Correlating Frictional Forces Generated by Different Bracket Types during Sliding and Surface Topography Using Scanning Electron Microscopy and Optical Profilometer.

AIM: The study aims to correlate the frictional forces (FF) of four different types of commercially available ceramic brackets to their surface topography. MATERIALS AND METHODS: Two monocrystalline (MC) brackets (CLEAR™, Adanta, Germany; Inspire ICE™, Ormco, USA), one polycrystalline (PC) bracket (Symetri Clear™, Ormco, USA), one clear hybrid esthetic bracket (DISCREET™, Adanta, Germany), and a stainless-steel (SS) bracket (Victory™, 3M Unitek, USA) served as control. Both static friction (SF) and kinetic friction (KF) were recorded during sliding using an Instron universal machine in dry settings. The bracket slot surface topography was evaluated. A scanning electron microscope (SEM) and a profilometer machine were used for assessment before and after sliding. RESULTS: Frictional forces values during sliding were as follows in descending order; Inspire ICE™, CLEAR™, DISCREET™, Symetri Clear™, and, lastly, Victory™. Also, DISCREET™ scored the highest in surface roughness (Sa) values followed by Symetri Clear™. None of the correlations were statistically significant. CONCLUSION: Frictional forces produced during sliding were not always directly related to surface roughness. Monocrystalline ceramic brackets appeared to have the greatest FF and a low surface roughness. Furthermore, DISCREET™ scored a very low frictional value comparable to metal brackets yet showed the highest surface roughness. Metal brackets exhibited the greatest surface smoothness before sliding and the least SF. CLINICAL SIGNIFICANCE: Predicting the FFs produced during sliding mechanics would help the practitioner while choosing the bracket system to be used, and while planning the treatment mechanics, how much force to deliver, and how much tooth movement to expect. How to cite this article: AlBadr AH, Talic NF. Correlating Frictional Forces Generated by Different Bracket Types during Sliding and Surface Topography Using Scanning Electron Microscopy and Optical Profilometer. J Contemp Dent Pract 2024;25(1):41-51.

The impact of alloying element Cu on corrosion and biofilms of 316L stainless steel exposed to seawater.

Copper-containing stainless steel (SS) has been reported to mitigate biofilms in industrial and clinical environments. However, the impact of copper released from copper-containing SS in natural seawater on biofilms and corrosion is still unclear. In this study, three kinds of 316L SS were immersed in natural seawater for 6 months, and the pitting depth decreased in the order: 316L-Cu SS (annealed) > 316L SS > 316L-Cu SS (aged). The biofilm thickness and number of sessile cells on the surface of 316L-Cu SS (annealed) and 316L SS were similar but notably greater than those of 316L-Cu SS (aged). Furthermore, the results of the community analysis indicated that the addition of copper in 316L-Cu SS (aged) reduced the diversity and richness of the microbial community, resulting in a significant reduction in the number of genera constituting the biofilms. Copper ions exhibit a broad-spectrum bactericidal effect, effectively reducing the abundance of dominant populations and microbial genera in the biofilms, thereby mitigating pitting corrosion induced by microorganisms. In addition, the PCoA scatter plot showed that time also played an important role in the regulation of microbial community structure.

Biosurfactant-Assisted Cu Doping of Brushite Coatings: Enhancing Structural, Electrochemical, and Biofunctional Properties.

Stainless steel (316L SS) has been widely used in orthopedic, cardiovascular stents, and other biomedical implant applications due to its strength, corrosion resistance, and biocompatibility. To address the weak interaction between steel implants and tissues, it is a widely adopted strategy to enhance implant performance through the application of bioactive coatings. In this study, Cu-doped brushite coatings were deposited successfully through pulse electrodeposition on steel substrates facilitated with a biosurfactant (BS) (i.e., surfactin). Further, the combined effect of various concentrations of Cu ions and BS on the structural, electrochemical, and biological properties was studied. The X-ray diffraction (XRD) confirms brushite composition with Cu substitution causing lattice contraction and a reduced crystallite size. The scanning electron microscopy (SEM) and energy-dispersive spectroscopy (EDS) studies reveal the morphological changes of the coatings with the incorporation of Cu, which is confirmed by X-ray photoelectron spectroscopy (XPS) and elemental mapping. The Fourier transform infrared (FTIR) and Raman spectroscopy confirm the brushite and Cu doping in the coatings, respectively. Increased surface roughness and mechanical properties of Cu-doped coatings were analyzed by using atomic force microscopic (AFM) and nanohardness tests, respectively. Electrochemical assessments demonstrate corrosion resistance enhancement in Cu-doped coatings, which is further improved with the addition of biosurfactants. In vitro biomineralization studies show the Cu-doped coating's potential for osseointegration, with added stability. The cytocompatibility of the coatings was analyzed using live/dead and 3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyl tetrazolium bromide (MTT) assays; cell adhesion, proliferation, and migration studies were evaluated using SEM. Antibacterial assays highlight significant improvement in the antibacterial properties of Cu-doped coatings with BS. Thus, the developed Cu-doped brushite coatings with BS demonstrate their potential in the realm of biomedical implant technologies, paving the way for further exploration.

