Sensitive Solid-phase Microextraction Method Research Articles

A functionalized glass fiber as the adsorbent for efficient analysis of endocrine disruptors in aqueous environments

Estrogens and bisphenols are typical endocrine disruptors (EDs) that pose a potential hazard to the human body due to their widespread presence in aqueous environments. In this study, a β-cyclodextrin porous crosslinked polymer (β-CD-PCP) was prepared in-situ on a glass fiber surface by a nucleophilic substitution reaction. An effective and sensitive solid phase microextraction method using functionalized glass fiber with β-CD-PCP coating as the adsorbent was established for the detection of 11 EDs in a water environment. The β-CD-PCP was in-situ prepared on a glass fiber surface by a nucleophilic substitution reaction. The β-CD-PCP successfully separated five estrogens (ESTs) and six bisphenols (BPs) through hydrophobic and π-π interactions. The conditions affecting extraction were optimized. Under the optimized conditions, the ESTs obtained a high enrichment effect (1795–2328), low limits of detection (0.047 µg L−1) and a good linearity range (0.2–15.0 µg L−1). Furthermore, the spiked recoveries of analyte ESTs in aqueous environments were between 82.9–115.7 %. The results indicated that the prepared functionalized glass fibers exhibited good adsorption properties, and the established analytical method was reliable for monitoring trace ESTs and BPs in aqueous environments.

Synthesis of graphitic carbon nitride on 3D porous anodized aluminum wire as new fiber for microextraction of polycyclic aromatic hydrocarbons in water and wastewater samples

ABSTRACT A simple, fast, and sensitive solid phase microextraction method (SPME) has been applied for the enrichment and simultaneous determination of trace and toxic polycyclic aromatic hydrocarbons in water and wastewater samples. This method is based on the adsorption of these volatile compounds on a new robust fiber built from anodized aluminum wire coated with g-C3N4. Extraction of the analytes from different matrices on the fiber surface was performed by headspace mode (HS-SPME) at optimized conditions. This proposed method was used to determine trace amounts of some polycyclic aromatic hydrocarbons (PAHs) in real water and wastewater samples and provided good repeatability with a low limit of detection (LOD).

Solid phase microextraction method using a novel polystyrene oleic acid imidazole polymer in micropipette tip of syringe system for speciation and determination of antimony in environmental and food samples

A simple, rapid and sensitive solid phase microextraction method was used for the speciation of inorganic antimony (Sb) by using a novel synthesized polymeric material in micropipette tip of syringe system. In present methodology, the specie of Sb (III) made hydrophobic complex with diethyl dithiocarbamate (DDTC) at pH 5.5 and subsequently adsorbed on polystyrene oleic acid imidazole polymer (POIP), whereas Sb(V) did not made complex and adsorbed on the polymer, remained in aqueous solutions. The strategy of multivariate was carried out to screen out the different variables and assessed the optimum values of their experimental values for the extraction efficiency of analyte. Then the analyte was sorbed on the polymer in micropipette tip of syringe system was quantitatively eluted by different types of acids at different levels for 2–6 aspirating/dispensing cycles. The extracted Sb(III) ions with modifiers were directed into the graphite furnace atomic absorption spectrometry for analysis. The limit of detection (LOD), limit of quantification (LOQ) and preconcentration factor (PF) for Sb(III) was found to be 6 ng L−1, 20 ng L−1 and 100. The RSD value was found to be 4.2%. The standard addition method and certified reference materials were checked for accuracy and validity of method. The developed method was effectively applied for the determination of total and inorganic species of Sb(III) and Sb(V) in different types of water samples, whereas only total Sb was determined in acid digested soil, Tuna fish, rice, spinach, black tea, mixed fruit juice and ice tea samples.