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Silver-containing nanoparticles (AgCNPs) have attracted increasing concerns because of their potential adverse effects on aquatic ecosystems. However, minimal information is available regarding their concentration, distribution, and speciation in the actual environment. In this work, different species of AgCNPs, including silver nanoparticles (AgNPs), silver chloride (AgCl NPs) and silver sulfide (Ag 2 S NPs) in water and sediment samples from Taihu Lake were analyzed by a multistep selective dissolution method combined with single-particle inductively coupled plasma mass spectrometry. The results showed that the concentrations of AgCNPs in the water and sediment of Taihu Lake were in the range of 0.61 - 3.10 × 10 7 particles/L and 0.57 - 1.41 × 10 9 particles/g, respectively, with mean particle sizes of 22.84 ± 1.62 nm and 20.10 ± 4.57 nm. Spatial distribution analysis indicated that AgCNPs were significantly concentrated in the northern areas of Taihu Lake. Ag 2 S NPs were found to be the predominant component in both water and sediment. Based on the toxicological data of AgNPs, the predicted no-effect concentration of AgNPs on freshwater species was calculated to be 0.03 μg/L. The calculated risk quotient based on the concentrations of AgNPs obtained from the species analysis was less than 0.01, indicating a low ecological risk posed by AgNPs in the Taihu Lake. This work is critical for reliable risk assessment and regulation of AgCNPs., Competing Interests: Declaration of Competing Interest ☒ The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2025. Published by Elsevier Ltd.)

Metal-containing nanoparticles (MNPs) ubiquitously exist in the environment and organisms, playing distinct roles in the fate and toxicity of metals. However, the extraction and analysis of the MNPs in biological samples is still a great challenge and the interferences of other metal species and complex matrices remains unclear. In this work, we established a method for efficient extraction and accurate analysis of MNPs in biological samples to eliminate the interference caused by metal ions and biological matrices based on the alkali extraction and single particle mode inductively coupled plasma mass spectrometry (SP-ICP-MS). Obvious interference signals of lead-containing nanoparticles (PbNPs) were found in various biological matrices (liver, brain, bile, intestine, stomach), causing false positive results or overestimation of PbNPs. Then, a novel strategy using EDTA and ultrasonic during the TMAH extraction process were proposed to successfully eliminate the interferences due to the strong and competitively binding of EDTA to Pb ions, which was identified as ionic signals in SP-ICP-MS and resulted in the elimination of interferences. Finally, this method was successfully applied for the extraction, characterization and quantification of PbNPs in different biological tissues collected near a power plant, revealing the occurrence of PbNPs in stomach, intestine and liver tissues and indicating their oral exposure and potential translocation. This method could be universally applied for the efficient extraction and accurate analysis of MNPs in biological samples and thus provided a reliable and powerful tool for the investigation of the occurrence, fate and toxicity of MNPs in environmental and organisms., Competing Interests: Declaration of competing interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2024 Elsevier B.V. All rights reserved.)

Our work aimed to examine nanoparticle levels in 69 distinct pooled mussel samples along the Norwegian coastline, considering samples from different environmental contexts, including natural locations, potentially polluted hotspots, and mussel farms. Single-particle ICP-MS was utilized to determine particle mass and number concentrations at environmentally relevant levels in addition to the total content of 11 elements: aluminum, barium, cerium, copper, iron, manganese, lead, silicon, silver, titanium, and zirconium. Results showed nanoparticle mass concentrations of few ng/g up to tens of μg/g and number concentrations of 10 6 to 10 9 particles/g (wet weight). Certain urban and industrially impacted locations were linked to increased levels of, e.g., silver, lead, cerium, zirconium, and titanium NPs. Farmed mussels exhibited lower concentrations. However, natural variations were considerable, and impacted locations mostly did not differ from the highest levels in pristine areas. The study presents the first extensive survey of NPs of 11 different elements in marine biota and provides evidence of increased levels of NPs in areas with anthropogenic activities.

Information on the emission of coal combustion-sourced magnetite nanoparticles (MNPs) is lacking, which is critical for their health-related risks. In this study, MNPs in coal fly ashes (CFAs) from various coal-fired power plants (CFPPs) in China equipped with various dust removal devices were extracted and quantified using single particle ICP-MS. The number concentrations of MNPs in CFAs captured by dust removal increased with stage, while their size decreased. Among all the dust removal devices, electrostatic-fabric-integrated precipitators showed the best removal of MNPs. Furthermore, throughout all the coal combustion by-products in a typical CFPP, MNPs in EFA (fly ash escaped from the stack) showed the highest number concentration (1.2 × 10 7 particles/mg) and lowest size (78 nm). Although the mass of CFA escaping through the stack is extremely low, it still had an emission rate of 1.9 × 10 15 particles/h, contributing 3.56 % of the total emissions of MNPs in number. In addition, the purity of MNPs and their associated toxic metals showed a size-dependent variation pattern. As the particle size of MNPs decreased, the proportion of Fe in MNPs increased from 43 % in bottom ash (BA) to 84 % in EFA, while the abundance of trace toxic metals in EFA was 3.3 times higher than that of BA. These MNPs with the highest purity can adsorb elevated concentrations of toxic metals, and can be discharged directly into the atmosphere, posing a risk of synergistic toxicity., Competing Interests: Declaration of competing interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2024 Elsevier B.V. All rights reserved.)

The use of a new nanomaterial in the feed chain requires a risk assessment that involves in vitro gastrointestinal digestions to predict its degradation and oral exposure to nanoparticles. In this study, a nanosilver-based material was incorporated into pig and chicken feed as a growth-promoting additive and subjected to the corresponding in vitro gastrointestinal digestions. An inductively coupled plasma mass spectroscopy (ICP-MS) analytical platform was used to obtain information about the silver released in the different digestion phases. It included conventional ICP-MS for total silver determination, but also single particle ICP-MS and coupling to hydrodynamic chromatography for detection of dissolved and particulate silver. The bioaccessible fraction in the intestinal phase accounted for 8-13% of the total silver, mainly in the form of dissolved Ag(I) species, with less than 0.1% as silver-containing particles. Despite the additive behaving differently in pig and chicken digestions, the feed matrix played a relevant role in the fate of the silver., (© 2024. The Author(s).)

Resuspension of road dust is a major source of airborne particulate matter (PM) in urban environments. Inhalation of ultrafine particles (UFP; < 0.1 μm) represents a health concern due to their ability to reach the alveoli and be translocated into the blood stream. It is therefore important to characterize chemical properties of UFPs associated with vehicle emissions. We investigated the capability of Single-Particle ICP-MS (SP-ICP-MS) to quantify key metal(loid)s in nanoparticles (NPs; < 0.1 μm) isolated from road dust collected in Toronto, Canada. Water extraction was performed to separate the <1-μm fraction from two different road dust samples (local road vs. arterial road) and a multi-element SP-ICP-MS analysis was then conducted on the samples' supernatants. Based on the particle number concentrations obtained for both supernatants, the metal(loid)-containing NPs could be grouped in the following categories: high (Cu and Zn, > 1.3 × 10 11 particles/L), medium (V, Cr, Ba, Pb, Sb, Ce, La), low (As, Co, Ni, < 4.6 × 10 9 particles/L). The limit of detection for particle number concentration was below 5.5 × 10 6 particles/L for most elements, except for Cu, Co, Ni, Cr, and V (between 0.9 and 7.7 × 10 7 particles/L). The results demonstrate that road dust contains a wide range of readily mobilizable metal(loid)-bearing NPs and that NP numbers may vary as a function of road type. These findings have important implications for human health risk assessments in urban areas. Further research is needed, however, to comprehensively assess the NP content of road dust as influenced by various factors, including traffic volume and speed, fleet composition, and street sweeping frequency. The described method can quickly characterize multiple isotopes per sample in complex matrices, and offers the advantage of rapid sample scanning for the identification of NPs containing potentially toxic transition metal(loid)s at a low detection limit., Competing Interests: Declaration of competing interest The authors of this publication declare no conflicts of interest., (Crown Copyright © 2024. Published by Elsevier B.V. All rights reserved.)

