Jesús Salafranca

Critical review on recent developments in solventless techniques for extraction of analytes

The most recent contributions on solventless extraction techniques have been reviewed. This paper deals with those techniques that use solid phases, such as solid-phase microextraction, liquid phases, such as single-drop microextraction and hollow-fibre liquid-phase microextraction, and subcritical fluids, such as subcritical water extraction. In all cases, the most recent publications have been critically studied. Direct extraction and derivatization processes to facilitate the extraction of analytes in different areas have been included. Hyphenated approaches, if available, are also included in this review. Comparison of techniques organized by analytes and matrices also enhances this critical overview of solventless techniques.

Determination of bisphenol-type contaminants from food packaging materials in aqueous foods by solid-phase microextraction-high-performance liquid chromatography.

A fast screening method consisting of off-line solid-phase microextraction coupled to HPLC and fluorescence detection, suitable for the analysis of several bisphenol derivatives and their degradation products in aqueous solution, has been developed. Detection limits of 0.7 ng ml(-1) for 2,2-bis[4-(glycidyloxy)phenyl]propane, 0.9 ng ml(-1) for bisphenol A bis(3-chloro-2-hydroxypropyl)ether, 1.1 ng ml(-1) for 2,2-bis(4-hydroxyphenyl)propane and 2.4 ng ml(-1) for bisphenol F diglycidyl ether have been achieved working in the linear range 10-500 ng ml(-1). The good analytical features achieved make the proposed method an interesting option for the direct determination of these compounds in aqueous canned food such as peas, tuna, olives, maize, artichokes or palm hearts. Both the optimization process and the results, including the analysis of real samples, are given and discussed.

Use of solid-phase microextraction for the analysis of bisphenol A and bisphenol A diglycidyl ether in food simulants

A new method has been developed to simultaneously analyse bisphenol A (BPA) and bisphenol A diglycidyl ether (BADGE) in aqueous based food simulants. The method consists on direct immersion solid-phase microextraction (SPME) of the analytes from the liquid matrix and subsequent chromatographic analysis by gas chromatography-mass spectrometry. Using the proposed method, a whole analysis (including chromatographic step) can be completed in less than 40 min, with minimum sample handling. The SPME method shows good analytical performance for simultaneous BPA and BADGE analysis, except for BADGE determination in the aqueous alcohol (simulant C) solution. Detection limits ranging from 0.1 to 2.0 ng/g for BPA and from 13 to 15 ng/g from BADGE were obtained, with a linear range from the low-ng/g to several-microg/g range for BPA and from 0.1 microg/g to 40 microg/g for BADGE. A possible optimisation method has been also developed and introduced.

Assessment of specific migration to aqueous simulants of a new active food packaging containing essential oils by means of an automatic multiple dynamic hollow fibre liquid phase microextraction system.

The determination of specific migration in the three aqueous food simulants (water, 3% acetic acid and 10% ethanol) from experimental active packaging polypropylene-based films containing natural essential oils as active agents has been carried out for the first time by a two-phase hollow fibre liquid phase microextraction (HFLPME). Due to the high number of variables involved, an experimental design has been applied. High throughput, with six samples running simultaneously in a highly automated system working in dynamic extraction mode, has been achieved. The main analytical characteristics are detection limits as low as 0.01 microg kg(-1), linearity higher than 0.99 for almost 5 magnitude orders, average precision below 16% as RSD and concentration factors ranging from 4 to 189. Migration of 43 compounds including terpenes, alkanes, plastic additives and degradation compounds is reported. According to the results obtained and European legislation, the packaging prototypes tested could be safely marketed.

Parts-per-trillion determination of styrene in yoghurt by purge-and-trap gas chromatography with mass spectrometry detection.

Headspace sampling methods prior to capillary gas chromatography have been widely used for the determination of volatile compounds present in very different kinds of samples. This paper describes an automated and rapid system to determine volatiles from yoghurt. Thirty-five volatile organic compounds (VOCs) were identified in polystyrene cups used for yoghurt packaging and 42 VOCs from yoghurt samples. Quantitation of styrene in several samples from the Spanish retail market was carried out.

