The ways to the trace level analysis in infrared spectroscopy

The future of infrared (IR) spectroscopy as an analytical technique is assured due to its versatility and its numerous advantages; such as the possibility to obtain molecular specific information for virtually any sample in any state with no treatment or minimal sample preparation. However, spectroscopists are not satisfied with relegating IR spectroscopy just to major and minor component analysis and have been looking at analysis at the trace level too. This review is the recognition of the brilliant research performed during the past two decades and the advances achieved in this area, which have made possible the analysis of contaminants at parts per billion (ppb) levels by IR in differen…

Elemental fingerprint of wines from the protected designation of origin Valencia

Abstract Inductively coupled plasma optical emission (ICP-OES), in combination with different chemometric approaches, has been used to verify the origin of different red wine samples from Utiel-Requena, Jumilla, Yecla and Valencia protected designation of origin (PDO). The ability of multivariate analysis methods, such as hierarchical cluster analysis (HCA), principal component analysis (PCA), classification and regression trees (CARTs) and discriminant analysis (DA), to achieve wine classification from their elemental contents has been investigated. The calculations were performed using 38 variables (contents of Al, Ba, Be, Ca, Cd, Ce, Co, Cr, Cu, Dy, Er, Eu, Fe, Gd, Ho, K, La, Li, Lu, Mg,…

Elemental composition of seasoning products

The elemental composition of seasoning products, like spices garlic and onion, has been reviewed paying special attention to methods proposed in the literature to determine specific elements or as much as possible components of these products which are widespread used in food preservation or food flavouring and can contribute to the intake of both, essential and toxic elements. Sample treatment and metal speciation aspects have been critically revised concerning onion, garlic and pepper (the most commonly studied products).

Determination at low ppm levels of dithiocarbamate residues in foodstuff by vapour phase-liquid phase microextraction-infrared spectroscopy

Abstract A methodology based on the vapour phase (VP) generation of carbon disulphide from non-volatile dithiocarbamate compounds has been developed for determination of pesticide residues in foodstuff at low ppm levels. The method involves a selective reaction combined with liquid phase microextraction (LPME) and transmission infrared measurements. The use of a home made transmission cell improved the detection limits (LOD) compared to the use of attenuated total reflectance measurements by a factor of approximately 80. Using the most appropriate experimental conditions for the CS2 generation and LPME preconcentration, the precision of the methodology, expressed as the relative standard de…

Trace elemental composition of curry by inductively coupled plasma optical emission spectrometry (ICP-OES)

A methodology based on inductively coupled plasma optical emission spectrometry (ICP-OES) after microwave-assisted acid digestion was developed to determine the content of traces elements in curry samples from the Spanish market. The methodology was validated in terms of accuracy by the analysis of citrus and tomato leaf reference materials achieving comparable results with the certified values. The trace metal content of curry samples was compared with data available from previously published reports concerning Indian samples, especially in terms of heavy metal composition, in order to guarantee the quality of the commercially available spices in the European countries. Values found for th…

Non-chromatographic speciation of inorganic arsenic in mushrooms by hydride generation atomic fluorescence spectrometry

Abstract A non-chromatographic speciation method has been developed for the determination of inorganic arsenic in cultivated and wild mushroom samples from different origins. The ultrasound-assisted extraction of the toxic arsenic species As (III) and As (V) was performed for 10 min with 1 mol l −1 H 3 PO 4 and 0.1% (m/v) Triton X-100. After phase separation the residue was washed with 0.1% (w/v) EDTA and centrifuged. As (III) and As (V) were determined by hydride generation atomic fluorescence spectrometry. Speciation was made using proportional equations corresponding to two different measurement conditions, (i) directly feeding sample extracts diluted with HCl and (ii) after reduction wi…

Inductively coupled plasma optical emission spectroscopy determination of trace element composition of argan oil.

A methodology based on inductively coupled plasma optical emission spectroscopy (ICP-OES) after microwave assisted acid digestion has been developed to determine the trace element content of Moroccan argan oil. Limit of detection values equal or lower than few mg/kg were obtained for all elements under study. To assure the accuracy of the whole procedure, recovery studies were carried out on argan oil samples spiked at different concentration levels from 10 to 200 µg/L. Quantitative average recovery values were obtained for all elements evaluated, demonstrating the suitability of this methodology for the determination of trace elements in argan oil samples. Aluminum, calcium, chromium, iro…

Selenium and heavy metals content in some Mediterranean soils

Abstract The study of metal contents in industrial, agricultural or/and polluted soils compared with natural or unpolluted soils is currently necessary to obtain reference values and to assess soil contamination. Nonetheless, very few works published appear in international journals on elements like Se, Li and Sr in Spanish soils. This study determines the total levels of Se, Li, Sr, As, Cd, Co, Cr, Cu, Ni, Pb, V, Zn, Fe, Mn and Ba in 14 natural (unpolluted) soils (Gypsisols, Leptosols, Arenosols and Acrisols), 14 agricultural soils (Anthrosols, Fluvisols and Luvisols), and 4 industrial–urban affected-surface soil horizons (Anthrosols and Fluvisols) of Eastern Spain. The geochemical baselin…

Non-chromatographic speciation

We evaluate the main strategies for screening trace-element species in most types of sample to establish their strengths and weaknesses, as they offer fast, sensitive and cheaper alternatives to classical methods involving chromatography. We consider the principles of non-chromatographic speciation analysis, based on the different behaviors of chemical species before measurement by atomic and molecular spectrometry and electroanalytical methods, so as to give an update on the literature in this field of research.

