Supercritical fluid extraction as a preparative tool for strawberry aroma analysis

To improve the aroma characterization of various strawberry cultivars, we tested supercritical fluid extraction (SFE) to determine its suitability for the extraction of aroma compounds from fresh fruit, comparing SFE results with traditional solvent extraction with dichloromethane. Using SFE it was possible to recover the majority of the aroma compounds which can be also found in the solvent extract; patterns related to variety and degree of maturation were preserved. Our results showed, however, that SFE is more selective and was able to recover the ‘character impact’ compound of wild strawberry. Our findings from the odor analysis of furaneol standard emphasize the importance of using a more selective extraction procedure, and always combining instrumental detection with sensory analysis.     

High transverse momentumη production in π− p, π+ p,andpp interactions at 280 GeV/c

The inclusive cross sections for η production by the interactions of 280 GeV/c momentum π^?, π⁺, and proton beams in hydrogen have been measured. The kinematical range covered is ?0.45<x _F <0.45, and 4.0<P _T <7.0 GeV/c for Feynmanx _F and transverse momentum respectively. The η to π⁰ cross section ratios are given for the three reactions. The ratio of π^? p to π⁺ p cross sections for η production in the above kinematic ranges is 1.22±0.08±0.11.     

Ion chromatography determination of trace level bromate by large volume injection with conductivity and spectrophotometric detection after post column derivatisation

Bromate is a well known by-product produced by the ozonisation of drinking water; the allowed concentration for human consumption has to be regulated to the low microg l(-1) range. A direct injection, ion chromatographic method was developed using a tetraborate eluent with serially connected conductivity and spectrophotometric detection. Bromate was detected after post-column reaction with fuchsin at 520 nm. Sample capacity was investigated by injecting large volumes (up to 6 ml) using a high total hardness and chloride tap water. Linear correlation of bromate response with volumes from 1 ml to 6 ml was demonstrated, the main limitation being the overlapping of the chloride peak with bromate. Up to 1.5 ml sample can be injected without any pre-treatment. With more than 1.5 ml injection volume, a sample pre-treatment with a cartridge in Ag and H form, followed by a 10 min degassing in an ultrasonic bath, was needed. This method was validated by analysing secondary reference materials and real samples from a drinking water treatment plant. The method was linear from the limit of quantification to 20 microg l(-1). Reproducibilities in tap water were 18% (5 microg l(-1), n=12) and 21% (1 microg l(-1), n=4) respectively for 1.5 and 6 ml injection volumes with conductivity detection, and 17% at 0.5 microg l(-1) (n=9) with spectrophotometric detection. Calculated detection limits were 0.5 microg l(-1) (6 ml) ahd 2 microg l(-1) (1.5 ml) for conductivity detection and 0.3 microg l(-1) (1.5 ml) for spectrophotometric detection.     

Ion chromatography performances evaluated from the third AQUACON freshwater analysis interlaboratory exercise

This paper describes a collaborative interlaboratory exercise for freshwater analysis held in the framework of the Analytical Quality Control and Assessment Studies in the Mediterranean Basin Project (AQUACON). Two sample types were prepared and distributed: the first for the analysis of pH, conductivity and major ions (calcium, magnesium, sodium, potassium, chloride, sulphate, bicarbonate) and the second for algal nutrients (ammonium, nitrate, phosphate, total phosphorus and total nitrogen, silicate). Two solutions with different concentration levels were prepared for each of the samples; homogeneity throughout bottles and stability of samples in time were tested from the two organising laboratories. Results were obtained from 155 laboratories from 30 countries around the world. A detailed examination of results obtained by ion chromatography showed that an important source of error was the neglect of the non-linearity of calibration curves. Repeatability and reproducibility tests were performed in a selected number of experienced laboratories in accordance with the ISO standard 5725 for anion and cation ion chromatography determination. The best obtainable repeatability and reproducibility limits of IC methods of water analysis are about 5 and 10%, respectively.Presented at BERM-9—Ninth International Symposium on Biological and Environmental Reference Materials, June 15–19, 2003, Berlin, Germany.     

Production of high transverse momentum prompt photons and neutral pions in proton-proton interactions at 280 GeV/c

The inclusive cross sections for production of prompt photons and π⁰ s by 280 GeV/c protons incident on a liquid hydrogen target, have been measured forp _T in the range 4.0 to 6.5 GeV/c and for |x _F |<0.45. A quantitative comparison of the prompt photon cross section with next-to-leading order QCD predictions using Duke and Owens structure functions is performed. Phenomenological fits to the π⁰ and prompt photon cross sections are given.     