Seasonal variation in the biological succession of marine diatoms over 316L stainless steel in a coastal environment of Chile.

Characterizing seasonal changes in diatom community profiles in coastal environments is scarce worldwide. Despite diatoms being prevalent in microfouling, their role in microbially influenced corrosion of metallic materials remains poorly understood. This study reports the effect of seasonal variations on the settlement of marine diatoms and corrosion of 316 L stainless steel surfaces exposed to Chilean coastal seawater. Electron microscopy imaging revealed a diverse assembly of diatoms, exhibiting pronounced differences at genus level between summer and winter seasons, with a significant delay in diatom settlement during winter. Electrochemical measurements indicated an active role of diatoms in increasing corrosion current during biofilm development. While the final diatom composition was similar irrespective of the season, the analyses of diatom assemblages over time differed, showing faster colonization when silicate and nitrate were available. This study lays the foundation for future research on the dominant season-specific genera of diatoms to unveil the microbial interactions that could contribute to corrosion and to evaluate their potential as bioindicators for alternative surveillance strategies.

Fabrication of a novel aesthetic orthodontic bracket and evaluation of friction properties between PEEK and stainless steel wires.

BACKGROUND: Polyetheretherketone (PEEK) is a polyaromatic semi-crystalline thermoplastic polymer with mechanical and lubrication properties favorable for biomedical applications. Despite of its aesthetic appearance, ceramic brackets are unsatisfactory in brittleness and thickness, while PEEK is a potential material for aesthetic orthodontic brackets. OBJECTIVE: To fabricate a novel aesthetic orthodontic bracket and evaluate friction properties of PEEK and stainless steel wires. METHODS: All polyether ether ketone (PEEK) and ceramic samples disks were made into disks (diameter, 5 mm; thickness, 2 mm). The tested surfaces of PEEK were ground with #600, #800 and #1200 SiC papers, followed by polishing with Sof-Lex kit (3M ESPE, USA). The surface roughness was tested using a laser profilometer device (VK-X200, Keyence, Japan). The COFs of the specimens and stainless steel (SS) archwires were tested using a Universal Micro-Tribotester (UMT-3, Bruker, USA). The wear scratches on the materials' surfaces were examined by using a scanning electron microscope (SEM) (Hitachi SU8010). The elastic modulus and hardness of samples were examined with a nano-indenter (XP, Keysight Technologies, USA). RESULTS: The mean surface roughness of PEEK and Ceramic are 0.320 ± 0.028 µm and 0.343 ± 0.044 µm, respectively. PEEK has a lower Friction coefficient than Ceramic and the difference between the two groups was statistically significant (P< 0.05). The abrasive wear of Ceramic was the main wear style and was characterized by the observation of chipping fractures, while PEEK surface looked smooth without obvious scale-like desquamations and granular debris, indicating adhesive wear. CONCLUSION: Within the limitations of the present study, PEEK shows lower coefficient of friction than ceramic. PEEK has excellent properties such as low friction coefficient, smooth surface and good mechanical properties, and thus meets the requirements for orthodontic brackets. It is considered as a potential bracket material with both low friction and aesthetic performance.

Combatting cyanobacteria: unraveling the potency of 316L-Cu stainless steel in inhibiting Microcystis aeruginosa growth.

Harmful algal blooms, particularly those of Microcystis aeruginosa, present significant ecological and health risks. To address this issue, this study utilized a custom static algal growth assessment apparatus to investigate the anti-algal performance of a copper-alloyed 316L stainless steel (SS), named 316L-Cu SS. This material was compared with traditional 316L SS, which is widely utilized in freshwater systems for its corrosion resistance. Algal growth dynamics were monitored through optical density (OD) and chlorophyll A concentration measurements. Notably, 316L-Cu SS exhibited superior inhibitory effects on Microcystis aeruginosa growth compared to 316L SS and control groups. Inductively coupled plasma mass spectrometry (ICP-MS) confirmed that the copper ion release from 316L-Cu SS played a critical role in this algal suppression, which interfered with photosynthesis, induced oxidative stress, and damaged algal cell membranes. In contrast, other metal ions (Ni, Cr, Fe) had a negligible impact on algal growth. The study highlights 316L-Cu SS as a promising material for mitigating harmful algal blooms, thereby offering potential benefits for both aquatic ecosystem conservation and public health protection.

