Mesostructured Silicas as Cation-Exchange Sorbents in Packed or Dispersive Solid Phase Extraction for the Determination of Tropane Alkaloids in Culinary Aromatics Herbs by HPLC-MS/MS.

In this work, Hexagonal Mesoporous Silica (HMS) and Santa Barbara Amorphous-15 (SBA-15) mesostructured silicas were synthesized and functionalized with sulfonic acid groups. The materials (HMS-SO3− and SBA-15-SO3−) were evaluated as strong cation exchange sorbents for sample extract clean-up, by solid phase extraction (SPE) and dispersive solid phase extraction, to determine atropine (At) and scopolamine (Sc) in commercial culinary aromatic herbs. Under optimized conditions, 0.

Sulfonic Acid-Functionalized SBA-15 as Strong Cation-Exchange Sorbent for Solid-Phase Extraction of Atropine and Scopolamine in Gluten-Free Grains and Flours.

A novel method was developed and applied to the determination of the most representative tropane alkaloids (TAs), atropine and scopolamine, in gluten-free (GF) grains and flours by HPLC-MS/MS. Accordingly a suitable sample treatment procedure based on solid-liquid extraction (SLE) and followed by strong cation-exchange solid-phase extraction (SCX-SPE) was optimized. SBA-15 mesostructured silica functionalized with sulfonic acids was evaluated as sorbent.

New Advanced Materials and Sorbent-Based Microextraction Techniques as Strategies in Sample Preparation to Improve the Determination of Natural Toxins in Food Samples.

Natural toxins are chemical substances that are not toxic to the organisms that produce them, but which can be a potential risk to human health when ingested through food. Thus, it is of high interest to develop advanced analytical methodologies to control the occurrence of these compounds in food products. However, the analysis of food samples is a challenging task because of the high complexity of these matrices, which hinders the extraction and detection of the analytes.

On-line flow injection molecularly imprinted solid phase extraction for the preconcentration and determination of 1-hydroxypyrene in urine samples.

New analytical strategies tend to automation of sample pre-treatment and flow analysis techniques provided a number of enhanced analytical methods allowing high throughput. Flow techniques are usually faster, more robust and more flexible than their batch equivalents. In addition, flow methods use less sample and reagent amounts and reduce analytical costs and waste.

One-pot synthesized functionalized mesoporous silica as a reversed-phase sorbent for solid-phase extraction of endocrine disrupting compounds in milks.

A new procedure for the determination of 12 naturally occurring hormones and some related synthetic chemicals in milk, commonly used as growth promoters in cattle, is reported. The method is based on liquid-liquid extraction followed by solid-phase extraction (SPE) using a new one-pot synthesized ordered mesoporous silica (of the SBA-15 type) functionalized with octadecyl groups (denoted as SBA-15-C18-CO) as reversed-phase sorbent. The analytes were eluted with methanol and then submitted to HPLC with diode array detection.

Novel supports in chiral stationary phase development for liquid chromatography. Preparation, characterization and application of ordered mesoporous silica particles.

Recent advances in the development of new materials are having a major impact on analytical chemistry. For example, the unique properties of ordered mesoporous silicas (OMSs) have been shown to enhance the analytical performance of many existing techniques or allow new, exciting ones to be developed. Likewise, the introduction of organo-functional groups makes OMSs highly versatile and enables them to perform specialized tasks, such as the separation of chiral compounds.

Evaluation of a molecularly imprinted polymer for determination of steroids in goat milk by matrix solid phase dispersion.

A molecularly imprinted polymer-matrix solid-phase dispersion methodology for simultaneous determination of five steroids in goat milk samples was proposed. Factors affecting the extraction recovery such as sample/dispersant ratio and washing and elution solvents were investigated. The molecularly imprinted polymer used as dispersant in the matrix solid-phase dispersion procedure showed high affinity to steroids, and the obtained extracts were sufficiently cleaned to be directly analyzed.

Comparison of different mesoporous silicas for off-line solid phase extraction of 17β-estradiol from waters and its determination by HPLC-DAD.

Functionalized (SBA-C₁₈ and SM-C₁₈) and non-functionalized (SBA-15 and SM) mesoporous silicas were then examined as sorbents for solid-phase extraction of 17β-estradiol in aqueous media. Experiments were run in order to test critical factors affecting the procedure extraction efficiency, including the type of sorbent, the analyte concentration, the solvent and volume used for elution and the sample volume. Among the prepared materials, SBA-C₁₈ had the highest adsorption affinity towards 17β-estradiol and under optimized conditions (200mg of sorbent, 150 mL of water sample, elution with 3 × 2 mL of methanol) this sorbent proved good extraction capacity and elution efficiency for this hormone from aqueous media (recovery near 100%).

Development of a molecularly imprinted polymer-matrix solid-phase dispersion method for selective determination of β-estradiol as anabolic growth promoter in goat milk.

A simple, fast, and sensitive method for determination of 17 β-estradiol (E2) in goat milk samples has been developed by combining selective molecularly imprinted matrix solid-phase dispersion (MIP-MSPD) and liquid chromatography with diode-array detection (DAD). The molecularly imprinted polymer was synthesized by use of 17β-estradiol as template molecule, methacrylic acid as functional monomer, ethylene glycol dimethacrylate as crosslinker monomer, azobisisobutyronitrile as initiator, and acetonitrile as porogen, and was used as selective solid support for matrix solid-phase dispersion. The selected dispersant had high affinity for E2 in the goat milk matrix and the extract obtained was sufficiently clean for direct injection for HPLC analysis without any interferences from the matrix.

Adsorption of p-nitrophenol on activated carbon fixed-bed.

Carbon fixed-beds are usually used to remove organic contaminants. Adsorption in a carbon filter is a dynamic, non-steady process which is not yet completely understood. The objective of this paper is to establish a methodology to simplify the study of this process based on the wave theory, rapid small-scale column test and experimental design/surface response analysis.

Determination of the energy potential of gases produced in the pyrolysis processes of the vegetal carbon manufacture industry.

In this work, a pyrolysis plant located in Valverde de Leganes, Badajoz (SW Spain) was studied. At present, only the solid phase obtained by pyrolysis finds an application as domestic fuel. In order to analyze the feasibility of a further energetic exploitation of the plant under study, the gases flowing through the chimneys were collected at different times throughout the pyrolysis process.