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Authors: Stefano Dugheri, Alessandro Bonari, Ilenia Pompilio, Marco Colpo, Nicola Mucci, Manfredi Montalti and Giulio Arcangeli

World consumption of formaldehyde (FA) is forecast to grow at an average annual rate of about 4% from 2015 to 2020 with world production to exceed 52 million tons in 2017. From the first day of January 2016, the Commission Regulation No. 91/2015 established the FA classification through an indication from European Chemical Agency as category 2 mutagenic and category 1B carcinogen. A novel method for the determination of gaseous FA in air is presented herewith. The sampling was carried out using a miniaturized cartridge by means of a medium-flow pumping system (1.0 L min-1, 5–60 min) and absorption of FA vapors on 2,4-dinitrophenylhydrazine. Cartridge desorption removing the excess derivatizing agent based upon solid-phase extraction was performed by an innovative xyz robotic system on-line with fast gas chromatography (GC)—mass spectrometry (MS). Through the generation of standard atmospheres of known concentration of FA, we evaluated the precision (relative standard deviation for n = 10, 8.8%), lower limit of quantification (0.072 µg/cartridge), and linearity (from 0.125—64 µg/cartridge with correlation coefficient of 0.99) of the method. The described procedure combines the efficiency of fast GC—MS systems with both the high throughput of autosampler and the quantitative accuracy of FA-dinitrophenylhydrazone for measuring American Conference of Governmental Industrial Hygienists TLV Ceiling.

Open access
Authors: Stefano Dugheri, Nicola Mucci, Alessandro Bonari, Giorgio Marrubini, Giovanni Cappelli, Daniela Ubiali, Marcello Campagna, Manfredi Montalti and Giulio Arcangeli

In the last decade, the development and adoption of greener and sustainable microextraction techniques have been proved to be an effective alternative to classical sample preparation procedures. In this review, 10 commercially available solid-phase microextraction systems are presented, with special attention to the appraisal of their analytical, bioanalytical, and environmental engineering. This review provides an overview of the challenges and achievements in the application of fully automated miniaturized sample preparation methods in analytical laboratories. Both theoretical and practical aspects of these environment-friendly preparation approaches are discussed. The application of chemometrics in method development is also discussed. We are convinced that green analytical chemistry will be really useful in the years ahead. The application of cheap, fast, automated, “clever”, and environmentally safe procedures to environmental, clinical, and food analysis will improve significantly the quality of the analytical data.

Open access
Authors: Stefano Dugheri, Giorgio Marrubini, Nicola Mucci, Giovanni Cappelli, Alessandro Bonari, Ilenia Pompilio, Lucia Trevisani and Giulio Arcangeli

Abstract

Sample pretreatment is one of the most crucial and error-prone steps of an analytical procedure; it consents to improve selectivity and sensitivity by sample clean-up and pre-concentration. Nowadays, the arousing interest in greener and sustainable analytical chemistry has increased the development of microextraction techniques as alternative sample preparation procedures. In this review, we aimed to show two different categorizations of the most used micro-solid-phase extraction (μSPE) techniques. In essence, the first one concerns the solid-phase extraction (SPE) sorbent selection and structure: normal-phase, reversed-phase, ion-exchange, mixed-mode, molecular imprinted polymer, and special techniques (e.g., doped cartridges for specific analytes). The second is a grouping of the commercially available μSPE products in categories and sub-categories. We present every device and technology into the classifications paying attention to their historical development and the actual state of the art. So, this study aims to provide the state-of-the-art of μSPE techniques, highlighting their advantages, disadvantages, and possible future developments in sample pretreatment.

Open access
Authors: Stefano Dugheri, Nicola Mucci, Alessandro Bonari, Giorgio Marrubini, Giovanni Cappelli, Daniela Ubiali, Marcello Campagna, Manfredi Montalti and Giulio Arcangeli

Sample pretreatment is the first and the most important step of an analytical procedure. In routine analysis, liquid–liquid microextraction (LLE) is the most widely used sample pre-treatment technique, whose goal is to isolate the target analytes, provide enrichment, with cleanup to lower the chemical noise, and enhance the signal. The use of extensive volumes of hazardous organic solvents and production of large amounts of waste make LLE procedures unsuitable for modern, highly automated laboratories, expensive, and environmentally unfriendly. In the past two decades, liquid-phase microextraction (LPME) was introduced to overcome these drawbacks. Thanks to the need of only a few microliters of extraction solvent, LPME techniques have been widely adopted by the scientific community. The aim of this review is to report on the state-of-the-art LPME techniques used in gas and liquid chromatography. Attention was paid to the classification of the LPME operating modes, to the historical contextualization of LPME applications, and to the advantages of microextraction in methods respecting the value of green analytical chemistry. Technical aspects such as description of methodology selected in method development for routine use, specific variants of LPME developed for complex matrices, derivatization, and enrichment techniques are also discussed.

Open access