Quantification of free auxins in semi-hardwood plant cuttings and microshoots by dispersive liquid–liquid microextraction/microwave derivatization and GC/MS analysis

Several studies have suggested that differences in the natural rooting ability of plant cuttings could be attributed to differences in endogenous auxin levels. Hence, during rooting experiments, it is important to be able to routinely monitor the evolution of endogenous levels of plant hormones. This work reports the development of a new method for the quantification of free auxins in auxin-treated Olea europaea (L.) explants, using dispersive liquid–liquid microextraction (DLLME) and microwave assisted derivatization (MAD) followed by gas chromatography/mass spectrometry (GC/MS) analysis. Linear ranges of 0.5–500 ng mL 1 and 1–500 mg mL 1 were used for the quantification of indole-3-acetic acid (IAA) and indole-3-butyric acid (IBA), respectively. Determined by serial dilutions, the limits of detection (LOD) and quantification (LOQ) were 0.05 ng mL 1 and 0.25 ng mL 1, respectively for both compounds. When using the calibration curve for determination, the LOQ corresponded to 0.5 ng mL 1 (IAA) and 0.5 mg mL 1 (IBA). The proposed method proved to be substantially faster than other alternatives, and allowed free auxin quantification in real samples of semi-hardwood cuttings and microshoots of two olive cultivars. The concentrations found in the analyzed samples are in the range of 0.131–0.342 mg g 1 (IAA) and 20–264 mg g 1 (IBA).

Dual layer solid phase extraction based on molecular imprinting technology: Seeking a route to enhance selectivity for trace analysis of pesticide residues in olive oil.

Aiming to introduce a multiresidue analysis for the trace detection of pesticide residues belonging to organophosphorus and triazine classes from olive oil samples, a new sample preparation methodology comprising the use of a dual layer of “tailor-made” molecularly imprinted polymers (MIPs) SPE for the simultaneous extraction of both pesticides in a single procedure has been attempted. This work has focused on the implementation of a dual MIP-layer SPE procedure (DL-MISPE) encompassing the use of two MIP layers as specific sorbents. In order to achieve higher recovery rates, the amount of MIP layers has been optimized as well as the influence of MIP packaging order. The optimized DL-MISPE approach has been used in the preconcentration of spiked organic olive oil samples with concentrations of dimethoate and terbuthylazine similar to the maximum residue limits and further quantification by HPLC. High recovery rates for dimethoate (95%) and terbuthylazine (94%) have been achieved with good accuracy and precision. Overall, this work constitutes the first attempt on the development of a dual pesticide residue methodology for the trace analysis of pesticide residues based on molecular imprinting technology. Thus, DL-MISPE constitutes a reliable, robust, and sensitive sample preparation methodology that enables preconcentration of the target pesticides in complex olive oil samples, even at levels similar to the maximum residue limits enforced by the legislation.

QUANTIFICATION OF CALCIUM IN SPARKLING WINES BY INFRARED SPECTROSCOPY

Markets are increasingly competitive and the companies feel the urge to improve their manufacturing processes. Blending that with a larger control of quality and safety it was created a need to develop new methods of analysis each time more accurate, faster and with lower costs. Alentejo is a region with a wide variety of soils, most of them are rich in calcium and potassium. In the production of sparkling wine many wineries use encapsulated yeast in alginate beads, instead of the traditional method, champenoise. The first method is faster, allowing a more versatile production, reducing the risk of contamination and features organoleptic characteristics similar to the traditional method (yeast free). However, encapsulated yeast spheres should be only used if the base wine matches a number of features, among them calcium content. In this study the calcium content in the wine was determined by atomic absorption spectroscopy (AAS) and by near-infrared spectroscopy. The AAS is a high sensitivity method clearly produces a reliable result, however it is very time consuming and produces great quantities of environmental waste, therefore the possibility of using near-infrared spectroscopy as a method was studied to be a fast, simple and clean alternative to the AAS. It was obtained a calibration model with a variation coefficient higher than 0.80 which indicates that the near-infrared spectroscopy as an adequately alternative the ASS.