Silver nanoparticles (AgNPs), widely used in various fields of technology as an antimicrobial agent, represent a new type of environmental pollutant. Through various routes, AgNPs might penetrate into agricultural crops and foodstuffs. It is important to know if AgNPs contained in food persist in digested food and are therefore available for entering the inner organs of the consumer's body. Using the technique of single-particle ICP-MS, we analysed the changes in the number and size distribution of AgNPs added to a sample of bread submitted to in vitro simulated gastrointestinal digestion. The majority of silver, in terms of mass, was transformed from the state of particles to the dissolved state during bread digestion, but the number of particles was reduced by 25% only. The most abundant particle size was reduced from 60 nm to 49 nm. Hence, a substantial part of transformed nanoparticles is still present in food digestate. This means that AgNPs consumed together with food can theoretically enter the inner cells of human body., Competing Interests: The authors declare no conflicts of interest.

The use of zinc oxide nanoparticles (ZnO NPs) in cosmetic and pharmaceutical industry has been increased in recent years due to their good properties as solar radiation filters and antibacterial agent. According to the literature, the potential toxicity of these NPs could be size-dependent and the amount of solubilized metal. This work investigates new reliable and straightforward methodologies that enables the determination of ZnO NPs, discriminating them from ionic zinc in cosmetic samples. Two different techniques of analysis have been applied in this study: high-resolution continuum source graphite furnace atomic absorption spectrometry (HR-CS-GFAAS), and "single particle" inductively coupled plasma mass spectrometry (sp-ICP-MS). Triton X-100 has been used as a surfactant for the formation of homogeneous and stable slurries which allowed the determination of the concentration and sizes of ZnO NPs and Zn 2+ in baby creams, eyeshadows, and lotions. A central composite design (CCD) was performed for the two techniques to optimize the concentration of Triton X-100 and sonication time. For validation purpose, the results of Zn 2+ and ZnO NPs contents achieved by HR-CS-GFAAS were compared with the total Zn content obtained by acid digestion of the samples. A size comparison of the ZnO NPs was also carried out with the data obtained through the two methodologies and validated with transmission electron microscopy (TEM). In the case of TEM analysis, two different media were tried to study possible agglomerates and interactions between the particles and the matrix., Competing Interests: Declaration of competing interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2023 The Authors. Published by Elsevier B.V. All rights reserved.)

Selenium is a non-essential element with beneficial and toxic effects on plants, whose exact role in plant physiology leaves many unanswered questions. Various species of hydroponically grown plants produce defined selenium nano particles (SeNP) with a narrow size distribution and about 2 million selenium atoms by biosynthesis when being exposed to selenite, proving that green synthesis of SeNP is not only possible in plants extracts, but also in living organisms. The detection was performed with single particle inductively coupled plasma mass spectrometry. These results require a new view of the selenium biochemistry in plants and its impact on nutrition, food sciences and medicine. To the best of our knowledge, this is the first report on the synthesis of elemental nanoparticles in general and selenium nanoparticles in particular by living plants.

Selenium is an essential trace element in human nutrition. Recent findings suggest that the biosynthesis of selenium nano particles (SeNPs) in plants might be a ubiquitous phenomenon. We investigated the potential of SeNP biosynthesis in food plants and our core objective was to explore the commonness and possible ubiquitousness of nano selenium in food plants and consequently in the human diet. By growing a variety of plants in controlled conditions and the presence of selenite we found strong evidence that SeNPs are widely present in vegetables. The shoots and roots of seven different plants, and additionally Brazil nuts, were analyzed with single-particle inductively coupled plasma mass spectrometry with a focus on edible plants including herbs and salads. SeNPs were found in every plant of our study, hence we conclude, that SeNPs are common ingredients in plant-based food and are therefore eaten daily by most humans. Considering the concerning worldwide prevalence of selenium deficiency and the great physiological properties of SeNPs, we see a high potential in utilizing this discovery.

Metal-based nanoparticles (NPs) attract increasing concerns because of their adverse effects on aquatic ecosystems. However, their environmental concentrations and size distributions are largely unknown, especially in marine environments. In this work, environmental concentrations and risks of metal-based NPs were examined in Laizhou Bay (China) using single-particle inductively coupled plasma-mass spectrometry (sp-ICP-MS). First, separation and detection approaches of metal-based NPs were optimized for seawater and sediment samples with high recoveries of 96.7% and 76.3%, respectively. Spatial distribution results showed that Ti-based NPs had the highest average concentrations for all the 24 stations (seawater, 1.78 × 10 8 particles/L; sediments, 7.75 × 10 12 particles/kg), followed by Zn-, Ag-, Cu-, and Au-based NPs. For all the NPs in seawater, the highest abundance occurred around the Yellow River Estuary, resulting from a huge input from Yellow River. In addition, the sizes of metal-based NPs were generally smaller in sediments than those in seawater (22, 20, 17, and 16 of 22 stations for Ag-, Cu-, Ti-, and Zn-based NPs, respectively). Based on the toxicological data of engineered NPs, predicted no-effect concentrations (PNECs) to marine species were calculated as Ag at 72.8 ng/L < ZnO at 2.66 µg/L < CuO at 7.83 µg/L < TiO 2 at 72.0 µg/L, and the actual PNECs of the detected metal-based NPs may be higher due to the possible presence of natural NPs. Station 2 (around the Yellow River Estuary) was assessed as "high risk" for Ag- and Ti-based NPs with risk characterization ratio (RCR) values of 1.73 and 1.66, respectively. In addition, RCR total values for all the four metal-based NPs were calculated to fully assess the co-exposure environmental risk, with 1, 20, and 1 of 22 stations as "high risk", "medium risk", and "low risk", respectively. This study helps to better understand the risks of metal-based NPs in marine environments., Competing Interests: Declaration of Competing Interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2023. Published by Elsevier Ltd.)

This work presents the role of commercial microfiltration membranes combined with single particle inductively coupled plasma-mass spectrometry (SP-ICP-MS) in removing environmental matrix interference for model silver nanoparticles (AgNPs) determination. The filters with different pore sizes (0.22 μm, 0.45 μm, 0.8 μm) and materials (mixed cellulose ester, polyether sulfone, and nylon) were investigated to acquire the recovery of particle concentration and size of AgNPs spiked into different real aqueous solutions, including ultrapure water, tap water, surface water, and sewage effluent. The maximum recovery of nanoparticle concentration was 70.2% through the 0.8 μm polyether sulfone membrane. The heated filters were able to improve the recovery of AgNPs particle concentration in the real aqueous environment. Hence, the pretreatment method by SP-ICP-MS combined with filtration membrane was simple, fast, and low-cost to quantify AgNPs in natural water environments., (© 2023. The Author(s), under exclusive licence to The Japan Society for Analytical Chemistry.)

The use of nanoparticles in agrichemical formula and food products as additives has increased their chances of accumulation in humans via oral intake. Due to their potential toxicity, it is critical to understand their fate and distribution following oral intake. Cerium oxide nanoparticle (CeO 2 NP) is commonly used in agriculture and is highly stable in the environment. As such, it has been used as a model chemical to investigate nanoparticle's distribution and clearance. Based on their estimated human exposure levels, 0.15-0.75 mg/kg body weight/day of CeO 2 NPs with different sizes and surface charges (30-50 nm with negative charge and <25 nm with positive charge) were gavaged into C57BL/6 female mice daily. After 10-d, 50% of mice in each treatment were terminated, with the remaining being gavaged with 0.2 mL of deionized water daily for 7-d. Mouse organ tissues, blood, feces, and urine were collected at termination. At the tested levels, CeO 2 NPs displayed minimal overt toxicity to the mice, with their accumulation in various organs being negligible. Fecal discharge as the predominant clearance pathway took less than 7-d regardless of charges. Single particle inductively coupled plasma mass spectrometry analysis demonstrated minimal aggregation of CeO 2 NPs in the gastrointestinal tract. These findings suggest that nanoparticle additives >25 nm are unlikely to accumulate in mouse organ after oral intake, indicating limited impacts on human health., Competing Interests: Declaration of Competing Interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper.

