/PDMS, needle size 24 ga, StableFlex, for use with autosampler

57348-U

Supelco

SPME fiber assembly Divinylbenzene/Carboxen/Polydimethylsiloxane (DVB/CAR/PDMS), needle size 24 ga, StableFlex

57344-U

Supelco

SPME fiber assembly Carboxen/Polydimethylsiloxane (CAR/PDMS), d_f 75 μm(CAR/PDMS, needle size 23 ga, for use with manual holder

57299-U

Supelco

SPME fiber assembly Divinylbenzene/Carboxen/Polydimethylsiloxane (DVB/CAR/PDMS), needle size 23 ga, StableFlex, for use with manual holder or autosampler, fiber L 2 cm

57906-U

Supelco

SPME fiber assembly Carboxen/Polydimethylsiloxane (CAR/PDMS), d_f 85 μm(CAR/PDMS, for use with autosampler, needle size 23 ga, metal alloy fiber

137316

Sigma-Aldrich

5-Methylfurfural, ReagentPlus^®, 99%

57298-U

Supelco

SPME fiber assembly Divinylbenzene/Carboxen/Polydimethylsiloxane (DVB/CAR/PDMS), needle size 23 ga, StableFlex, for use with autosampler

54294-U

Supelco

Carboxen^® 572 for Tobacco Smoke, Adsorbent Bed Wt: 300 mg, cartridge size 3 mL, pkg of 50 ea

28718-U

Supelco

Tenax^® TA / Carboxen^® 1018, glass TD tube, preconditioned, O.D. × L 1/4 in. × 3 1/2 in., Sealed with (Swagelok^® End-Fittings), pkg of 10 ea

20358

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)