A novel analytical approach for the determination of ethylene-thiourea and propylene-thiourea in vegetal foodstuffs by high-performance liquid chromatography hyphenated to inductively coupled plasma-tandem mass spectrometry.

This study reports a novel analytical approach for the simultaneous determination of ethylene-thiourea (ETU) and propylene-thiourea (PTU) in fruits and vegetables by (reverse phase) high-performance liquid chromatography (HPLC) coupled to inductively coupled plasma-tandem mass spectrometry (ICP-QQQMS or ICP-MS/MS). A baseline separation of ETU and PTU was achieved in less than 5 min. A robust method validation by using the accuracy profile approach was performed by carrying out four measurement series in duplicate at six different levels over a timespan of 4 weeks (different days). The recovery factors ranged from 87 to 101% for ETU and from 98 to 99% for PTU (depending on the spiking level). The coefficient of variation in terms of repeatability (CVr) ranged from 1 to 4.7% for ETU and from 1.8 to 3.9% for PTU (depending also on the analyte level) while the coefficient of variation in terms of intermediate reproducibility (CVR) ranged from 3.4 to 10% for ETU and from 1.8 to 10.8% for PTU. The limit of quantification was 0.022 mg kg-1 (wet weight) for ETU and 0.010 mg kg-1 (ww) for PTU. This novel approach was proved to be highly robust and suitable for the determination of ETU and PTU in foodstuffs of vegetal origin.

Carbon Nanotubes Covalently Attached to Functionalized Surfaces Directly through the Carbon Cage.

The covalent attachment of nonfunctionalized and carboxylic acid-functionalized carbon nanotubes to amine-terminated organic monolayers on gold and silicon surfaces is investigated. It is well established that the condensation reaction between a carboxylic acid and an amine is a viable method to anchor carbon nanotubes to solid substrates. The work presented here shows that the presence of the carboxylic group on the nanotube is not required for attachment to occur, as direct attachment via the substrate amine and the nanotube cage can take place. Scanning and transmission electron microscopy and atomic force microscopy confirm the presence of carbon nanotubes in intimate contact with the surface. X-ray photoelectron spectroscopy is utilized to compare the surface chemistry of the functionalized and nonfunctionalized carbon nanotubes and is supported by a computational investigation. Ion fragments attributed to the direct attachment between the surface and carbon nanotube cage are detected by time-of-flight secondary ion mass spectrometry. The overall attachment scheme is evaluated and can be further used on multiple carbonaceous materials attached to solid substrates.