Due to the analytical challenges of detecting and quantifying nanoparticles in seawater, the data on distributions of NPs in the marine environment is limited to qualitative studies or by ensemble measurements subject to various analytical artifacts. Single particle inductively coupled plasma mass spectrometry (SP-ICP-MS) allows determination of individual inorganic NPs at environmentally relevant concentrations, yet only few studies have been conducted on selected elements in surface sea water. Here, a sequential multi-element screening method was developed and implemented to provide a first survey of the horizontal and vertical distributions of inorganic nanoparticles and trace elements in a pristine Norwegian fjord prospect for submarine tailings deposition. Statistical control of false-positive detections while minimizing the size detection limit was ensured using a novel raw signal processing. Scanning electron microscopy (SEM) and energy-dispersive X-ray spectroscopy (EDS) gave confirmative and qualitative information regarding particle morphology and composition. Following SP-ICP-MS screening for particles of 16 elements, particulate Al, Fe, Mn, Pb, Si and Ti were found and determined to mass concentrations in ng/L of 1-399, 1-412, below limit of detection (8 particles per liter. Total metals concentrations were at least an order of magnitude higher, at concentrations in μg/L of 1-12 for Al, 2-13 for Fe, 0.3-11 Mn, 0.02-0.5 for Pb, 46 to 318 Si and 0.04-0.4 for Ti. A strong depth dependence was observed for both trace elements and particles with concentrations increasing with depth. Our results provide a baseline for the fjord and new data on environmental levels of both total metals and metal containing nanoparticles including the vertical and horizontal distribution of natural nanoparticles., Competing Interests: Declaration of competing interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2023 The Authors. Published by Elsevier Ltd.. All rights reserved.)

Single particle-inductively coupled plasma-mass spectrometry (SP-ICP-MS) has become a powerful technique for the characterization of nanoparticles (NPs). However, the accuracy of the characterization of NPs by SP-ICP-MS is greatly affected by the data acquisition rate and the way of data processing. For SP-ICP-MS analysis, ICP-MS instruments typically apply microsecond to millisecond dwell times (10 μs-10 ms). Considering the duration of one nanoparticle event in the detector is 0.4-0.9 ms, NPs will show different data forms when working with microsecond and millisecond dwell times. In this work, the effects of dwell times from microsecond to millisecond (50 μs, 100 μs, 1 ms and 5 ms) on the data forms in SP-ICP-MS analysis are discussed. The data analysis and data processing for different dwell times is discussed in detail, including the measurement of transport efficiency (TE), the distinction of signal and background, the evaluation of diameter limit of detection (LOD d ) and the quantification of mass, size and particle number concentration (PNC) of NPs. This work provides data support for the data processing process and aspects to be considered in the characterization of NPs by SP-ICP-MS, which is expected to provide guidance and reference for researchers in SP-ICP-MS analysis., Competing Interests: Declaration of competing interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2023 Elsevier B.V. All rights reserved.)

Single particle inductively coupled plasma mass spectrometry (SP-ICP-MS) is a technique widely used to obtain direct information about the number concentration and the size distribution of nanoparticles in liquid suspensions. However, its methods still lack clear quality control strategies to confirm the validity of the information derived from them. Only the detection of the complete size distribution of the nanoparticles in a sample over the size critical value ensures obtaining unbiased quantitative information, otherwise information should be restricted to report the presence of nanoparticles over a certain size and number concentration since their actual total number concentration is underestimated and the size overestimated. Under the latter conditions, data processing produces histograms showing the tails of the incomplete size distributions, although apparently, complete distributions can also be obtained when particle events are recorded as peaks, as reported here for the first time. The occurrence of these misleading situations must be critically evaluated for each SP-ICP-MS analysis. An approach, based on estimation of size critical values and successive dilutions, is proposed for the assessment of the validity of the quantitative information obtained, together with specific criteria for reconsidering the information that can be derived from those measurements. The approach was verified with different case studies and applied to the analysis of complex nanomaterials, confirming the validity of the reported information by comparison with other techniques. A calculation tool is also included to facilitate the estimation of size critical values under experimental conditions., (© 2022. The Author(s).)

Background: This work studies the presence of the Ti, Al and V metal ions and Ti nanoparticles released from the debris produced by the implantoplasty, a surgical procedure used in the clinic, in rat organs., Methods: The sample preparation for total Ti determination was carefully optimized using microsampling inserts to minimize the dilution during the acid attack of the lyophilized tissues by a microwave-assisted acid digestion method. An enzymatic digestion method was optimized and applied to the different tissue samples in order to extract the titanium nanoparticles for the single-particle ICP-MS analysis., Results: A statistically significant increase was found for Ti concentrations from control to experimental groups for several of the studied tissues, being and particularly significant in the case of brain and spleen. Al and V concentrations were detected in all tissues but they were not different when comparing control and experimental animals, except for V in brain. The possible presence of Ti-containing nanoparticles mobilized from the implantoplasty debris was tested using enzymatic digestions and SP-ICP-MS. The presence of Ti-containing nanoparticles was observed in all the analyzed tissues, however, differences on the Ti mass per particle were found between the blanks and the digested tissue and between control and experimental animals in some organs., Conclusion: The developed methodologies, both for ionic and nanoparticulated metal contents in rat organs, have shown the possible increase in the levels of Ti both as ions and nanoparticles in rats subjected to implantoplasty., Competing Interests: Declaration of Competing Interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2023 The Authors. Published by Elsevier GmbH.. All rights reserved.)

The work described herein assesses the ability to characterize gold nanoparticles (Au NPs) of 50 and 100 nm, as well as 60 nm silver shelled gold core nanospheres (Au/Ag NPs), for their mass, respective size, and isotopic composition in an automated and unattended fashion. Here, an innovative autosampler was employed to mix and transport the blanks, standards, and samples into a high-efficiency single particle (SP) introduction system for subsequent analysis by inductively coupled plasma-time of flight-mass spectrometry (ICP-TOF-MS). Optimized NP transport efficiency into the ICP-TOF-MS was determined to be >80%. This combination, SP-ICP-TOF-MS, allowed for high-throughput sample analysis. Specifically, 50 total samples (including blanks/standards) were analyzed over 8 h, to provide an accurate characterization of the NPs. This methodology was implemented over the course of 5 days to assess its long-term reproducibility. Impressively, the in-run and day-to-day variation of sample transport is assessed to be 3.54 and 9.52% relative standard deviation (%RSD), respectively. The determination of Au NP size and concentration was of <5% relative difference from the certified values over these time periods. Isotopic characterization of the 107 Ag/ 109 Ag particles ( n = 132,630) over the course of the measurements was determined to be 1.0788 ± 0.0030 with high accuracy (0.23% relative difference) when compared to the multi-collector-ICP-MS determination.

