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The potential carcinogenicity of formaldehyde (FA) has prompted increasing preventive measures in anatomic pathology (AP) laboratories and new strategies aimed at innovating airborne FA monitoring systems. This review provides an updated overview of the most recent improvements in preventive measures, safe practices, and exposure monitoring tools in the FA usage and handling. A computer-based search of scientific and non-scientific sources was performed on PubMed, Web of Science, Google and Google Patents databases, querying the main topics of real-time, in-continuous FA monitoring instruments for sale, and commercially available tools for improving preventive measures in formalin management. In order to simplify the sampling process and to choose a better analytic solution to FA assessment, the main characteristics of each FA monitoring instrument were described. The novel technical tools recently introduced on the global market, aimed at reducing FA emissions in AP laboratories, were summarized. This review is directed at anatomic pathologists to draw their attention to the rapidly growing field of safe formalin practices. A repeated exposure assessment is recommended to evaluate technical changes in air monitoring programs to keep FA emissions low, in compliance with the limit value; thus, evolved monitoring devices are needed. Int J Occup Med Environ Health. 2021;34(3):319-38.

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.

The last two decades have been crucial for the assessment of airborne formaldehyde (FA) exposure in healthcare environments due to changes in limits and reference values, definition of carcinogenicity, and new monitoring methods. The aim of this study was to analyse twenty years (1999-2019) of experience in automatic, continuous airborne FA monitoring in the Pathology Laboratory and operating rooms at the Careggi University Hospital, Florence, Italy. These 20 years saw gradual improvements in FA monitoring of exposed employees considered at maximum risk, including improvements in analytical methods of detection and sampling strategies, which came with changes in procedures and workflow operations. In 2019, after the adoption of safe practices, including a closed-circuit system using pre-loaded containers and a vacuum sealing, 94 % of the total measurements (FA concentrations) were lower than 16 μg/m3, and only 6 % ranged from 21 to 75 μg/m3. In the studied work units, the ratio between area and personal readings ranged from 0.9 to 1.0, both for long and short-term sampling. Personal sampling was simplified with a new workstation, which integrated different monitoring systems into an innovative ergonomic armchair equipped with personal sampling devices. Area monitoring was also improved with a real-time, continuous photoacoustic instrument. Over these 20 years, FA exposure significantly dropped, which coincided with optimised histology workflow and implementation of safety practices. For high-throughput screening and cost savings we propose an innovative ergonomic armchair station which allows remote continuous monitoring.Posljednja dva desetljeća bila su iznimno važna za procjenu izloženosti formaldehidu (FA) u zraku u zdravstvenim ustanovama zahvaljujući promjenama u preporučenim maksimalnim i referentnim vrijednostima, definiciji njegove kancerogenosti i novim metodama mjerenja/praćenja. Cilj je ovog istraživanja bio analizirati dvadeset godina (1999. – 2000.) iskustva u automatskom, kontinuiranom mjerenju razina FA-a u laboratoriju za patologiju i operacijskim dvoranama talijanske sveučilišne bolnice Careggi u Firenzi. Tijekom tih dvadeset godina bolnica je postupno poboljšavala metode praćenja razina FA-a i osoblja izloženoga najvećem riziku, analitičke metode detekcije i strategije uzorkovanja koje su bile popraćene promjenama u odgovarajućim postupcima i organizaciji rada. Nakon usvajanja novih postupaka zaštite na radu 2019., uključujući i zatvoreni sustav rukovanja spremnicima i sustav vakuumskoga zatvaranja, razine FA-a u 94 % izmjera bile su niže od 16 μg/m

This review is an update of a previous review in 2009 and covers publications from 2009 to 2019. The review focuses on experimental design, referred to as the design of experiments (DoE), used in developing bioanalytical solid-phase microextraction (SPME) methods. Characteristics of different SPME approaches are illustrated and critically discussed. The literature selection evidences that two-level full factorial designs, with a limited number of factors (5), are most frequently used for preliminary factors screening. When applying the response surface methodology for the quantitative assessment of factorial effects, few quadratic models were used. The most popular were the rotatable central composite and Box-Benkhen designs. Models including more than four factors, such as fractional factorial designs (including the Plackett-Burman and Taguchi designs), were rarely used. Definitive screening and D-Optimal designs were not reported anywhere in the literature selection. When examining the diagnostic criteria used to evaluate different model's quality and validity, it was apparent the researchers relied heavily on commercial software for experimental design, analysis, and reporting of the results.

