A total analytical system featuring a novel solid-liquid extraction chamber for solid sample flow analysis.

In this work, a total flow analysis system based on a novel solid-liquid extraction chamber is presented. This strategy enables all the main experimental procedures for the analysis of a solid sample to be performed automatically: enrichment of the liquid extract, sample treatment, filtration of the liquid extract from the solid sample, directing the extract towards detection, and finally cleansing of the chamber for the following solid sample to be analyzed. The chamber designed to be incorporated in the flow manifold presents two main features: it accommodates stirring bars for enhancing the extraction process, and it presents replaceable solid sample containers (a spare part of the solid-liquid extraction chamber) to easily replace the solid sample and therefore enhance sample analysis throughput. The chamber performance was assessed using two different solid samples, an ion exchanger resin and vegetable samples, focussing on proton and nitrate ion extraction, respectively. The main figures of merit achieved were relative standard deviation (RSD) and relative error values below 7 % for all determinations. The determination rate for vegetable samples was ca. 12 samples h-1. The proposed strategy may be exploited to perform automatically the analysis of solid samples as it embodies a simple automatic strategy of a very important but time-consuming and laborious analytical operation. Graphical abstract TAS for solid liquid extraction and nitrate potentiometric determination of vegetable samples.

Standard addition flow method for potentiometric measurements at low concentration levels: application to the determination of fluoride in food samples.

A standard addition method was implemented by using a flow manifold able to perform automatically multiple standard additions and in-line sample treatment. This analytical strategy was based on the in-line mixing of sample and standard addition solutions, using a merging zone approach. The flow system aimed to exploit the standard addition method to quantify the target analyte particularly in cases where the analyte concentration in the matrix is below the lower limit of linear response of the detector. The feasibility of the proposed flow configuration was assessed through the potentiometric determination of fluoride in sea salts of different origins and different types of coffee infusions. The limit of quantification of the proposed manifold was 5×10(-6) mol L(-1), 10-fold lower than the lower limit of linear response of the potentiometric detector used. A determination rate of 8 samples h(-1) was achieved considering an experimental procedure based on three standard additions per sample. The main advantage of the proposed strategy is the simple approach to perform multiple standard additions, which can be implemented with other ion selective electrodes, especially in cases when the primary ion is below the lower limit of linear response of the detector.

Fourier transform near-infrared spectroscopy application for sea salt quality evaluation.

Near-infrared (NIR) spectroscopy in diffuse reflectance mode was explored with the objective of discriminating sea salts according to their quality type (traditional salt vs "flower of salt") and geographical origin (Atlantic vs Mediterranean). Sea salts were also analyzed in terms of Ca(2+), Mg(2+), K(+), alkalinity, and sulfate concentrations to support spectroscopic results. High concentrations of Mg(2+) and K(+) characterized Atlantic samples, while a high Ca(2+) content was observed in traditional sea salts. A partial least-squares discriminant analysis model considering the 8500-7500 cm(-1) region permitted the discrimination of salts by quality types. The regions 4650-4350 and 5900-5500 cm(-1) allowed salts classification according to their geographical origin. It was possible to classify correctly 85.3 and 94.8% of the analyzed samples according to the salt type and to the geographical origin, respectively. These results demonstrated that NIR spectroscopy is a suitable and very efficient tool for sea salt quality evaluation.

Method for analysis dried vine fruits contaminated with ochratoxin A.

The EU maximum limit of 10 microg kg(-1) of OTA for dried vine fruits has been established since 2002 (European Commission, 2005). The presented work explore the capability of using Fourier infrared spectroscopy attenuated total reflection (FTIR-ATR) for the detection of ochratoxin A (OTA) in dried vine fruits in a range of concentration between 2 and 50 microg kg(-1) OTA. The method developed included a sample pretreatment using a C18 cartridge which was efficient for the isolation of the mycotoxin. The PLS1 analysis of the spectrum of sultanas spiked with different OTA concentrations showed a good correlation between the spectral data and reference concentration for OTA (R(2)=0.85).

FTIR-ATR infrared spectroscopy for the detection of ochratoxin A in dried vine fruit.

A method of screening sultanas for ochratoxin A (OTA) contamination, using mid-infrared spectroscopy/Golden Gate single-reflection ATR (attenuated total reflection), is described. The main spectral characteristics of sultanas from different sources were identified in a preliminary acquisition and spectral analysis study. Principal component analysis (PCA) showed that samples of various origins had different spectral characteristics, especially in water content and the fingerprint region. A lack of reproducibility was observed in the spectra acquired on different days. However, spectral repeatability was greatly improved when water activity of the sample was set at 0.62. A calibration curve of OTA was constructed in the range 10-40 microg OTA kg(-1). Samples with OTA levels higher than 20 microg kg(-1) were separated from samples contaminated with a lower concentration (10 microg OTA kg(-1)) and from uncontaminated samples. The reported methodology is a reliable and simple technique for screening dried vine fruit for OTA.