Evaluation of Time-Dependent Corrosion Inhibition Rate for f-MWCNT-BCP Composite Coatings on 316L Stainless Steel in Simulated Body Fluid for Orthopedic Implantation.

A well-developed-multiwall carbon nanotube (f-MWCNT)/biphasic calcium phosphate (BCP) composites were synthesized using ultrasonication method for orthopedic implantation applications. The formation of composites and its phase was confirmed by using X-ray diffraction. The presence of various functional groups was identified by using Fourier transform infra-red (FT-IR) spectroscopy. The presence of f-MWCNT was confirmed by Raman spectroscopy. High-resolution transmission electron microscopy (HR-TEM) analysis revealed that BCP units were bound by the surface of f-MWCNTs. The synthesized composites were coated on medical grade 316L stainless steel substrates using electro deposition technique. To determine its corrosion resistance characteristics, the developed substrates were exposed to a simulated bodily fluid (SBF) solution for 0, 4, and 7 days. These results strongly suggest that the coated composites can be utilized for bone tissue repair.

Exploring the optimal electropolymerization strategy for the preparation of solid-phase microextraction fibers using pyrrole-dopamine copolymers.

In-situ electropolymerization of conductive polymers on the surface of stainless-steel substrates is a well-established but promising procedure for the preparation of solid-phase microextraction (SPME) tools. Herein, different electrochemical methods including constant potential (CP), constant potential pulse (CPP), and cyclic voltammetry (CV) were utilized to fabricate SPME fibers by in-situ electropolymerization of pyrrole-dopamine copolymers (PPY/PDA) on the surface of stainless-steel fibers. The coated fibers were characterized and applied for the direct-immersion SPME (DI-SPME) sampling of ultra-trace amounts of plant hormones including abscisic acid (ABA), gibberellic acid (GA3), and indole acetic acid (IAA) in fruit juices, followed by HPLC-UV determination. The results showed that CV electropolymerization is significantly more efficient than the two other methods. The coatings created by the CV method were satisfactorily uniform, adhesive, and durable and exhibited higher extraction performance compared to the CP and CPP procedures. The important experimental variables of the proposed DI-SPME-HPLC method were evaluated and optimized using response surface methodology with a Box-Behnken design. The developed method showed wide-range linearities, spanning from 0.05 to 20µg mL-1 for GA3, and 0.02 to 20µg mL-1 for ABA and IAA. The limits of detection were obtained 0.01µg mL-1 for GA3, and 0.005µg mL-1 for ABA and IAA. The fiber was successfully employed for the simultaneous DI-SPME-HPLC analysis of plant hormones in fruit juice samples.

Rapid Surface Modification of Stainless Steel 304L Electrodes for Microbial Electrochemical Sensor Application.

Electrogenic microorganisms serve as important biocatalysts for microbial electrochemical sensors (MESes). The electrical signal produced is based on the rate of electron transfer between the microbes and electrodes, which represents the biotoxicity of water. However, existing MESes require complex and sophisticated fabrication methods. Here, several low-cost and rapid surface modification strategies (carbon powder-coated, flame-oxidized, and acid-bleached) have been demonstrated and studied for biosensing purposes. Surface-modified MESe bioanodes were successfully applied to detect multiple model pollutants including sodium acetate, ethanol, thinner, and palm oil mill effluent under three different testing sequences, namely, pollutant incremental, pollutant dumping, and water dilution tests. The carbon powder-coated bioanode showed the most responsive signal profile for all the three tests, which is in line with the average roughness values (Ra) when tested with atomic force microscopy. The carbon powder-coated electrode possessed a Ra value of 0.844, while flame-oxidized, acid-bleached, and control samples recorded 0.323, 0.336, and 0.264, respectively. The higher roughness was caused by the carbon coating and provided adhesive sites for microbial attachment and growth. The accuracy of MESe was also verified by correlating with chemical oxygen demand (COD) results. Similar to the sensitivity test, the carbon powder-coated bioanode obtained the highest R2 value of 0.9754 when correlated with COD results, indicating a high potential of replacing conventional water quality analysis methods. The reported work is of great significance to showcase facile surface modification techniques for MESes, which are cost-effective and sustainable while retaining the biocompatibility toward the microbial community with carbon-based coatings.