Accurate quantification of nanoplastics (NPs) in complex matrices remains a challenge, especially for biological samples containing high content of organic matters. Herein, a new method extracting and quantifying polystyrene (PS) NPs from biological samples was developed. The extraction included alkaline digestion, centrifugation, and cloud point extraction (CPE), and the quantification included gold nanoparticles formation and labeling on surfaces of the extracted NPs and thereafter measurement with single particle inductively coupled plasma mass spectrometry (SP-ICP-MS). Results show that 25% tetramethylammonium hydroxide solution was an effective alkaline digestion solution for biological matrices, and CPE after centrifugation (3000 rpm, 10 min) was applicable to purify and enrich PS NPs with different sizes (100 and 500 nm) and surface functionalities (-COOH and -NH 2 modifications) from the digestion solution. The efficiency of Au labeling on PS NPs surface was improved by about 70% in the presence of 100 μM cetyltrimethylammonium bromide. The performance of the quantification method was examined by extraction and measurement of PS NPs spiked in four representative organism samples including bacteria, algae, nematode, and earthworm, and was further validated by analyzing the accumulated PS NPs in exposed nematodes. Good recovery rates (65 ± 10%-122 ± 22%) were achieved for spiking levels of 5-50 μg g -1 ; the limit of detection was 3.7 × 10 7 particles g -1 , corresponding to the mass concentration of about 0.02 and 2.5 μg g -1 for the 100 nm and 500 nm PS NPs, respectively. The established extraction and quantification methods are efficient and sensitive, providing a useful approach for further exploring the environmental behavior and toxicity of NPs., Competing Interests: Declaration of competing interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2022 Elsevier Ltd. All rights reserved.)

Selenium nanoparticles (SeNPs) have recently attracted attention because they combine the benefits of Se and lower toxicity compared to other chemical forms of this element. In this study, SeNPs were synthesized by a green method using ascorbic acid as the reducing agent and polyvinyl alcohol as stabilizer. The nanoparticles were widely characterized. To determine the total concentration of Se by ICP-MS, several isotopes and the use of He as collision gas were evaluated, which was effective in minimizing interferences. A method for sizing SeNPs by single particle ICP-MS (SP-ICP-MS) was developed. For this purpose, He and H 2 were evaluated as collision/reaction gases, and the second one showed promising results, providing an average diameter of 48 nm for the SeNPs. These results agree with those obtained by TEM (50.1 nm). Therefore, the SP-ICP-MS can be implemented for characterizing SeNPs in terms of size and size distribution, being an important analytical tool for Se and other widely studied nanoparticles (e.g. Ag, Au, Ce, Cu, Fe, Zn). Finally, the antibacterial activity of SeNPs was assessed. The SeNPs showed bacteriostatic activity against three strains of Gram-positive bacteria and were particularly efficient in inhibiting the growth E. faecalis even at very low concentrations (MIC < 1.4 mg l -1 ). In addition, a bactericidal activity of SeNPs against S. aureus was observed. These nanoparticles may have potential application in pharmaceutical industry, biomedicine and agriculture., (© 2022 IOP Publishing Ltd.)

The engineered silver nanoparticles (AgNPs) have been widely used in various food contact materials (FCMs) based on their antibacterial properties. This widespread use of nanosilver has, however, increased the risk of exposure of AgNPs to human due to their migration from FCMs causing a potential hazard present in foods. Therefore, it is important to establish a reliable and practical method for the detection of AgNPs in food matrices to support risk assessment on AgNPs exposure. Taking the examples of milk and AgNPs-containing breast milk storage bags, this study established an approach for size characterization and quantification of AgNPs in milk and evaluated the relevant silver migration, based on enzymatic digestion and the analysis by asymmetric flow field-flow fractionation (AF4) hyphenated with inductively coupled plasma mass spectrometry (ICP-MS) and single particle inductively coupled plasma mass spectrometry (SP-ICP-MS). No migration of AgNPs was found from breast milk storage bags under various simulated storage conditions as well as extreme scenarios. The suitability and reliability of this method were also validated by the determination of multiple parameters, including accuracy, repeatability, limit of detection (LOD), limit of quantification (LOQ), and recovery, for AF4-ICP-MS and SP-ICP-MS, respectively, with good and overall acceptable evaluation results obtained for all. The established and validated approach was demonstrated to be suitable for the characterization and quantitation of AgNPs in milk as well as the analysis of their migration from breast milk storage bags.

Nowadays consumers have constantly exposed to nanoparticles (NPs) ingestion. Although the impact of NPs on the human has been studied by many authors, they did not consider the influence of food matrix components on bioaccessibility of NPs. This fact has encouraged us to investigate the influence of different food components on NPs. The investigation has been carried out to assess the influence of main food components on the MNPs (metallic nanoparticles) fate during the in vitro gastrointestinal simulation. The experiments have been carried out with the single-particle inductively coupled plasma mass spectrometry (SP-ICP-MS) as a tool for quantitative and qualitative analysis and the scanning transmission electron microscopy (STEM) as a means of qualitative analysis. The influence of various food components on NPs has been confirmed and it may be concluded that the matrix has an impact on the size and form of NPs. The presence of food components significantly changes the behaviour of NPs during simulated gastrointestinal digestion. Possible explanations of the influence of main nutrient groups, i.e. lipids, protein, salts, saccharides and vitamins on NPs have been proposed., (Copyright © 2021 The Author(s). Published by Elsevier Ltd.. All rights reserved.)

Bimetallic nanoparticles (NPs), including core-shell structure and bimetallic alloy nanoparticles, were synthesized and characterized using flow field-flow fractionation (FlFFF), single particle inductively coupled plasma mass spectrometry (SP-ICP-MS), and transmission electron microscope (TEM) with energy-dispersive x-ray spectroscopy (EDS). For the core-shell particles, a nominal 80 nm commercial core-shell AuAg bimetallic nanoparticle was used to examine the applicability of SP-ICP-MS to determine the core size of Au and shell thickness of Ag. Then, the method was applied to estimate the core size of Au and shell thickness of Ag for the laboratory synthesized particles. The results were compared with those obtained from TEM-EDS. For the alloy nanoparticles, two synthesis protocols, based on the galvanic replacement of Ag seed particles with Au, were used. One was to prepare a hollow AgAu particle by varying the volume of dissolved Au in basic solution (K-gold) to etch some parts of AgNPs to dissolved ionic silver with the formation of AuNPs covering the remaining AgNPs, producing a hole inside the core nanoparticles. Another protocol was to prepare AgAu alloy nanoparticles. SP-ICP-MS was used in combination with FlFFF to provide information on the changes of particle size with varying volume of K-gold reagent. Hydrodynamic diameter increased with increasing K-gold, as observed by FlFFF. With SP-ICP-MS without prior FlFFF, bimodal distributions were observed in the size distribution of Au and Ag. With prior FlFFF, monomodal distributions were observed by SP-ICP-MS, which allow the use of particle concentration and size to estimate the mass concentration of elements on the fractionated bimetallic nanoparticles. This study illustrates the potential use of SP-ICP-MS for gaining information about particle transformation during the synthesis of bimetallic nanoparticles., (Copyright © 2021 Elsevier B.V. All rights reserved.)

In recent years, single particle inductively coupled plasma mass spectrometry (SP-ICP-MS) has become a powerful tool for biological quantitative analysis. Homogeneous analysis method requires no separation and washing steps, which is suited for the analysis of highly infectious pathogens, so as to reduce the risk of infection during the operation. SARS-CoV-2 spreads all over the world, and its early infection symptoms are similar to influenza, which brings inconvenience to triage. Therefore, developing novel analytical method for simultaneous detection of multiple viral nucleic acids is essential. Taking the advantages of SP-ICP-MS and homogeneous analysis strategy, a SP-ICP-MS homogeneous nucleic acid assay by using gold nanoparticles (Au NPs) and silver nanoparticles (Ag NPs) probes was established for simultaneous sensitive analysis of SARS-CoV-2 and influenza A (H3N2). In the present of target SARS-CoV-2 or H3N2 nucleic acids, corresponding Au NPs or Ag NPs probes form larger aggregates, resulting in increased pulse signal intensity and reduced pulse signal frequency of the corresponding NPs in SP-ICP-MS measurement. In this assay, the reaction system of Au NPs and Ag NPs probes does not interfere with each other, and there was no separation and washing procedure, which facilitates operation, saves the analysis time, and improves the analysis efficiency. The linear range of this method is 5-1000 pmol L -1 , with low-level limits of quantification of target nucleic acid. The developed SP-ICP-MS simultaneous homogeneous detection method has a good potential for detecting nucleic acid, protein, cell and other biological samples by changing different modification sequences on the NPs probes., Competing Interests: Declaration of competing interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2021 Elsevier B.V. All rights reserved.)