Searching the most appropriate sample pretreatment for the elemental analysis of wines by inductively coupled plasma-based techniques.

Different sample preparation methods were evaluated for the simultaneous multielement analysis of wine samples by inductively coupled plasma optical emission spectrometry (ICP-OES) and inductively coupled plasma mass spectrometry (ICP-MS). Microwave-assisted digestion in closed vessel, thermal digestion in open reactor, and direct sample dilution were considered for the determination of Li, Be, Na, Mg, Al, K, Ca, Sc, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, As, Se, Sr, Y, Mo, Cd, Ba, La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu, Tl, Pb, and Bi in 12 samples of red wine from Valencia and Utiel-Requena protected designation of origin. ICP-MS allows the determination of 17 elements in most…

Basic Chemometric Tools

Abstract The authentication of protected designation of origin and other protected geographical indications for foods involves the need for a deep knowledge of these kinds of samples and the correct identification of appropriate markers that are suitable to be used for authentication purposes. For this, significance tests must be developed and applied to provide evidence in a fast and accurate way; from this, it seems clear that advances in analytical tools, to obtain data regarding food chemical composition, and chemometric data treatments must be continued to provide to the users powerful identification methodologies. In this sense, the objective must be to differentiate between foods pro…

Trace-element composition and stable-isotope ratio for discrimination of foods with Protected Designation of Origin

We review the literature on authentication of foods with Protected Designation of Origin (PDO) from their trace-element composition or stable-isotope ratios in order to evaluate the state of the art of this field and to identify the main parameters of analytical techniques and chemometric-data treatments that permit accurate discrimination of samples of different geographical origins and with different characteristics.

Mineral content of seasonings, salt and vinegar

Geographical traceability of “Arròs de Valencia” rice grain based on mineral element composition

The geographical traceability of rice grain samples involves the use of analytical methodologies that allow their differentiation on the basis of the rice composition, thus confirming their authenticity. In this paper, trace element determination of rice samples by inductively coupled plasma optical emission spectroscopy (ICP-OES) has been addressed to achieve a complete geographical origin classification. Samples (107) from Spain including Valencia, Tarragona, Murcia and Extremadura, Japan, Brazil and India were employed as training set whereas the validation set was formed by 46 samples of the aforementioned geographical origins. Data were processed by linear discriminant analysis (LDA), …

Mineral Profile

The identification of foods with protected designation of origin (PDO) has been a long-standing issue. Its detection provides valuable information to regulatory commissions (government and industries) which can regulate precise quality control procedures for their products. Authentication of food covers many different aspects, including characterization, mislabelling and misinformation regarding origin, and adulteration, which is defined as the process to reduce the quality or nature of a given substance by adding a foreign or an inferior substance and removing a vital element. Numerous methods have been developed as fingerprinting methodologies for PDO products. The analytical techniques c…

Headspace-Liquid Phase Microextraction for Attenuated Total Reflection Infrared Determination of Volatile Organic Compounds at Trace Levels

A combination of headspace (HS) sampling and liquid phase microextraction (LPME) has been successfully developed to solve sensitivity problems in attenuated total reflection (ATR) infrared determination of volatile organic compounds (VOCs). The HS sampling facilitates the selective extraction of the target volatile analytes from the sample matrix, while the liquid phase microextraction allows their preconcentration prior to infrared analysis. The direct determination of extracted analytes in the acceptor solvent provides high preconcentration factors of the order of 200 with a reduced consumption of organic solvents and a minimum generation of wastes, being thus the developed methodology a …

A review of non-chromatographic methods for speciation analysis.

This manuscript overviews relevant scientific literature concerning speciation of trace elements by using non-chromatographic methods. The main principles of the different strategies proposed in the published works and their advantages and drawbacks are discussed in order to provide to the readers an appropriate picture of the state-of the-art of fast and cheap methodologies available to obtain information about the presence of different chemical forms of trace elements in environmental, clinical and food samples. A selection of the methods proposed for the speciation of the different elements studied was also provided together with their main features.

Adulteration detection of argan oil by inductively coupled plasma optical emission spectrometry

Abstract The singularity of the trace element profile of argan oil has been demonstrated by means of inductively coupled plasma optical emission measurement in combination with different chemometric approaches. The ability of multivariate analysis methods; such as hierarchical cluster analysis (HCA), principal component analysis (PCA), classification trees using Chi -squared Automatic Interaction Detector (CHAID) and discriminant analysis (DA) to achieve edible oils classification based on its type or variety from their elemental content have been investigated. The calculations were performed using 16 variables (contents of Na, Mg, Al, K, Ca, Ti, Fe, Co, Ni, Cu, Zn, Cd, Pr, Sm, Er and Bi at…