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.

Trimellitic anhydride (TMAn) is an essential starting material of the chemical manufacturing industry; it is widely used in saturated polyester resins (SPR) manufacturing to produce plasticizers for different purposes. TMAn was recently added, as a new substance of very high concern, to the candidate list by the European Chemicals Agency, since it can lead to sensitization, respiratory tract irritation and lung disease. Any substance from the list of candidates if present in manufactured products at concentrations above 0.1% (w/w) obliges the manufacturer to communicate this to customers down the supply chain and to consumers. We propose here a method that allows the fully automated determination of TMAn in SPR samples by using large volume injection (LVI), with programmed temperature vaporization (PTV) injection, in a gas chromatographic (GC) system equipped with ion trap mass spectrometer (IT) operating in tandem mass spectrometry (MS/MS). The method optimization was obtained by a chemometric model, using the experimental design. Introducing the use of short chromatographic column, triethyloxonium tetrafluoroborate (TEO) as derivatization agent and IS granted specificity, sensitivity and robustness. The detection and quantification limits for TMAn were 0.01% and 0.03% w/w, respectively. Trueness (between 94 and 98%) and precision (RSD lower than 10%, n = 6) were also assessed.

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.

Freshwater lakes and pools contained within peatlands are unique habitats that support rare and specialised species. Despite this, these ecosystems have been overlooked in conservation and management practices. One of these habitats, ‘3160 Natural dystrophic lakes and ponds’, is protected under the European Union (EU) Habitats Directive with a concerning proportion of these habitats having an “unfavourable-bad” or an “unfavourable-inadequate” conservation status across Europe. Our current understanding of the key physico-chemical and ecological features of this habitat is inadequate which is hindering the implementation of effective conservation measures. This review summarises the current knowledge of this protected lake habitat as defined under the EU Habitats Directive. With a focus on Ireland, we demonstrate how the current monitoring and assessment methods used to characterise and assess the structure and function and conservation status of this habitat, which relies largely on the use of macrophyte community composition and surrogate physico-chemical data collected under the EU Water Framework Directive, is ineffective. We propose the incorporation of further or alternative ecological metrics including, but not limited to, algae and macroinvertebrates which are needed to improve our understanding of the structure and function of this priority lake habitat. In addition, application of such data via ecological metrics would allow for the quantification of biodiversity and species rarity metrics which would aid in identifying sites of conservation importance. yes

Colovesical fistula (CVF) is an abnormal connection between the colon and the urinary bladder. Faecaluria, reported in 40–70% of cases, is virtually pathognomonic for CVF. During the 5th day of recovery in an 84 years old subject, the passage of cloudy, malodorous urine with visible debris was observed. According to the pathognomonic character of faecaluria, the sample was signed to the laboratory for biochemical and microbiological investigation, able to define the type and origin of materials. Following clinical requirements, both biochemical pathways and instrumental procedures able to confirm or exclude the presence of faecal components in urine were considered. No biochemical compound or component addressing faecal compounds in urine results available between laboratory tests. The brown powder component of the pellet was identified as Keratin, with 90% overlapping with the reference spectrum of the compound. FT-IR analysis on urine pellet can be proposed as a simple, non-invasive, and fast method to improve the diagnostic course of CVF.

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 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.

