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Herein we report the development of solid-phase microextraction (SPME) devices designed to perform fast extraction/enrichment of target analytes present in small volumes of complex matrices (i.e. V≤10 μL). Micro-sampling was performed with the use of etched metal tips coated with a thin layer of biocompatible nano-structured polypyrrole (PPy), or by using coated blade spray (CBS) devices. These devices can be coupled either to liquid chromatography (LC), or directly to mass spectrometry (MS) via dedicated interfaces. The reported results demonstrated that the whole analytical procedure can be carried out within a few minutes with high sensitivity and quantitation precision, and can be used to sample from various biological matrices such as blood, urine, or Allium cepa L single-cells.

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Abstract:The current study reports the development of solid phase microextraction (SPME) devices designed to perform fast extraction/enrichment of target analytes present in small volumes of complex matrices (i.e. V ≤ 10 μL). Micro-sampling was performed with the use of etched metal tips coated with a thin layer of biocompatible nano-structured polypyrrole (PPy (tip diameter ≤ 10 µm), or by using coated blade spray (CBS) devices with an extraction phase thickness ≤ 10 µm, facilitating rapid extraction. These devices can be coupled either to liquid chromatography (LC), or directly to mass spectrometry (MS) via dedicated interfaces. The reported results demonstrated that the whole analytical procedure can be carried out within a few minutes (tanalysis ≤ 7 min) with high sensitivity and quantitation precision, and can be used to sample from various biological matrices such as blood, plasma, and urine, towards the analysis of therapeutics, pesticides, and controlled substances as model analytes. As a proof-of-concept, the analysis and quantification of target compounds present in single cells of Allium cepa L was demonstrated.

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Time weighted average (TWA) passive sampling with thin film solid phase microextraction (TF-SPME) and liquid chromatography tandem mass spectrometry (LC-MS/MS) was used for collection, identification, and quantification of benzophenone-1, benzophenone-2, benzophenone-3, benzophenone-4, 2-phenylbenzimidazole-5-sulfonic acid, octocrylene, octylmethoxycinnamate, butylmethoxydibenzoylmethane, triclocarban and triclosan in the aquatic environment. Two types of TF-SPME passive samplers, including a retracted thin film device using a hydrophilic lipophilic balance (HLB) coating, and an open bed configuration with an octadecyl silica-based (C18)coating, were evaluated in an aqueous standard generation system. Laboratory calibration results indicated that the thin film retracted device using HLB coating is suitable to determine TWA concentrations of polar analytes in water, with an uptake that was linear up to 70 days. In open bed form, a one-calibrant kinetic calibration technique was accomplished by loading benzophenone3-d as calibrant on the C18 coating to quantify all nonpolar compounds. The experimental results showed that the one-calibrant kinetic calibration technique can be used for determination of classes of compounds in cases where deuterated counterparts are either not available or expensive. The developed passive samplers were deployed in wastewater-dominated reaches of the Grand River (Kitchener, ON) to verify their feasibility for determination of TWA concentrations in on-site applications. Field trials results indicated that these devices are suitable for long-term and short-term monitoring of compounds varying in polarity, such as UV blockers and biocide compounds in water, and the data were in good agreement with literature data.

A highly selective voltammetric sensor for the determination of meloxicam using a MIP@MWCNT–CPE is introduced.