Applications of micro-fluidic platforms integrating packed stationary phases

To design and fabricate novel centrifugal micro-fluidic platforms integrating packed stationary phases for solid-phase micro-extraction in a wide range of (bio)analytical applications. To design and fabricate novel micro-fluidic platforms integrating packed stationary phases capable of withstanding significant high pressures

Microextraction of Xenobiotics and Biomolecules from Different Matrices on Nano Structures

Sample preparation is the backbone of any analytical procedure; it involves extraction and pre-concentration of the desired analytes; often at trace levels. The present article describes the applications of nanomaterials (carbon based inorganic and polymeric materials) in miniaturized extraction such as solid phase micro-extraction, stir-bar sorptive extraction, liquid phase micro-extraction, and dispersive liquid phase micro-extraction in the analyses of aqueous samples. The nanoparticles used for micro-extractions are discussed on the basis of their chemical natures. The synthetic route and the preparation of nanomaterials are described along with the optimization strategies for micro-extraction. A comparison between the conventional materials and nanomaterials for micro-extraction is proposed. The key roles of the nanomaterials for the micro-extraction of different analytes such as drugs, pesticides, polycyclic aromatic hydrocarbons, proteins and peptides from aqueous samples are reported. The use of nanomaterials, combined with miniaturized micro-extraction techniques, proved to be highly promising for sample preparation of various matrices with analytes at trace levels

Magnetic micro-solid-phase extraction based on magnetite-MCM-41 with gas chromatography–mass spectrometry for the determination of antidepressant drugs in biological fluids

A new facile magnetic micro‐solid‐phase extraction coupled to gas chromatography and mass spectrometry detection was developed for the extraction and determination of selected antidepressant drugs in biological fluids using magnetite‐MCM‐41 as adsorbent. The synthesized sorbent was characterized by several spectroscopic techniques. The maximum extraction efficiency for extraction of 500 μg/L antidepressant drugs from aqueous solution was obtained with 15 mg of magnetite‐MCM‐41 at pH 12. The analyte was desorbed using 100 μL of acetonitrile prior to gas chromatography determination. This method was rapid in which the adsorption procedure was completed in 60 s. Under the optimized conditions using 15 mL of antidepressant drugs sample, the calibration curve showed good linearity in the range of 0.05–500 μg/L (r2 = 0.996–0.999). Good limits of detection (0.008–0.010 μg/L) were obtained for the analytes with good relative standard deviations of <8.0% (n = 5) for the determination of 0.1, 5.0, and 500.0 μg/L of antidepressant drugs. This method was successfully applied to the determination of amitriptyline and chlorpromazine in plasma and urine samples. The recoveries of spiked plasma and urine samples were in the range of 86.1–115.4%. Results indicate that magnetite micro‐solid‐phase extraction with gas chromatography and mass spectrometry is a convenient, fast, and economical method for the extraction and determination of amitriptyline and chlorpromazine in biological samples

n-Aldehydes ( C 6 - C 10 ) in snow samples collected at the high alpine research station Jungfraujoch during CLACE 5

Samples of freshly fallen snow were collected at the high alpine research station Jungfraujoch, Switzerland, during the Cloud and Aerosol Characterization Experiments (CLACE) 5 in February and March 2006. Sampling was carried out on the Sphinx platform. Headspace-solid-phase-dynamic extraction (HS-SPDE) combined with gas chromatography/mass spectrometry (GC/MS) was used to quantify C6–C10 n-aldehydes in the snow samples. The most abundant n-aldehyde was n-hexanal (median concentration 1.324 micro g L -1) followed by n-nonanal, n-decanal, n-octanal and n-heptanal (median concentrations 1.239, 0.863, 0.460, and 0.304 micro g L -1, respectively). A wide range of concentrations was found among individual snow samples, even for samples taken at the same time. Higher median concentrations of all n-aldehydes were observed when air masses reached Jungfraujoch from the north-northwest in comparison to air masses arriving from the southeast-southwest. Results suggest that the n-aldehydes detected most likely are of direct and indirect biogenic origin, and that they entered the snow through the particle phase

Concentrations of higher dicarboxylic acids C5 – C13 in fresh snow samples collected at the High Alpine Research Station Jungfraujoch during CLACE 5 and 6

Samples of freshly fallen snow were collected at the high alpine research station Jungfraujoch (Switzerland) in February and March 2006 and 2007, during the Cloud and Aerosol Characterization Experiments (CLACE) 5 and 6. In this study a new technique has been developed and demonstrated for the measurement of organic acids in fresh snow. The melted snow samples were subjected to solid phase extraction and resulting solutions analysed for organic acids by HPLC-MS-TOF using negative electrospray ionization. A series of linear dicarboxylic acids from C5 to C13 and phthalic acid, were identified and quantified. In several samples the biogenic acid pinonic acid was also observed. In fresh snow the median concentration of the most abundant acid, adipic acid, was 0.69 micro g L -1 in 2006 and 0.70 micro g L -1 in 2007. Glutaric acid was the second most abundant dicarboxylic acid found with median values of 0.46 micro g L -1 in 2006 and 0.61 micro g L -1 in 2007, while the aromatic acid phthalic acid showed a median concentration of 0.34 micro g L -1 in 2006 and 0.45 micro g L -1 in 2007. The concentrations in the samples from various snowfall events varied significantly, and were found to be dependent on the back trajectory of the air mass arriving at Jungfraujoch. Air masses of marine origin showed the lowest concentrations of acids whereas the highest concentrations were measured when the air mass was strongly influenced by boundary layer air