Children are potentially exposed to products that contain nanoparticles (NPs). In particular, silver NPs are commonly present both in products used by and around children, primarily due to their antibacterial properties. However, very few data are available regarding the ability of silver NPs to penetrate through the oral mucosa in children. In the present work, we used baby porcine buccal mucosa mounted on vertical Franz diffusion cells, as an in vitro model to investigate penetration of silver NPs (19 ± 5 nm). Permeability experiments were performed using pristine physiologically-relevant saline solution in the receiver chamber and known concentrations of NPs or ions in the donor chamber; conditions mimicked the in vivo physiological pH conditions. After physicochemical characterization of silver nanoparticles dispersed in physiological solution, we evaluated the passage of ions and NPs through the mucosa, using single particle inductively coupled plasma mass spectrometry. A flux of 4.1 ± 1.7 ng cm -2  min -1 and a lag time of 159 ± 17 min were observed through mucosa exposed to silver nanoparticles. The latter suggests nanoparticle penetration through the baby porcine mucosa and release Ag + ions in the receptor fluid, as confirmed by computational model. Due to physiological similarity between human and pig membranes it is reasonable to assume that a trans-oral mucosa penetration could occur in children upon contact with silver nanoparticles.

The quantitative analysis of nanoparticles (NPs) in the environment is significantly important for the exploration of the occurrence, fate, and toxicological behaviors of NPs and their subsequent environmental risks. Some protocols have been recommended for the separation and extraction of NPs that are potentially dispersed in complex environmental matrixes, e.g. sediments and soils, but they remain limited. However, certain factors that may significantly affect extraction efficiency have not been comprehensively explored. In this study, on the basis of the single-particle inductively coupled plasma mass spectrometry (SP-ICP-MS) technique, a simple standardized protocol for separating and analyzing metal-containing NPs in sediment samples was developed. On consideration of the extraction efficiencies of indigenous NPs (Ti- and Zn-NPs) and spiked NPs (Ag- and Au-NPs) in sediments, sedimentation with a settling time of 6 h is recommended for the separation of NPs and large particles, and the optimal sediment to water ratio, ultrasonication power, time, and temperature are 0.4 mg/mL, 285 W, 20 min, and 15-25 °C, respectively. On the basis of the optimized method, the recoveries of spiked Ag and Au-NPs were 71.4% and 81.1%, respectively. The applicability of the optimal protocols was verified, and TOC was proved to be an important factor controlling the separation and extraction of NPs in environmental samples. The separation and extraction of NPs in elevated TOC samples can be improved by increasing the ultrasonication power, time, and temperature.

Characterization of nanoparticles (NPs) in coal fly ashes (CFAs) is critical for better understanding the potential health-related risks resulting from coal combustion. Based on single-particle (SP)-inductively coupled plasma mass spectrometry (ICP-MS) coupled with transmission electron microscopy techniques, this study is the first to determine the concentrations and sizes of metal-containing NPs in low-rank coal-derived fly ashes. Despite only comprising a minor component of the studied CFAs by mass, NPs were the dominant fraction by particle number. Fe- and Ti-containing NPs were identified as the dominant NPs with their particle number concentration ranging from 2.5 × 10 7 to 2.5 × 10 8 particles/mg. In addition, the differences of Fe-/Ti-containing NPs in various CFAs were regulated by the coalification degree of feed coals and combustion conditions of all of the low-rank CFAs tested. In the cases where these NPs in CFAs become airborne and are inhaled, they can be taken up in pulmonary interstitial fluids. This study shows that in Gamble's solution (a lung fluid simulant), 51-87% of Fe and 63-89% of Ti (ratio of the mass of Fe-/Ti-containing NPs to the total mass of Fe/Ti) exist in the NP form and remain suspended in pulmonary fluid simulants. These NPs are bioavailable and may induce lung tissue damage.

Silver-based nanoparticles (Ag-b-NPs) are currently a cause for concern because they are being produced in increasing quantities for use in industrial goods and consumer products. This goes hand in hand with their release to the environment and the resultant risks for the entire ecosystem. Therefore, it is essential that these materials are monitored. A promising technique that overcomes a number of shortcomings in handling environmental samples is magnetic solid phase extraction (MSPE) of Ag-b-NPs, which is applied in this study. It has been possible to extract different kinds of Ag-b-NPs at environmentally relevant concentrations in the low ng L -1 range using iron oxide magnetic particles (IOMPs) of different size and shape with efficiencies in the range from 80 to 100%. Furthermore, environmentally relevant inorganic ions and TiO 2 particles exhibited no major effect on the extraction efficiency. However, natural organic matter (NOM) exhibited a significant influence from 1 mg L -1 resulting in a 50% drop in extraction efficiency. This effect could be overcome by adding 10 mM Ca 2+ or increasing the iron oxide magnetic particle (IOMP) concentration to 500 mg L -1 . Applying the presented procedure, Ag-b-NPs added to a river water sample at β Ag  = 50 ng L -1 were successfully extracted. We also investigated the coextraction of Ag + , demonstrating that NOM could eliminate coextraction. The subsequent species-selective elution of Ag 2 S-NPs after MSPE, was carried out based on ethylene diamine tetraacetate (EDTA) as eluent in different matrices. A desorption efficiency of 76 ± 6% could be achieved while preserving the Ag 2 S-NPs' size. By contrast, core Ag-NPs and AgCl-NPs are dissolved if the presented method is followed., (Copyright © 2020 Elsevier B.V. All rights reserved.)

Copper oxide nanoparticles (CuO-NP) are used as an efficient alternative to conventional Cu in agriculture and might end up in soils. They show a high toxicity towards cells and microorganisms, but only low toxicity towards soil invertebrates. However, most existing soil ecotoxicological studies were conducted in a sandy reference soil and at test concentrations ≥100 mg Cu/kg soil. Therefore, there is a knowledge gap concerning the effect of soil texture on the toxicity of CuO-NP at lower, more realistic test concentrations. In our study, a sandy reference soil and three loamy soils were spiked with CuO-NP at up to four concentrations, ranging from 5 to 158 mg Cu/kg. We investigated 28-day reproduction as well as weight and Cu content after 14-day bioaccumulation and subsequent 14-day elimination for the springtail Folsomia candida. For the first time we analysed the size distribution of CuO-NP in aqueous test soil extracts by single particle-ICP-MS which revealed that the diameter of CuO-NP significantly increased with increasing concentration, but did not vary between test soils. Negative effects on reproduction were only observed in loamy soils, most pronounced in a loamy-acidic soil (-61%), and they were always strongest at the lowest test concentration. The observed effects were much stronger than reported by other studies performed with sandy soils and higher CuO-NP concentrations. In the same soil and concentration, a moderate impact on growth (-28%) was observed, while Cu elimination from springtails was inhibited. Rather than Cu body concentration, the diameter of the CuO-NP taken up, as well as NP-clay interactions might play a crucial role regarding their toxicity. Our study reports for the first time toxic effects of CuO-NP towards a soil invertebrate at a low, realistic concentration range. The results strongly suggest including lower test concentrations and a range of soil types in nanotoxicity testing., Competing Interests: Declaration of competing interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2020 Elsevier Ltd. All rights reserved.)