Separation of polymer and on-line determination of several antioxidants and UV stabilizers by coupling size-exclusion and normal-phase high-performance liquid chromatography columns

Abstract A procedure consisting of connecting in series two different HPLC columns, one for size-exclusion chromatography (SEC) and the second one a normal-phase (silica) column has been developed. An automatic three-way switching valve was placed between the two columns. Through the valve, the polymer was drained whereas the rest of the compounds, a group of antioxidants and UV stabilizers, were separated and analyzed in the second column. The behaviour of the SEC column in different organic phases is studied. Detection limits about 0.1 μg ml −1 were obtained for BHT, Tinuvin 326 and Tinuvin 327; 0.2 μg ml −1 for Irganox 1076, and 1.1 μg ml −1 for Cyasorb UV 9 and Cyasorb UV 1084. R.S.D. values of the whole process are lower than 4%.

Analytical procedure for the determination of Ethyl Lauroyl Arginate (LAE) to assess the kinetics and specific migration from a new antimicrobial active food packaging

Ethyl Lauroyl Arginate (LAE) is a cationic tensoactive compound, soluble in water, with a wide activity spectrum against moulds and bacteria. LAE has been incorporated as antimicrobial agent into packaging materials for food contact and these materials require to comply with the specific migration criteria. In this paper, one analytical procedure has been developed and optimized for the analysis of LAE in food simulants after the migrations tests. It consists of the formation of an ionic pair between LAE and the inorganic complex Co(SCN)(4)(2-) in aqueous solution, followed by a liquid-liquid extraction in a suitable organic solvent and further UV-Vis absorbance measurement. In order to evaluate possible interferences, the ionic pair has been also analyzed by high performance liquid chromatography with UV-Vis detection. Both procedures provided similar analytical characteristics, with linear ranges from 1.10 to 25.00 mg kg(-1), linearity higher than 0.9886, limits of detection and quantification of 0.33 and 1.10 mg kg(-1), respectively, accuracy better than 1% as relative error and precision better than 3.6% expressed as RSD. Optimization of analytical techniques, thermal and chemical stability of LAE, as well as migration kinetics of LAE from experimental active packaging are reported and discussed.

Supercritical fluid extraction (SFE) optimization by full-factorial design for the determination of Irganox 1076, Irgafos 168, and Chimassorb 81 in virgin and recycled polyolefins

The performance and feasibility of supercritical fluid extraction (SFE) applied to the extraction of some antioxidants (Irganox 1076, Irgafos 168) and one UV-stabilizer (Chimassorb 81) from both virgin and recycled low density polyethylene (LDPE), and virgin high density polyethylene (HDPE) are studied. Due to the high number of variables a full-factorial design has been applied to minimize the number of experiments required to reach the optimum extraction conditions. Further analysis has been carried out off-line by reversed-phase HPLC. Modification of the physical properties of the polymeric matrix and increased number of recycling cycles as well as the influence of physical properties on the efficiency of SFE are also discussed.

Multicomponent recycled plastics: Considerations about their use in food contact applications

Two multicomponent post-use recycled plastics named as NPP40A3 (formulated with 85% HDPE and 15% of a PP-PS-PVC mixture) and NPP40A6 (formulated with 80% NPP40A3, 10% ABS and 10% HIPS), both of them with 3.1% of plasticizer and 0.6% of stabilizer to obtain a better final product, have been analysed. Plastics were extracted both with dichloromethane and methylbenzene, and analysed by HPLC and GC-MS to identify the maximum possible number of compounds. Major additives quantified were di(ethylhexyl)phthalate (3.262% and 2.955% respectively) and Irganox 1010 (0.473% and 0.498% respectively). Several degradation compounds have been detected. In order to check if these plastics could be used in food contact applications, global and specific migration tests have been applied. The results obtained are discussed.

Determination of Volatile and Semi-Volatile Model Contaminants in Recycled High-Impact Polystyrene from Food-Contact Applications. Comparison of Extraction by Purge-and-Trap, Co-evaporation, and Total Dissolution

SummarySeven samples of high-impact polystyrene (HIPS) flakes, from post-consumer coffee cups, previously deliberately contaminated with four volatile and semivolatile model compounds (1,1,1-trichloroethane, methylbenzene, chlorobenzene, and phenylcyclohexane) to simulate misuse, have been collected at different times from a recycling plant and analyzed directly after extraction by purge-and-trap or by co-evaporation (a modified static headspace procedure).As a reference method HIPS samples were also dissolved in dimethylacetamide (to furnish an homogeneous matrix) and analyzed after extraction by coevaporation. Significance tests were used to evaluate the feasibility of using these methods for the direct analysis of solid polymers. Results obtained by use of the three methods are compared and discussed.