Solid-phase microextraction (SPME) via on-fiber derivatization with O-(2,3,4,5,6-pentafluorobenzyl)-hydroxylamine (PFBHA) and gas chromatographic determination is considered a technique of choice in ...many analytical fields for formaldehyde (FA) monitoring. Vapor phase adsorption models of experimentally loaded PFBHA on porous divinylbenzene (DVB) SPME were investigated at 60 °C, 35 cm s-1 of air velocity, in a 1-64 min range: with the fiber completely exposed, loaded PFBHA was about 276 µg. Among the models tested, i.e. heat transfer, pseudo-second-order (PSO), Elovich, intra-particle diffusion, extra-particle diffusion and Langmuir, PFBHA adsorption was best fit by the PSO model, showing agreement with experimental data (272 µg). The sampling rate of FA in our conditions, obtained with a permeation tube system, was in agreement with literature (17.4 and 18.3 mL min-1, respectively). Thus, an overall standardization of the sampling phase is presented, leaving the sampling time as the most crucial parameter to be set for future applications.
The solid-phase microextraction (SPME), invented by Pawliszyn in 1989, today has a renewed and growing use and interest in the scientific community with fourteen techniques currently available on the ...market. The miniaturization of traditional sample preparation devices fulfills the new request of an environmental friendly analytical chemistry. The recent upswing of these solid-phase microextraction technologies has brought new availability and range of robotic automation. The microextraction solutions propose today on the market can cover a wide variety of analytical fields and applications. This review reports on the state-of-the-art innovative solid-phase microextraction techniques, especially those used for chromatographic separation and mass-spectrometric detection, given the recent improvements in availability and range of automation techniques. The progressively implemented solid-phase microextraction techniques and related automated commercially available devices are classified and described to offer a valuable tool to summarize their potential combinations to face all the laboratories requirements in terms of analytical applications, robustness, sensitivity, and throughput.
Formaldehyde (FA) is a carbonyl compound, ubiquitous in the environment and among the most widespread pollutants: it has exhibited toxic properties and is classified as a human carcinogen. FA is ...released from several sources, both temporary (e.g., combustion processes) and permanent (e.g., building products). This work proposes an innovative fully-automated application of headspace solid-phase microextraction (SPME) with on-fiber derivatization for the analysis of airborne FA emitted from liquid solutions or solid manufacts, in static mode, via gas chromatography-mass spectrometry. The method was tested in a wide range of airborne FA concentrations, using SPME and SPME Arrow fibers: the inter-day LOD and LOQ for SPME and SPME Arrow were evaluated, resulting in 0.072 and 0.215 ppm and 0.014 and 0.042 ppm, respectively. Moreover, other conventional detectors, such as Electron Capture Detector (ECD), Thermoionic Specific Detector (TSD), Photoionization Detector (PID), and Flame Ionization Detector (FID), were tested to set an analytical method to meet different requirements. The sensitivity and linearity of PID, FID and MS were comparable, while TSD and ECD were not suitable for the developed method, due to issues of response or linearity. MS results to be the most suitable and perfoming detector, however PID and FID result to be cheaper valid alternatives.
Metal-additive manufacturing (AM), particularly the powder-bed fusion (PBF) technique, is undergoing a transition from the short-run production of components to higher-volume manufacturing. The ...industry’s increased production efficiency is paired with a growing awareness of the risks related to the inhalation of very fine metal powders during PBF and AM processes, and there is a pressing need for a ready-to-use approach to assess the risks and the occupational exposure to these very final metal powders. This article presents a study conducted in an AM facility, which was conducted with the aim to propose a solution to monitor incidental airborne particle emissions during metal AM by setting up an analytical network for a tailored approach to risk assessment. Quantitative data about the respirable and inhalable particle and metal content were obtained by gravimetric and ICP-MS analyses. In addition, the concentrations of airborne particles (10–300 nm) were investigated using a direct reading instrument. A qualitative approach for risk assessment was fulfilled using control banding Nanotool v2.0. The results show that the operations in the AM facility are in line with exposure limit levels for both micron-sized and nano-sized particles. The particulate observed in the working area contains metals, such as chromium, cobalt, and nickel; thus, biological monitoring is recommended. To manage the risk level observed for all of the tasks during the AM process, containment and the supervision of an occupational safety expert are recommended to manage the risk. This study represents a useful tool that can be used to carry out a static evaluation of the risk and exposure to potentially harmful very fine metal powders in AM; however, due to the continuous innovations in this field, a dynamic approach could represent an interesting future perspective for occupational safety.