Background: The transformation of nanoparticles (NPs) internalized in plant tissues is the human digestive system that can provide a better understanding of the impact of NPs on the human system. The presented methodology was developed to study the bioaccessibility of cerium oxide (CeO 2 ) and copper oxide (CuO) NPs from radish after the in vitro simulation of gastrointestinal digestion using single-particle inductively coupled plasma mass spectrometry (SP-ICP-MS)., Results: Radish plants were cultivated hydroponically in a growth medium containing: (i) CeO 2 NPs and (ii) CuO NPs. Both cerium (Ce) and copper (Cu) were found in all organs of the radish plants after analysis by standalone ICP-MS. This confirms the bioaccumulation of CeO 2 and CuO NPs and the translocation of their Ce and Cu to the aerial parts of the plant. Less Ce (4.095 μg g -1 ) has been detected in leaves than in roots (1.156 mg g -1 ) while Cu content in leaves was 5.245 μg g -1 and in roots was 10.41 μg g -1 . Analysis of the digestive extracts obtained after the in vitro simulation of gastro (pepsin) and gastrointestinal (pancreatin) digestion showed that Ce has easy access to human system at least by 73%., Conclusion: The size of CeO 2 NPs in digestive extracts showed no significant changes. However, the results obtained for CuO NPs digestion were variable and suggested that CuO NPs dissolved during the digestion process. The CuO NPs were observed in roots after the gastrointestinal digestion concluding that CuO NPs recovered after the initial dissolution. © 2020 Society of Chemical Industry., (© 2020 Society of Chemical Industry.)

With the extensive application of nanotechnology, metal nanoparticles (MNPs) have been widely used, thus are universally detected in the environment. This has caused increasingly concerns due to their toxicity and the potential health risks they pose to humans. In this work, the concentrations and particle size distributions of MNPs and concentrations of associated metal ionic species in shellfish seafood (clams and oysters) were investigated using single particle inductively coupled plasma mass spectrometry (sp-ICP-MS) and inductively coupled plasma mass spectrometry (ICP-MS). The MNPs in the clam and oyster tissues were extracted via an alkaline digestion method with a recovery rate of 95.9% (for gold nanoparticles (AuNPs)). Then total concentrations of 41 metal elements were measured in the two types of seafood, of which 20 were selected for sp-ICP-MS analysis. The results showed that 5 types of MNPs were detectable in clams (Y, La, Ce, Pr, Gd) and 5 types of MNPs were detectable in oysters (Y, La, Ce, Pr, Nd). Size distributions of MNPs in clams and oysters were in the range of 35-55 nm and 30-65 nm, respectively. Nanoparticle concentrations in clams and oysters ranged from 0.6 to 37.7 ng/g and 4.2-19.7 ng/g, and accounted for 3.4%-50% and 5.5%-46% of the total metal content, respectively. Based on this analysis, the health risks of metals in the two kinds of seafood were evaluated by comparing the Provisional Tolerable Weekly Intake (PTWI) with limits recommended by the World Health Organization (WHO)/Food and Agriculture Organization (FAO). These results provide important information about the presence of metal nanoparticles in seafood and, to the best of our knowledge, this is the first time that the nanoparticles of rare earth elements have been detected and reported in bivalve mollusc tissues., Competing Interests: Declaration of competing interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2020 Elsevier Inc. All rights reserved.)

Effluent from wastewater treatment plants contains a wide variety of engineered nanoparticles (ENPs) released from different sources. Although single type ENPs have been studied extensively with respect to their environmental impact, ENPs in mixed forms have not been investigated much at environmentally relevant concentrations. This study was designed to test the effect of mixed ENPs at three combinations and concentrations on an aquatic bacterial community. After mixing artificial treated wastewater with river water and exposing the microbial community to ENPs for three days, the ENPs were characterized by SP-ICP-MS. Results from this study showed that: 1) the size distribution of Ti and Zn at the beginning and end of the experiment did not vary much among all tested conditions. For Ag, the most frequent size increased more than 2-fold when the highest Ag ENPs were added; 2) particle concentrations of ENPs generally correlated positively with added concentrations; 3) dissolved Zn and Ag increased significantly as a result of spike; and 4) the bacterial community structure was shifted significantly as a consequence of ENPs' addition. With the dominant population being suppressed, the community exposed to ENPs became more diverse and even. Surprisingly, further increase of the doses of the three ENPs did not bring significant change to the microbial community. These results revealed that ENPs could bring significant impacts to prokaryotes even at low concentrations. But these impacts do not necessarily correlate positively with doses., (Published by Elsevier Ltd.)

This work demonstrates the effect of NaCl and carbon-related interferences on the analysis of arsenic and silver nanoparticles (NPs) by single-particle inductively coupled plasma mass spectrometry. Spectral interference caused by ArCl + ions disturbing arsenic NPs analysis was eliminated using ammonia as reaction gas in a dynamic reaction cell of inductively coupled plasma mass spectrometer. In comparison to aqueous dispersions, non-spectral interferences caused by sodium lead to under-evaluation of arsenic and silver NPs diameter by about 7% and 15% at NaCl concentration of 450 mg L -1 and about 28% and 41% at NaCl concentration of 4500 mg L -1 , respectively. As a consequence of lower transport efficiency, sodium non-spectral interferences also lead to about a 9% lower number of detected NPs for dispersions of both arsenic and silver NPs in 4500 mg L -1 NaCl. On the contrary, measurement of NPs in matrices containing methanol gives results where Ag and As NPs diameter is over-evaluated by about 3% and 15% at a methanol content of 1% (v/v) and about 6% and 20% at a methanol content of 2% (v/v), respectively, in comparison to aqueous dispersions. In addition, the organic carbon species behave as surfactants and increase the transport efficiency; this leads to an increase in the determined number concentration of NPs. In comparison to aqueous dispersions, this is over-evaluated by about 17% for Ag NPs and about 10% for As NPs at a methanol content of 5% (v/v)., (Copyright © 2019 Elsevier B.V. All rights reserved.)

The use of nanomaterials is increasing but the real risk associated with their use in humans has to be defined. In fact, nanomaterials tend to accumulate in organs over a long period of time and are slowly degraded or eliminated by the body. Exosomes are nanovesicles actively shuttle molecules, including chemical products and metals, through the body. Macrophages scavenge the body from both organic and inorganic substances, and they use to release high amounts of exosomes. We hypothesized that macrophages may have a role in eliminating nanomaterials through their exosomes. We treated human primary macrophages with 20 nm gold nanoparticles (AuNPs), analyzing the presence of AuNPs in both cells and the released exosomes by the implementation of different techniques, including SP-ICP-MS and NTA. We showed that macrophages endocytosed AuNPs and released them through exosomes. Our study on one hand provide the evidence for a new methodology in the early identification of the nanomaterials levels in exposed subjects. On the other hand we depict a way our body shuttle virtually intact nanoparticles through macrophage-released exosomes., (Copyright © 2019 Elsevier B.V. All rights reserved.)

A reliable sample pre-treatment based on enzymatic hydrolysis has been fully optimized and validated for TiO 2 NPs isolation and determination/characterization in surimi (crab sticks). Efficient extractions have been found when using a pancreatin/lipase mixture at pH 7.4 and 37 °C for 12 h under continuous stirring. The proposed sample pre-treatment procedure has been found not to change TiO 2 NPs size distribution, therefore guaranteeing TiO 2 NPs integrity. TiO 2 NPs determination (TiO 2 NPs concentration) and TiO 2 NPs characterization (size distribution) were assessed by single-particle inductively coupled plasma mass spectrometry (sp-ICP-MS) working with dwell times in the microsecond range (high frequency of data acquisition). Method validation was performed for TiO 2 NPs concentrations and TiO 2 NPs sizes. Good repeatability (25% and 8% for TiO 2 NPs concentration and TiO 2 NPs most frequent size), and sensitivity (limit of detection of 5.28 × 10 5 NPs g -1 for TiO 2 NPs concentrations, and 31.3-37.1 nm for TiO 2 NPs size) were obtained. Accuracy, calculated through analytical recovery was adequate. Recoveries for TiO 2 NPs standards of 50 and 100 nm were 108 ± 5 and 105 ± 4%, respectively. The proposed methodology was applied to several surimi samples for assessing TiO 2 NPs concentrations and size distribution. Some surimi samples were found to contain TiO 2 NPs (concentrations from 1.40 × 10 7 to 1.19 × 10 9 NPs g -1 ). TiO 2 NPs size distributions were very different among the samples, and some of them showed wide size ranges (the most frequent size varied from 53.8 to 62.1 nm; whereas, the mean size values were within the 73.4-217.5 nm range)., (Copyright © 2018 Elsevier B.V. All rights reserved.)