HPLC separation and fluorimetric estimation of chlorophylls and pheophytins in fresh and frozen peas

Summary A HPLC method for the separation and estimation of chlorophylls and pheophytins in fresh and frozen peas was assessed with the aim of following the colour changes of the products during storage under frozen conditions.The method involves the acetone extraction of the pigments, followed by HPLC on RP18 with isocratic elution by acetone: ethanol:water, (70:17:13), detecting and estimating the separated compounds by fluorimetry. The mobile phase composition was selected by monitoring the separation efficiency of several mixtures of solvents by HPLC. The reliability and the accuracy of the method were checked.     

Determination of endocrine disrupting chemicals in environmental solid matrices by extraction with a non-ionic surfactant (Tween 80)

A readily applicable method based on extraction by aqueous non-ionic surfactant solutions (Tween 80) and RP-HPLC coupled to fluorescence detection, has been developed for the simultaneous determination of the phenolic endocrine disrupting chemicals (EDCs) nonylphenol (NP), nonylphenol monoethoxylate (NP1EO) and nonylphenol diethoxylate (NP2EO) and bisphenol A (BPA) in environmental solid matrices. Clean up of sample extracts was performed on Si-C18 solid phase extraction (SPE) cartridges. The overall Tween 80 extraction-SPE-RP-HPLC procedure was validated for accuracy and precision by analyzing sediment samples spiked with known amounts of EDCs. Recoveries for NP, NP1EO, NP2EO and BPA and limits of detection are in agreement with conventional extraction methods. The developed methodology was successfully applied to the analysis of target compounds in Italian river sediments, river suspended matter and benthonic macroinvertebrate organisms (oligochaetes Lumbriculus variegatus). Results confirmed that this relatively simple procedure performed satisfactorily in the determination of phenolic EDCs in environmental solid matrices of different complexity and that it can be a suitable alternative method to conventional systems even for routine analyses.     

Determination of 4-nonylphenol and 4-nonylphenol ethoxylates in river sediments by microwave assisted solvent extraction

The efficiency of Microwave Assisted Solvent Extraction (MASE) for the simultaneous determination of nonylphenol (NP) and nonylphenol ethoxylates (NPE) in river sediments has been evaluated. An optimisation study was carried out in order to identify the variables having the greatest influence on the extraction efficiency. The comparison between the solvents (methanol and acetone-hexane 1:1) shows that the more polar solvent (i.e. methanol) allows a more effective extraction of NP and NPE from sediments. Analytical results show that there is not a considerable improvement by doubling extraction time, while the increase of solvent volume is significant. The comparative study with Soxhlet and pressurised liquid extraction (PLE) methods demonstrates that Microwave Assisted Solvent Extraction is a suitable alternative extraction method for the 4-NP and 4-NPE determination in river sediments, showing an accuracy and precision comparable to those obtained with PLE and better than those obtained with Soxhlet.     

Determination of total dissolved inorganic carbon in freshwaters by reagent-free ion chromatography

Studies of inorganic carbon cycle in natural waters provide important information on the biological productivity and buffer capacity. Determination of total inorganic carbon, alkalinity and dissolved carbon dioxide gives an indication of the balance between photosynthesis and respiration by biota, both within the water column and sediments, and carbon dioxide transfers from the water column to the atmosphere. There are few methods to measure and distinguish the different forms of inorganic carbon, but all require a measure or an indirect quantification of total inorganic carbon. A direct measurement of TIC in water is made possible by the introduction of electrolytic generated hydroxide eluent in ion chromatography which allows to detect a chromatographic peak for carbonate. The advantage of this method is that all the inorganic forms of carbon are converted in carbonate at eluent pH and can be detected as a single peak by conductivity detection. Repeatability of carbonate peak was evaluated at different levels from 0.02 to 6 mequiv.l(-1) both in high purity water and in real samples and ranged from 1 to 9%. The calibration curve was not linear and has to be fitted by a quadratic curve. Limit of detection was estimated to be 0.02 mequiv.l(-1). Accuracy has been estimated by comparing ion chromatography method with total inorganic carbon calculated from alkalinity and pH. The correlation between the two methods was good (R(2)=0.978, n=141). The IC method has been applied to different typologies of surface waters (alpine and subalpine lakes and rivers) characterised by different chemical characteristics (alkalinity from 0.05 to 2 mequiv.l(-1) and pH from 6.7 to 8.5) and low total organic carbon concentrations. This analytical method allowed to describe the distribution of TIC along the water column of two Italian deep lakes.