Pascual Serra-Mora

In tube-solid phase microextraction-nano liquid chromatography: Application to the determination of intact and degraded polar triazines in waters and recovered struvite

In-tube solid-phase microextraction (IT-SPME) coupled to miniaturized liquid chromatography (LC) techniques are attractive mainly due to the column efficiency improvement, sensitivity enhancement and reduction of solvent consumption. In addition, the nanomaterials based sorbents can play a key role in the improvement of the extraction efficiency taking into account their interesting physical and chemical properties. Thus, in this work the performance of IT-SPME coupled to nano LC (NanoLC) has been compared with the performance of IT-SPME coupled to capillary LC (CapLC) with similar configurations for the determination of polar triazines including their degradation products. In both cases, a DAD detector was used. Different extractive phases such as TRB-5, TRB-5/c-SWNTs, TRB-5/c-MWNTs capillary columns have been tested. The dimensions of the capillary columns were 0.32mm id×40cm length and 0.1 or 0.075mm i.d.×15cm length for the couplings with CapLC and NanoLC, respectively. The processed volume was 4mL for CapLC and 0.5mL for NanoLC. The elution was carried out with ACN:H2O (30:70, v/v). IT-SPME-NanoLC has shown a higher performance than IT-SPME-CapLC for the target analytes demonstrating the enhancement of the extraction efficiency with the former configuration. A new phase TEOS-MTEOS-SiO2NPs has been also proposed for IT-SPME-NanoLC, which improves the retention of polar compounds. Compared with previously published works, improved LODs were achieved (0.025-0.5μgL-1). The practical application of the proposed procedure has been demonstrated for the analysis of water samples and recovered struvite samples from wastewater treatment plants. Therefore, the proposed procedure can be an alternative method for regulatory purposes.

A sustainable on-line CapLC method for quantifying antifouling agents like irgarol-1051 and diuron in water samples: Estimation of the carbon footprint

In this work, in-tube solid phase microextraction (in-tube SPME) coupled to capillary LC (CapLC) with diode array detection has been reported, for on-line extraction and enrichment of booster biocides (irgarol-1051 and diuron) included in Water Frame Directive 2013/39/UE (WFD). The analytical performance has been successfully demonstrated. Furthermore, in the present work, the environmental friendliness of the procedure has been quantified by means of the implementation of the carbon footprint calculation of the analytical procedure and the comparison with other methodologies previously reported. Under the optimum conditions, the method presents good linearity over the range assayed, 0.05-10μg/L for irgarol-1051 and 0.7-10μg/L for diuron. The LODs were 0.015μg/L and 0.2μg/L for irgarol-1051 and diuron, respectively. Precision was also satisfactory (relative standard deviation, RSD<3.5%). The proposed methodology was applied to monitor water samples, taking into account the EQS standards for these compounds. The carbon footprint values for the proposed procedure consolidate the operational efficiency (analytical and environmental performance) of in-tube SPME-CapLC-DAD, in general, and in particular for determining irgarol-1051 and diuron in water samples.

A new tool for direct non-invasive evaluation of chlorophyll a content from diffuse reflectance measurements

Chlorophyll is a key biochemical component that is responsible for photosynthesis and is an indicator of plant health. The effect of stressors can be determined by measuring the amount of chlorophyll a, which is the most abundant chlorophyll, in vegetation in general. Nowadays, invasive methods and vegetation indices are used for establishing chlorophyll amount or an approximation to this value, respectively. This paper demonstrates that H-point curve isolation method (HPCIM) is useful for isolating the signal of chlorophyll a from non-invasive diffuse reflectance measurements of leaves. Spinach plants have been chosen as an example. For applying the HPCIM only the registers of both, a standard and the sample are needed. The results obtained by HPCIM and the invasive method were statistically similar for spinach leaves: 144±6mg/m2 (n=5) and 155±40mg/m2 (n=5), respectively. However, more precise values were achieved with the HPCIM, which also involved minimal experimental effort. The HPCIM method was applied to spinach plants stressed by the action of several pesticides and water scarcity, showing a decrease of chlorophyll a content with time, which is related with a loss of health. The results obtained were compared with those achieved by two different reflectance vegetation indices (Macc01 and NDVI). Although NDVI and HPCIM gave similar footprints for the plants tested, vegetation indices fail in the estimation of real content of the chlorophyll a. The HPCIM could contribute to improve the knowledge of the chlorophyll a content of vegetation like health indicator, by applying it to a much employed non-invasive technique such as diffuse reflectance, which can be used in place or in remote sensing mode.