A variety of food and drink samples (n = 21) were analyzed to evaluate the presence of (nano-) particles in their composition. After assessment of the sample pre-treatment step, a fast screening analysis was performed for drinks by Dynamic Light Scattering showing particles from 10 to 300 nm that could correspond to organic or metallic NPs. Metallic NPs were identified in foods by Single-Particle mode Inductively Coupled Plasma Mass Spectrometry and Asymmetrical Flow Field-Flow Fractionation coupled to Multiangle Laser Light Scattering and Inductively-Coupled Plasma Mass Spectrometry. The determination of Ti, Si and Ag concentration in the initial food suspensions, after filtration and centrifugal ultrafiltration enabled to estimate the ionic and nanoparticles content. Si-containing particles can be present in cappuccino powder as large aggregates and Si- and Al-containing particles in hot chocolate. Ti-containing NPs (80-200 nm) were found in chewing gum and Ag NPs in silver pearls (50-150 nm) used for decoration pastry., (Copyright © 2018 Elsevier Ltd. All rights reserved.)

With the increase in the application of nano-consumer products containing engineered nanoparticles (NPs), the unintended environmental exposure to NPs has been inevitable. Because of the bioaccumulation of NPs, concern about their potential cytotoxicity to aquatic organisms is also growing. Although measuring tools for analyzing particle size and/or concentration of NPs in intracellular uptake of tissues have been well developed, a simultaneous analysis of the two characteristics is difficult. The objective of this study was to use single particle-inductively coupled plasma-mass spectrometry (sp-ICP-MS) to measure the bioaccumulation and particle size changes of NPs exposed to zebrafish (Danio rerio) for 7 days. The uptake of NPs in the liver, intestine, and gill tissues was confirmed by electron microscopic (EM) analysis. However, the primary particle size of NPs in tissues could not be determined by the EM analysis. Therefore, sp-ICP-MS coupled with alkaline digestion was used for the easy extraction and immediate analysis of NPs from tissues. Zebrafish were exposed to four NPs (30 and 80 nm gold/silver NPs; AuNPs/AgNPs). Uptake amounts of AgNPs in the liver and intestine were significantly higher than those of AuNPs. Although larger NPs were finally accumulated in the liver and intestine tissues, most of the smaller NPs were filtered in the gills. The sp-ICP-MS method coupled with alkaline digestion enabled the accurate analysis of size, size distribution, and mass concentration of NPs in an aquatic organism., (Copyright © 2018 Elsevier Ltd. All rights reserved.)

Applicability of single-particle inductively coupled plasma mass spectrometry (sp-ICP-MS) using dwell times equal to or shorter than 100 μs has been tested for assessing titanium dioxide nanoparticles (TiO 2 NPs) in bivalve mollusks. TiO 2 NPs isolation from fresh mollusk tissues was achieved by ultrasound assisted enzymatic hydrolysis procedure using a pancreatin/lipase mixture. Optimum extraction conditions imply ultrasonication (60% amplitude) for 10 min, and 7.5 mL of a solution containing 3.0 g L -1 of pancreatin and lipase (pH 7.4). The developed method was found to be repeatable (repeatability of 17% for the over-all procedure, TiO 2 NPs concentration of 5.33 × 10 7  ± 8.89 × 10 6 , n = 11), showing a limit of detection of 5.28 × 10 6 NPs g -1 , and a limit of detection in size of 24.4-30.4 nm, based on the 3σ criteria, and on the 3σ/5 σ criteria, respectively. The analytical recovery within the 90-99% range (use of TiO 2 NPs standards of 50 nm at 7 and 14 μg L -1 as Ti). Several bivalve mollusks (clams, cockles, mussels, razor clams, oysters and variegated scallops) were analyzed for total titanium (ICP-MS after microwave assisted acid digestion), and for TiO 2 NPs by the proposed method. TiO 2 NPs concentrations were within the 2.36 × 10 7 -1.25 × 10 8 NPs g -1 range, and the most frequent sizes were from 50 to 70 nm., (Copyright © 2018 Elsevier B.V. All rights reserved.)

In recent years, silver nanoparticles (AgNPs) have attracted significant attention in medicinal, biomedical, and pharmaceutical research owing to their valuable physicochemical and antibacterial properties. Leaf sap extract (LSE) from Aloe arborescens can be used as an active ingredient for different biological applications, including wound healing. In this study, we have investigated the use of LSE from A. arborescens as a reducing, stabilizing and capping agent to produce AgNPs during the so called "green synthesis" (G-AgNPs). The objective of this study was to prepare, characterize and evaluate the potential of G-AgNPs against human pathogenic bacteria for the intended use as treatment of infected wounds. When the mixture of silver nitrate solution and LSE was exposed to direct sunlight it yielded a rapid color change from colorless to reddish-brown, indicating the formation of G-AgNPs. Physicochemical characterization such as Single particle inductively coupled plasma mass spectrometry, High resolution transmission electron microscopy and surface chemistry studies (Fourier transform infrared spectroscopy and X-Ray diffraction) revealed a small size in the range of 38±2nm, smooth surface and existence of LSE on the G-AgNPs. G-AgNPs possessed good antibacterial activity against both Pseudomonas aeruginosa and Staphylococcus aureus. The flow cytometry study revealed the increased percentage of dead cells treated by G-AgNPs through cell membrane damage, and it was further confirmed by confocal laser scanning microscopy. Thus, the present study reveals that the novel G-AgNPs demonstrated effective antibacterial properties against both Gram-negative and Gram-positive bacterial strains and shows great potential for its use in the treatment of pathogen infected wounds., (Copyright © 2017 Elsevier B.V. All rights reserved.)

Cosmetics are part of the daily life of most of the people. Thus, a complete characterization of the products we applied in our skin is necessary. In this work, an analytical investigation of a wide variety of cosmetics from the point of view of total element content and metallic nanoparticles (NPs) has been performed. Firstly, we analyzed the total element content by ICP-MS and ICP-OES after acid digestion as an assessment of the presence of metal impurities. Prohibited elements in cosmetics, according to the European Commission regulation No 1223/2009, were not detected, and only elements mentioned in the label were found (e.g. Al, Fe, Ti and Si). Secondly, a screening of the presence of NPs has been performed by Dynamic Light Scattering (DLS) and Single Particle Inductively-Coupled Plasma Mass Spectrometry (SP-ICP-MS). Two sample preparation procedures were applied. The first protocol consisted in the preparation of suspensions in 0.1% w/v SDS and the second based on defatting with hexane followed by resuspension in water. DLS was employed as a routine method for a fast analysis of NPs, but this technique showed limitations due to the lack of specificity. SP-ICP-MS analyses were then performed, first as a screening technique to evaluate the presence of TiO 2 and Au NPs in cosmetics suspensions prepared in SDS; and second, when a positive answer was obtained about the presence of NPs from the screening, SP-ICP-MS was used for particle size determination. Results showed that only TiO 2 NPs were present in two sunscreens, one anti-wrinkle day cream, one lip balm protector labeled as 'nano' and in one brand of toothpaste not labeled as 'nano'. Sizes obtained for both sample preparations were compared and ranged from 30 to 120nm in most of the samples., (Copyright © 2017 Elsevier B.V. All rights reserved.)

