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Annals of Occupational Hygiene Advance Access originally published online on September 23, 2008
Annals of Occupational Hygiene 2008 52(8):757-763; doi:10.1093/annhyg/men057
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© The Author 2008. Published by Oxford University Press on behalf of the British Occupational Hygiene Society

Validation of Transferability of DBA Derivatization and LC–MS/MS Determination Method for Isocyanates via an Interlaboratory Comparison

Ivana Bobeldijk1,*, Daniel Karlsson2, Anjoeka Pronk1,3, John Gonsalves1, Maarten Hekman1, Dick Van De Lagemaat4, Liesbeth Preller1, Dick Heederik3 and Gunnar Skarping2

1 TNO Quality of Life, Quality and Safety, Utrechtseweg 48, 3700 AJ Zeist, The Netherlands
2 Division of Work Environment Chemistry, Department of Analytical Chemistry, Stockholm University, PO Box 460, S-281 24 Hassleholm, Sweden
3 Division of Environmental Epidemiology, Institute for Risk Assessment Sciences, Utrecht University, Utrecht, The Netherlands
4 Ducares, Utrechtseweg 48, Zeist, The Netherlands

* Author to whom correspondence should be addressed; Tel: +31-30-6944282; fax: +31-30-6944894; e-mail: ivana.bobeldijk{at}tno.nl

An adapted method for the quantitative determination of isocyanates in air was implemented and validated in-house. The method was based on air sampling using an impinger flask containing di-n-butylamine (DBA) in toluene and a glass fibre filter in series. The DBA derivatives were determined using liquid chromatography and tandem mass spectrometry. Studied isocyanates were isophorone diisocyanate, isocyanic acid (ICA), methyl isocyanate, ethyl isocyanate, propyl isocyanate, hexamethylene diisocyanate (HDI), 2,6- and 2,4-toluene diisocyanate, 4,4'-methylene diphenyl diisocyanate (MDI), phenyl isocyanate (PhI), MDI oligomers and different HDI adducts. Monitoring of selected reactions resulted in quantifications with correlation coefficients >0.995, within-batch relative standard deviation (RSD) of repeatability was <13% for all analytes. Between-batch RSD (reproducibility) was determined for all the compounds with the exception of the adducts and oligomers and was also <13%. As an additional validation procedure, the method was evaluated by exchanging field (air) and standard samples between two laboratories. The RSDs observed by the two laboratories were comparable. The concentrations determined were between 80 and 120% of each other, depending on the analyte and the individual concentrations. The method was applied in a large field study on exposure of workers in car repair shops and industrial painters with >500 samples.

Keywords: DBA • interlaboratory method comparison • isocyanates • liquid chromatography mass spectrometry

Received April 6, 2008; in final form July 8, 2008


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