Giampaolo Gori

High-performance liquid chromatographic determination of urinary 2,5-hexanedione as mono-2,4-dinitrophenylhydrazone using ultraviolet detection.

The good correlation between exposure to n-hexane and 2,5-hexanedione urinary excretion confers on this diketone an important toxicological meaning. this paper proposes a reversed-phase HPLC method which includes, after acid hydrolysis, a derivatization step of 2,5-hexanedione with 2,4-dinitrophenylhydrazine at 70 degrees C for 20 min. The reaction conditions, such as temperature, reagent concentration and time, are optimized so as to allow the condensation of a single carbonyl group. A linear response was obtained in the 0.19-20.0 mg/l range with a detection limit of 0.03 mg/l, corresponding to a signal-to-noise ratio of 3. A phosphate buffer (pH 3.3)-acetonitrile mixture (50:50) as the eluent and UV detection at 334 nm were used.

2-Methylanthraquinone as a Marker of Occupational Exposure to Teak Wood Dust in Boatyards

A new gas chromatographic/mass spectrometric (GC/MS) method was developed to detect 2-methylanthraquinone (2-MeA) in wood dust. 2-MeA is present in teak wood (a suspected human carcinogen) but not in oak, beech, mahogany, birch, ash or pine. The method involved collection of workplace dust on filters and extraction of 2-MeA with methanol and GC/MS analysis. The method was tested on teak wood dust samples (n = 43) collected on polyvinylchloride membrane filters during various work operations in four small factories making furniture and fittings for leisure craft and boatyards (air teak wood dust concentration: range 0.32-14.32 mg m(-3)). A high correlation coefficient for the content of 2-MeA versus teak dust was obtained (logarithmic correlation: y = 1.5308x + 0.0998, r = 0.9215). Determination of airborne 2-MeA is a useful technique to confirm occupational exposure to teak wood dust.

High performance liquid chromatographic determination of methyl ethyl ketone in urine as its 3-methyl-2-benzothiazolinone hydrazone derivative

SummaryA HPLC method for the determination of methyl ethyl ketone (MEK) in urine after derivatization with 3-methyl-2-benzothiazolinone hydrazone is proposed. The calibration curve for the ketone was linear, ranging between 0.23–10 mg/L, with a detection limit of 0.025 mg/L. The results were compared to those obtained by GC-MS, coupled to the headspace technique. MEK derivatization and the derivative purification processes were verified with respect to the main variables such as reaction temperature, reagent concentration, probable interferences and enrichment phase. The method is simple and reliable and shows a good sensitivity.

Mass spectrometric and gas and high-performance liquid chromatographic behaviour of an impurity in 2,5-hexanedione

Abstract The analysis of 2,5-hexanedione, a metabolic compound of several industrial solvents, is normally carried out using gas chromatographic (GC) or GC-mass spectrometric (MS) techniques. This work, with the aim of verifying the possibility of determining the diketone by means of a high-performance liquid chromatographic (HPLC) method with UV detection, illustrates the importance of the choice of a 2,5-hexanedione standard for the determination of the diketone response factor. In some commercial diketone samples the presence of an impurity, which may interfere with the analysis of the target analyte, was ascertained. This impurity showed GC and HPLC behaviour similar to that of 2,5-hexanedione, but gave a very different UV response. This impurity was identified as 3-methylcyclopent-2-enone by means of MS, GC-MS, HPLC-photodiode-array detection, IR and UV spectrometry. The structure was confirmed by comparing the chromatographic, mass and ultraviolet data of the unknown compound with those of a synthesized reference sample. The well known difficulty in determining 2,5-hexanedione by HPLC with UV detection was reconfirmed owing to its low molar absorptivity.