Growing attention on carcinogenicity and mutagenicity of antineoplastic drugs (ADs) from the International Agencies has led to the present strict safe handling and administration regulations. ...Accordingly, one of the most common ways to assess occupational exposure to these substances is to identify and quantify possible surface contamination inside hospital preparation and administration units. Thus, it is essential to develop a fast and high-throughput monitoring method capable of identifying a significant number of ADs. The present study reports developing a UHPLC–MS/MS analysis to screen 26 ADs surface contamination through wipe test sampling. A Cortecs UPLC T3 50 × 2.1 mm (1.6 µm) column was selected to perform the analysis, using the evaluations of previous studies and the Product Quality Research Institute (PQRI) database. The design of experiments (DoE) methodological approach was used to optimize the chromatographic conditions concerning the best separation between all ADs. The limits of quantification for the analytes were between the pg/mL and ng/mL orders, and the turnaround time was limited to about 15 min. The obtained accuracy was mostly between 90% and 110% for all the analytes, while the precision was under 10% and a low matrix effect was observed for said analytes. Only vindesine and docetaxel presented lower performances.
Platinum-based antineoplastic drugs (PtADs) are among the most important and used families of chemotherapy drugs, which, even showing severe side effects and being hindered by drug resistance, are ...not likely to be replaced clinically any time soon. The growing interest in the occupational health community in antineoplastic drug (AD) surface contamination requires the development of increasingly fast and easy high-throughput monitoring methods, even considering the lack of harmonized legally binding regulation criteria. Thus, a wipe sampling method together with zwitterionic hydrophilic interaction liquid chromatography (HILIC-Z)–tandem mass spectrometry (MS/MS) analysis was developed for the simultaneous evaluation of oxaliplatin, cisplatin, and carboplatin surface contaminations. A design of experiments approach was used to optimize the chromatographic conditions. Limits of quantification ranging from 2 to 5 ng/mL were obtained from interday and intraday repetitions for oxaliplatin and carboplatin, and between 170 and 240 ng/mL for cisplatin. The wipe desorption procedure is equivalent to other AD sampling methods, enabling a fast sample preparation, with an LC-MS/MS analysis time of less than 7 min.
Antineoplastic drugs are a wide and heterogeneous group of substances that, as universally known, can cause highly severe toxic effects to whoever is exposed. From an occupational safety point of ...view, surface contaminations inside preparation and administration units are a growing issue and therefore require the development and implementation of sensible and fast monitoring methods. The unlikelihood of a unique all-embracing chromatography, able to correctly retain and separate each analyte led to the need to create an orthogonal normal phase analysis, which might be able to fill the gaps in the more common reversed-phase ones. An existing hydrophilic interaction method has thus been expanded to 6 other drugs and applied to real samples after an evaluation of its performances. The experimental data were then used to evaluate the possibility of estimating reliable relationships between the chromatographic retention and the chemical-structural features of the drugs under analysis.
Formaldehyde (FA) is ubiquitous in the atmospheric environment. It is generally the dominant atmospheric carbonyl compound. Due to its well-known carcinogenicity, FA is a compound that arises the ...attention in the scientific community. In studies concerning the toxicological effects of FA on humans, animals, and the environment, testing and calibration of air sampling systems and analytical instruments are pivotal. Therefore, the preparation of controllable standard gaseous atmospheres containing FA at levels known with precision and accuracy is essential. This review summarizes the procedures for generating the FA atmosphere, given that operative solutions have been evolving recently. Furthermore, an overview on the available system to collect and store gaseous standard is reported. The progressively implemented FA generation techniques, together with commercially-available instruments, are herein described, classified, and compared.
PDF