It is challenging to separate and measure the physical and chemical properties of monometallic and bimetallic engineered nanoparticles (NPs), especially when mixtures are similar in size and at low concentration. We report that single particle inductively coupled mass spectroscopy (SP-ICP-MS), alongside field flow fractionation (FFF), has allowed for the accurate measurement of size and particle number concentrations of mixed metallic nanoparticles (NPs) containing monometallic NPs of gold (Au) and silver (Ag) and a bimetallic core-shell structured NP (Au@Ag) of equivalent size. Two sets of these NPs were measured. The first contained only 60nm particles, where the Au@Ag NP had a 30nm core and 15nm shell to make a total diameter of 60nm. The second contained only 80nm particles (Au@Ag NP core particle of 50nm with a 15nm shell). FFF separation was used here as a sizing technique rather than a separation technique. It was used to confirm that suspensions containing either individual or mixtures of the Au 60nm, Ag 60nm and AuAg 60nm suspensions eluted together and were of the same size. Similarly, FFF was used to show that suspensions containing individual or mixtures of the equivalent 80nm, eluted together and were of the same size. Although the 60nm and 80nm suspensions did not elute at the same time they were not run together. SP-ICP-MS is then used to identify the size and concentration of the particles within the suspension. Successful separation of the NPs was effected and the limits of the instrument were obtained., (Copyright © 2016 Elsevier B.V. All rights reserved.)

The quality of the quantitative information in single-particle inductively coupled plasma mass spectrometry (SP-ICP-MS) depends directly on the number concentration of the nanoparticles in the sample analyzed, which is proportional to the flux of nanoparticles through the plasma. Particle number concentrations must be selected in accordance with the data acquisition frequency, to control the precision from counting statistics and the bias, which is produced by the occurrence of multiple-particle events recorded as single-particle events. With quadrupole mass spectrometers, the frequency of data acquisition is directly controlled by the dwell time. The effect of dwell times from milli- to microseconds (10 ms, 5 ms, 100 μs, and 50 μs) on the quality of the quantitative data has been studied. Working with dwell times in the millisecond range, precision figures about 5 % were achieved, whereas using microsecond dwell times, the suitable fluxes of nanoparticles are higher and precision was reduced down to 1 %; this was independent of the dwell time selected. Moreover, due to the lower occurrence of multiple-nanoparticle events, linear ranges are wider when dwell times equal to or shorter than 100 μs are used. A calculation tool is provided to determine the optimal concentration for any instrument or experimental conditions selected. On the other hand, the use of dwell times in the microsecond range reduces significantly the contribution of the background and/or the presence of dissolved species, in comparison with the use of millisecond dwell times. Although the use of dwell times equal to or shorter than 100 μs offers improved performance working in single-particle mode, the use of conventional dwell times (3-10 ms) should not be discarded, once their limitations are known.

Detection and sizing of natural colloids involved in the release and transport of toxic metals and metalloids is essential to understand and model their environmental effects. Single-particle inductively coupled plasma mass spectrometry (SP-ICP-MS) was applied for the detection of arsenic-bearing particles released from mine wastes. Arsenic-bearing particles were detected in leachates from mine wastes, with a mass-per-particle detection limit of 0.64 ng of arsenic. Conversion of the mass-per-particle information provided by SP-ICP-MS into size information requires knowledge of the nature of the particles; therefore, synchrotron-based X-ray absorption spectroscopy (XAS) was used to identify scorodite (FeAsO4·2H2O) as the main species in the colloidal particles isolated by ultrafiltration. The size of the scorodite particles detected in the leachates was below 300-350 nm, in good agreement with the values obtained by TEM. The size of the particles detected by SP-ICP-MS was determined as the average edge of scorodite crystals, which show a rhombic dipyramidal form, achieving a size detection limit of 117 nm. The combined use of SP-ICP-MS and XAS allowed detection, identification, and size determination of scorodite particles released from mine wastes, suggesting their potential to transport arsenic. Graphical abstract Analytical approach for the detection and size characterization of As-bearing particles by SP-ICP-MS and XAS in environmental samples.

Research focused on assessing potential consumer exposure to nanoparticles released from nano-enabled food-contact materials (FCMs) has often reached conflicting conclusions regarding the detection of migrating nanoparticles. These conflicting conclusions, coupled with the potential for nanoparticles to be unstable in certain food simulants, has necessitated a closer look at the role played by food simulants recommended for use in nanoparticle migration evaluation. The influence of aqueous food simulants on nanoparticles under migration evaluation conditions is reported herein. The stability of silver nanoparticles (AgNP) spiked into three food simulants (water, 10% ethanol and 3% acetic acid) was investigated using asymmetric flow field-flow fractionation (AF4), ultrafiltration, electron microscopy (EM), and single-particle inductively coupled plasma mass spectrometry (sp-ICP-MS). While 3% acetic acid induced significant oxidative dissolution of AgNP to silver ions, there were very minor to no changes in the physicochemical properties of AgNP in water and 10% ethanol.

Plants act as a crucial interface between humans and their environment. The wide use of nanoparticles (NPs) has raised great concerns about their potential impacts on crop health and food safety, leading to an emerging research theme about the interaction between plants and NPs. However, up to this day even the basic issues concerning the eventual fate and characteristics of NPs after internalization are not clearly delineated due to the lack of a well-established technique for the quantitative analysis of NPs in plant tissues. We endeavored to combine a quantitative approach for NP analysis in plant tissues with TEM to localize the NPs. After using an enzymatic digestion to release the NPs from plant matrices, single particle-inductively coupled plasma-mass spectrometry (SP-ICP-MS) is employed to determine the size distribution of silver nanoparticles (Ag NPs) in tissues of the model plant Arabidopsis thaliana after exposure to 10 nm Ag NPs. Our results show that Macerozyme R-10 treatment can release Ag NPs from Arabidopsis plants without changing the size of Ag NPs. The characteristics of Ag NPs obtained by SP-ICP-MS in both roots and shoots are in agreement with our transmission electron micrographs, demonstrating that the combination of an enzymatic digestion procedure with SP-ICP-MS is a powerful technique for quantitative determination of NPs in plant tissues. Our data reveal that Ag NPs tend to accumulate predominantly in the apoplast of root tissues whereby a minor portion is transported to shoot tissues. Furthermore, the fact that the measured size distribution of Ag NPs in plant tissue is centered at around 20.70 nm, which is larger than the initial 12.84 nm NP diameter, strongly implies that many internalized Ag NPs do not exist as intact individual particles anymore but are aggregated and/or biotransformed in the plant instead.

On behalf of the OECD Working Party on Manufactured Nanomaterials (WPMN) an expert meeting on ecotoxicology and environmental fate of nanomaterials (NMs) took place in January 2013 in Berlin. At this meeting experts from science, industry and regulatory bodies discussed the applicability of OECD test guidelines (TGs) for chemicals to nanomaterials. The objective was to discuss the current state of the relevant science and provide recommendations to the OECD WPMN on (1) the need for updating current OECD TGs and the need for developing new ones specific to nanomaterials; and (2) guidance needed for the appropriate and valid testing of environmental fate and ecotoxicity endpoints for NMs. Experts at the workshop agreed that the majority of the OECD TG for chemicals were generally applicable for the testing of NM, with the exception of TG 105 (water solubility) and 106 (adsorption-desorption). Additionally, the workshop also highlighted considerations when conducting OECD chemical TG on nanomaterials (e.g., sample preparation, dispersion, analysis, dosimetry and characterisation). These considerations will lead to the future development of proposals for new TG and guidance documents (GDs) to ensure that OECD TG give meaningful, repeatable, and accurate results when used for nanomaterials. This report provides a short overview of topics discussed during the meeting and the main outcomes. A more detailed report of the workshop will become available through the OECD, however, due to the urgency of having OECD TG relevant for nanomaterials, this brief report is being shared with the scientific community through this communication., (Copyright © 2013. Published by Elsevier B.V.)