Journalartikel

Jahr der Veröffentlichung: 2008

Seiten: 1237-1243

Zeitschrift: Journal of AOAC INTERNATIONAL

Bandnummer: 91

Heftnummer: 5

URL: https://aoac.publisher.ingentaconnect.com/contentone/aoac/jaoac/2008/00000091/00000005/art00035

Verlag: Oxford University Press

Abstract: 

A simple strategy for identification and quantification of lubricant additives in mineral oil was demonstrated by high-performance thin-layer chromatography with UV absorption and fluorescence detection using various coupling options, e.g., with attenuated total reflectance infrared (ATR-IR) spectroscopy, Fourier transform infrared (FTIR) spectroscopy, electrospray ionization mass spectrometry (ESI-MS), and direct analysis in real-time mass spectrometry (DART-MS). For the additives zinc bis(O,O'-diisobutyl dithlophosphate), zinc bis(O,O'-didodecyl dithlophosphate), and Anglamol 99(R),2 chromatographic systems were developed, i.e., a reversed-phase (RP) system on RP2 plates using an acetonitrile-based mobile phase and a normal-phase system on silica gel 60 plates using a toluene-based gradient. Densitometry was performed by absorption measurement at 220 nm. Repeatabilities (relative standard deviation, n = 6) between 2.2 and 5.5% and correlation coefficients >0.9973 were highly satisfactory for the analysis of these additives in the mineral oil. Primuline reagent was used to improve the detection limit of the lipophilic additives by a factor of 2, followed by fluorescence measurement at UV 366/>400 nm. For rapid identification by ATR-IR and FTIR, the respective additive zones on the plate were online extracted by an interface called ChromeXtract, concentrated, and directly applied for measurements in the wave number range of 4000-400 cm(-1). Identification was confirmed by online ESI-MS within a minute using ChromeXtract and by DART-MS within seconds.

Harvard-Zitierstil: Dytkiewitz, E. and Morlock, G. (2008) Analytical strategy for rapid identification and quantification of lubricant additives in mineral oil by high-performance thin-layer chromatography with UV absorption and fluorescence detection combined with mass spectrometry and infrared spectroscopy, Journal of AOAC INTERNATIONAL, 91(5), pp. 1237-1243. https://aoac.publisher.ingentaconnect.com/contentone/aoac/jaoac/2008/00000091/00000005/art00035

APA-Zitierstil: Dytkiewitz, E., & Morlock, G. (2008). Analytical strategy for rapid identification and quantification of lubricant additives in mineral oil by high-performance thin-layer chromatography with UV absorption and fluorescence detection combined with mass spectrometry and infrared spectroscopy. Journal of AOAC INTERNATIONAL. 91(5), 1237-1243. https://aoac.publisher.ingentaconnect.com/contentone/aoac/jaoac/2008/00000091/00000005/art00035