This review is directed at preventive health professionals, anatomic pathologists and technicians to focus their attention on the rapidly growing field of safe formalin practices. An updated overview of the most recent improvements in preventive measures versus formaldehyde (FA) in the anatomic pathology laboratories (APL) is provided. The occupational hygienist role and the required knowledge for a modern and clear occupational exposure assessment are described. Real-time, in-continuous, commercial analyzers for repeated FA exposure assessment are considered to evaluate technical changes in air monitoring programs, introduced to mitigate FA emissions, in compliance with the adopted limit values. To better choose the adequate instrumentation, the main features of each FA monitoring instrument recently introduced on the market are listed. Moreover, the main features of the modern workflow setting in APL are summarized. A computer-based scientific and non-scientific reports search by key-words was performed on PubMed, Web of Science, Google Scholar and Google Patents databases, querying the following topics: i) grossing workstation for ergonomic layout, ii) commercially available direct reading tools to measure formalin, iii) real-time, in-continuous FA monitoring instruments for sale. This review represents a useful tool to summarize the technical requirements and expert know-how necessary to minimize FA emissions and produce an exhaustive FA assessment in the APL., Ovaj pregled usmjeren je na preventivne zdravstvene radnike, anatomske patologe i tehničare kako bi svoju pozornost usredotočili na brzo rastuće područje sigurnih formalinskih praksi. Ažurirani pregled nudi najnovija poboljšanja preventivnih mjera u odnosu na formaldehid (FA) u laboratorijima za anatomsku patologiju (APL). Opisana je uloga higijeničara na radu i potrebna znanja za modernu i jasnu procjenu izloženosti na radu. Komercijalni analizatori u stvarnom vremenu za kontinuiranu procjenu izloženosti FA razmatraju se za procjenu tehničkih promjena u programima praćenja zraka, uvedenim radi ublažavanja emisija FA, u skladu s prihvaćenim graničnim vrijednostima. Kako bi se bolje odabrala odgovarajuća instrumentacija, navedene su glavne značajke svakog instrumenta za praćenje FA koji je nedavno predstavljen na tržištu. Štoviše, sažete su glavne značajke suvremenih postavki tijeka rada u APL-u. Računalno zasnovano pretraživanje znanstvenih i neznanstvenih izvješća po ključnim riječima provedeno je u bazama podataka PubMed, Web of Science, Google Scholar i Google Patents, s težištem na sljedeće teme: i) prikupljanje radnih stanica za ergonomski raspored, ii) komercijalno dostupni alati za izravno očitanje mjerenja formalina, iii) instrumenti za kontinuirano praćenje FA u stvarnom vremenu u prodaji. Ovaj pregled predstavlja koristan alat za sažimanje tehničkih zahtjeva i stručnog znanja potrebnog za minimiziranje emisija FA i izradu iscrpne procjene FA u APL-u.

Background The case concerns a 30-year-old woman in the 24th week of pregnancy presenting to the medical emergency room with fever and abdominal pain. Urine sediment microscopy revealed the presence of unknown needle-shaped crystals. Methods Crystals identification was performed by Fourier-Transform Infrared Spectroscopy coupled to Attenuated Total Reflectance (FTIR-ATR). Results Amoxicillin crystals were verified with semiquantitative results of 87.7%. Conclusions Drug-induced crystalluria is a frequent finding in urine examination and it may be asymptomatic. FTIR spectroscopy is a rapid and specific tool in identification of crystals and could be useful supporting renal disease diagnosis and monitoring drug therapy.

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.

Carbonyl compounds (CCs) are products present both as vapors and as condensed species adsorbed on the carbonaceous particle matter dispersed in the air of urban areas, due to vehicular traffic and human activities. Chronic exposure to CCs is a potential health risk given the toxicity of these chemicals. The present study reports on the measurement of the concentrations of 14 CCs in air as vapors and 2.5 &micro, m fraction PM by the ENVINT GAS08/16 gas/aerosol sampler, a serial sampler that uses annular denuder, as sampling device. The 14 CCs were derivatized during sampling prior to gas-chromatographic separation and multiple detection by mass spectrometry, nitrogen-phosphorus thermionic, electron capture detection. Outdoor air multiple samples were collected in four locations in the urban area of Florence. The results evidenced that formaldehyde, acetaldehyde, and acetone were the more abundant CCs in the studied areas. The data collected was discussed considering the particle to vapor ratio of each CC found. The CCs pollution picture obtained was tentatively related to the nature and intensity of the traffic transiting by the sampling sites. This approach allowed to determine 14 CCs in both concentrated and diluted samples and is proposed as a tool for investigating outdoor and indoor pollution.

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.

