The primary goal of the present study is the inter-laboratory evaluation of a thin film microextraction (TFME) technique to be used as an alternative approach to liquid-liquid extraction (LLE). Polydimethylsiloxane/divinylbenzene (PDMS/DVB) and PDMS/DVB-carbon mesh supported membranes were used for the extraction of 23 targeted pesticides, while a thermal desorption unit (TDU) was employed to transfer these analytes to a GC/MS instrument for separation and detection. After optimization of the most critical parameters, both membranes were capable of achieving limits of detection (LOD) in the low ng L range while demonstrating excellent robustness, withstanding up to 100 extractions/desorption cycles.
View Article and Find Full Text PDFIn chemical analysis, sample preparation is frequently considered the bottleneck of the entire analytical method. The success of the final method strongly depends on understanding the entire process of analysis of a particular type of analyte in a sample, namely: the physicochemical properties of the analytes (solubility, volatility, polarity etc.), the environmental conditions, and the matrix components of the sample.
View Article and Find Full Text PDFA temperature-controlling device for in-tube solid-phase microextraction was developed based on thermoelectric cooling and heating. This device can control the temperature of the capillary column from 0 to 100°C by applying a voltage to a Peltier cooler or stainless steel tube. The extraction temperatures for angiotensin I, propranolol, and ranitidine were optimized.
View Article and Find Full Text PDFA fully automated, high-throughput method based on thin-film solid-phase microextraction (SPME) and liquid chromatography-mass spectrometry was developed for simultaneous quantitative analysis of 110 doping compounds, selected from ten classes and varying in physical and chemical properties. Among four tested extraction phases, C18 blades were chosen, as they provided optimum recoveries and the lowest carryover effect. The SPME method was optimized in terms of extraction pH, ionic strength of the sample, washing solution, extraction and desorption times for analysis of urine samples.
View Article and Find Full Text PDFThis article discusses comparison of microextraction versus exhaustive extraction approaches for simultaneous extraction of compounds in wide range of polarity at low and high volumes of sample by comparing solid phase extraction (SPE) and solid phase microextraction (SPME). Here, both systems are discussed theoretically and evaluated based on experimental data. Experimental comparisons were conducted in terms of extraction recovery, sensitivity, and selectivity for the extraction of doping agent compounds (logP: 0.
View Article and Find Full Text PDFThe use of thin-film solid-phase microextraction (SPME) as the sampling preparation step before direct analysis in real time (DART) was evaluated for the determination of two prohibited doping substances, cocaine and methadone, in urine samples. Results showed that thin-film SPME improves the detectability of these compounds: signal-to-blank ratios of 5 (cocaine) and 13 (methadone) were obtained in the analysis of 0.5 ng/ml in human urine.
View Article and Find Full Text PDFWithin the family of polycyclic aromatic hydrocarbons (PAHs), nitrated derivatives are of particular interest in environmental science because they have well-known carcinogenic and mutagenic effects. They are in fact more toxic than their parent PAHs. One valuable diagnosis of atmospheric pollution can be obtained using biomonitors such as mosses.
View Article and Find Full Text PDFJ Chromatogr A
June 2012
A method consisting of multiple headspace solid-phase microextraction followed by gas chromatography-mass spectrometry analysis was developed and used to determine the main volatile radiolysis products formed by γ-irradiation of flexible multilayer food packaging samples. The developed method allows the use of solid-phase microextraction in the quantification of compounds from plastic solid samples. A screening of volatiles in the γ-irradiated and non-irradiated films was performed and 29 compounds were identified in the irradiated packaging, 17 of which were absent in the non-irradiated samples.
View Article and Find Full Text PDFA new active paraffin coating for paper and board was evaluated for antimicrobial protection and decay retardation for cherry tomatoes. Different active agents were evaluated against Alternaria alternata fungus both in vitro and in vivo using artificially inoculated cherry tomatoes. Bark cinnamon and oregano essential oil showed the best performance (versus clove and leaf cinnamon essential oils) when incorporated to active paper or board used for packaging at nominal concentrations of 3 and 6% (w/w), respectively.
View Article and Find Full Text PDFThe efficiency of photo-oxidation, chemical oxidation by sodium hypochlorite, and ozonization for the industrial-scale removal of volatile organic compounds (VOCs) and odors from gaseous emissions was studied by applying these treatments (in an experimental system) to substances passing through an emission stack of a factory producing maize derivatives. Absorption and ozonization were the most efficient treatment, removing 75% and 98% of VOCs, respectively, while photo-oxidation only removed about 59%. The emitted chemical compounds and odors were identified and quantified by gas chromatography-mass spectrometry (in full-scan mode).
View Article and Find Full Text PDFAutomated headspace solid-phase microextraction (HS-SPME) and hollow-fibre liquid-phase microextraction (HFLPME) methods for the determination of 15 active chemicals released from essential-oil-based active packaging have been considered. The HS-SPME procedure demonstrates good performance and was therefore optimised and validated, providing detection limits in the low microgram per kilogramme range and wide and convenient linear ranges from 40.0 to 900.
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