Applicability of head space solid phase microextraction (HS-SPME) with polyethylene glycol (PEG) fibre for GC-MS determination of volatile fatty acids in aqueous samples

A method consisting of head-space solid phase micro extraction (HS-SPME) followed by gas chromatography coupled with mass spectrometry (GC-MS) was developed for determination of volatile fatty acids in wastewater. A new fibre polyethylene glycol (PEG) was evaluated for the sample preparation. This fibre is designed to show high sample capacity, faster mass transfer during extraction, shorter equilibrium times and faster desorption process. The developed method showed good sensitivity with comparable limit of detection (LOD) and limit of quantitation (LOQ) values. The selection of various parameters included extraction time, extraction temperature, sample volume and desorption conditions. The experimental results showed low detection limits ranging between 0.01 mg/L to 0.06 mg/L for different acids. The new fibre was found to be efficient towards acetic and propionic acid

A field based method for pre-concentration of micro organics using solid phase extraction

British Geological Survey (BGS) have been researching micro-organic pollutants for many years in the UK (Gooddy et al 2004, Stuart et al 2012, White et al 2016) and overseas (Sorensen et al 2015). A hindrance to the research, especially overseas, has been the need to transport large volumes of water back to the laboratory and the worry of degradation during transportation prior to LCMS or GCMS analysis. The first step in the LCMS analytical procedure is the solid phase extraction of the micro-organic contaminants onto a small cartridge. This report details the field trial where by BGS, working in conjunction with NLS, carried out the pre-concentration step of sample processing in the field. NLS provided pre-conditioned sorbent Oasis® HLB cartridges supplied in sealed Corning centristar centrifuge tubes. Water samples were run through the cartridges by the field team using a small peristaltic pump prior to sending to NLS for semi-quantative broad screen LCMS analysis. To check the repeatability and the stability of this method the sorbed samples were analysed in duplicate and replicate analysis was carried out over set periods after storage for up to a month. The results from the duplicate replicates are compared to results from the original water sample analysed immediately after sampling. Laboratory and field equipment blanks were included in the trial to check for any contamination introduced by the sampling method and extraction process. Preliminary results demonstrate that for a large range of compounds, and different types of matrices, this method was able to preserve samples for up to a month. Once the procedure had been validated, it was used to investigate the occurrence of micro-pollutants in a rural groundwater, estuarine waters and a range of surface waters receiving treated sewerage outflows. The work was funded under the BGS Development Capabilities programme, and was also supported by the BGS Groundwater Science programme under the Groundwater Protection team. Analytical aspects of this work was undertaken in collaboration with Wayne Civil based at Star Cross National Science Laboratory (NLS)

An easily prepared graphene oxide-ionic liquid hybrid nanomaterial for micro-solid phase extraction and preconcentration of Hg in water samples

A preconcentration method based on the use of graphene oxide (GO) functionalized with an ionic liquid (IL) was developed for trace Hg determination in water samples. The IL-GO hybrid nanomaterial was prepared by a simple procedure to functionalize GO with the IL 1-butyl-3-dodecylimidazolium bromide ([C4C12im]Br) and its performance as a sorption material for Hg was evaluated. A microcolumn filled with the IL-GO nanomaterial was used for preconcentration and determination of Hg followed by electrothermal atomic absorption spectrometry (ETAAS) detection. Mercury was retained at pH 5.0 and 20% (v/v) HNO3 was used for the elution of Hg from the microcolumn. The effects of different variables, including the sample volume, extraction time, sample flow rate, type and concentration of eluent and eluent flow rate were carefully studied. High retention efficiency (100%) was achieved with the proposed IL-GO sorption nanomaterial without the need for additional chelating reagents or derivatization reagents, which is an important advantage compared with traditional preconcentration methods. A sensitivity enhancement factor of 100 and a low detection limit of 14 ng L-1 were obtained under optimal experimental conditions. The proposed method can be considered as a simple, cost-effective and efficient alternative for Hg determination in water samples like river, rain, mineral and tap water.Fil: Cruz Sotolongo, Annaly. Consejo Nacional de Investigaciones Científicas y Técnicas; Argentina. Universidad Nacional de Cuyo; ArgentinaFil: Martinis, Estefanía Mabel. Consejo Nacional de Investigaciones Científicas y Técnicas; Argentina. Universidad Nacional de Cuyo; ArgentinaFil: Wuilloud, Rodolfo German. Consejo Nacional de Investigaciones Científicas y Técnicas; Argentina. Universidad Nacional de Cuyo; Argentin