Air monitoring is the quantitative-qualitative assessment of the extent of pollutants. It is performed to ensure compliance with legislation and to evaluate control measures and mitigation solutions. There are numerous approaches to measure airborne formaldehyde (FA), ranging from passive sampling techniques to remote sensing devices. Research of sampling procedures and analytical methods was performed in a scientific database and on the web to offer a scenario of the devices and techniques that can be used to assess FA exposure. Moreover, in the design of FA assessment, some crucial aspects were considered, such as standard atmosphere generation for devices calibration. This review summarizes the tools and basics used in FA air monitoring, useful to organize a functional monitoring strategy for assessment of FA concentration levels. An insight into the sampling and analysis of FA is provided. Recent advances in solid sorbent technology allow analysts to use these devices coupled to chromatographic instruments. A comparison of the strengths and weaknesses of analytical methods (gas-/liquid-chromatography coupled with mass spectrometry or UV detection, chromogenic, colorimetric, electrochemical determination) and sampling devices (impregnated papers, solid sorbents, liquid sorbents, bubblers, impingers, micro-impingers, denuder samplers, sealed bags, canisters) methods are illustrated. This survey found that a monitoring strategy should be planned considering the most appropriate methodology in terms of costs and practicability. Therefore, it is necessary to know the aspects that can make the chosen strategy suitable and valid for the exposure scenario under investigation.

High-throughput screening of samples is the strategy of choice to detect occupational exposure biomarkers, yet it requires a user-friendly apparatus that gives relatively prompt results while ensuring high degrees of selectivity, precision, accuracy and automation, particularly in the preparation process. Miniaturization has attracted much attention in analytical chemistry and has driven solvent and sample savings as easier automation, the latter thanks to the introduction on the market of the three axis autosampler. In light of the above, this contribution describes a novel user-friendly solid-phase microextraction (SPME) off- and on-line platform coupled with gas chromatography and triple quadrupole-mass spectrometry to determine urinary metabolites of polycyclic aromatic hydrocarbons 1- and 2-hydroxy-naphthalene, 9-hydroxy-phenanthrene, 1-hydroxy-pyrene, 3- and 9-hydroxy-benzoantracene, and 3-hydroxy-benzo[a]pyrene. In this new procedure, chromatography&rsquo, s sensitivity is combined with the user-friendliness of N-tert-butyldimethylsilyl-N-methyltrifluoroacetamide on-fiber SPME derivatization using direct immersion sampling, moreover, specific isotope-labelled internal standards provide quantitative accuracy. The detection limits for the seven OH-PAHs ranged from 0.25 to 4.52 ng/L. Intra-(from 2.5 to 3.0%) and inter-session (from 2.4 to 3.9%) repeatability was also evaluated. This method serves to identify suitable risk-control strategies for occupational hygiene conservation programs.

The determination of urinary S-phenylmercapturic acid (S-PMA) represents the most reliable biomarker to monitor the intake risk of airborne benzene. Recently, the European Chemical Agency deliberated new occupational exposure limits for benzene and recommended an S-PMA biological limit value of 2-μg/g creatinine. This limit is an order of magnitude lower than the previous one, and its determination constitutes a challenge in the analytical field. We developed and validated a method that allows the fully automated and sensitive determination of S-PMA by the use of gas-chromatography negative chemical ionization tandem mass spectrometry in isotopic dilution. For negative chemical ionization, we selected a mixture of 1% isobutane in argon as reactive gas, by studying its chemical ionization mechanism and optimal parameters compared with pure isobutane or pure methane. This gas mixture produces a more abundant signal of the target analyte than isobutane or methane, and it extended the operative lifetime of the ion source, enabling us to start a high-throughput approach of the S-PMA analysis. Moreover, energy-resolved mass spectrometry experiments were carried out to refine the MS/MS analysis conditions, testing nitrogen and argon as collision gases. The method optimization was pursued by a chemometric model by using the experimental design. The quantification limit for S-PMA was 0.10 μg/L. Accuracy (between 98.3% and 99.6%) and precision (ranging from 1.6% to 6.4%) were also evaluated. In conclusion, the newly developed assay represents a powerful tool for the robust, reliable, and sensitive quantification of urinary S-PMA, and because of its automation, it is well suited for application in large environmental and biological monitoring.