Corrosion, surface, and tribological behavior of electrophoretically deposited polyether ether ketone coatings on 316L stainless steel for orthopedic applications.

Electrophoretic deposition (EPD) of polyether ether ketone (PEEK) coatings on metallic implants has recently attracted a great deal of interest; however, further investigation into their corrosion, surface, and tribological properties is required for their clinical application. Using Potentiodynamic polarization and Mott-Schottky analysis of PEEK coatings, we analyzed the electrochemical corrosion behavior of electrophoretically deposited PEEK coatings on 316L stainless steel (SS) substrates. In addition, the tribological behavior of the coatings was determined through pin-on-disc and scratch testing. Initially, the EPD parameters were optimized using a Taguchi Design of Experiment (DoE) approach. The coatings exhibited irregular shaped grains along with ∼66 µm of thickness. Fourier transform infrared spectroscopy confirmed the presence of functional groups ascribed with PEEK. The coatings were moderately hydrophobic and had an average roughness of ∼2 µm. The corrosion studies demonstrated promising features of current density and corrosion potential, indicating that corrosion resistance significantly improves with PEEK coating. Electrochemical impedance spectroscopy also confirmed the corrosion resistance of PEEK coating. The coatings exhibited a slightly lower wear resistance than SS samples, but still possessed adequate wear and scratch resistance for biomedical applications. The current study confirmed that the PEEK coatings on metallic implants is effective for orthopedic applications where corrosion and tribology are major concerns.

Surface nanocrystallization enhances the biomedical performance of additively manufactured stainless steel.

Additive manufacturing enables the fabrication of patient-specific implants of complex geometries. Although selective laser melting (SLM) of 316L stainless steel (SS) is well established, post-processing is essential to preparing high-performance biomedical implants. The goal of this study was to investigate surface mechanical attrition treatment (SMAT) as a means to enhance the electrochemical, biomechanical, and biological performances of 316L SS fabricated by SLM in devices for the repair of bone tissues. The SMAT conditions were optimized to induce surface nanocrystallization on the additively manufactured samples. SMAT resulted in a thicker oxide layer, which provided corrosion resistance by forming a passive layer. The fretting wear results showed that the rate of wear decreased after SMAT owing to the formation of a harder nanostructured layer. Surface modification of the alloy by SMAT enhanced its ability to support the attachment and proliferation of pre-osteoblasts in vitro. The study of the response in vivo to the additively manufactured alloy in a critical-sized cranial defect murine model revealed enhanced interactions with the cellular components after the alloy was subjected to SMAT without inducing any adverse immune response. Taken together, the results of this work establish SMAT of additively manufactured metallic implants as an effective strategy for engineering next-generation, high-performance medical devices for orthopedics and craniomaxillofacial applications.

Regulation of localized corrosion of 316L stainless steel on osteogenic differentiation of bone morrow derived mesenchymal stem cells.

Localized corrosion has become a concerning issue in orthopedic implants as it is associated with peri-implant adverse tissue reactions and implant failure. Here, the pitting corrosion of 316 L stainless steels (316 L SSs) was initiated by electrochemical polarization to simulate the in vivo localized corrosion of orthopedic implants. The effect of localized corrosion on osteogenic differentiation of bone marrow derived mesenchymal stem cells (BMSCs) was systematically studied. The results suggest that pitting corrosion of 316 L SS reduced the viability, adhesion, proliferation, and osteogenic differentiation abilities of BMSCs, especially for the cells around the corrosion pits. The relatively high concentrations of metallic ions such as Cr3+ and Ni2+ released by pitting corrosion could cause cytotoxicity to the BMSCs. The inhomogeneous electrochemical environment resulted from localized corrosion could promote reactive oxygen species (ROS) generation around the corrosion pits and cause oxidative stress of BMSCs. In addition, localized corrosion could also electrochemically interact with the cells and lead to cell membrane depolarization. The depolarized cell membranes and relatively high levels of ROS mediated the degradation of the osteogenic capacity of BMSCs. This work provides new insights into corrosion-mediated cell function degeneration as well as the material-cell interactions.

New reaction path for long-chain hydrocarbons by electrochemical CO2 and CO reduction over Au/stainless steel.

The Fischer-Tropsch (F-T) synthesis is recognized for its ability to produce long-chain hydrocarbons. In this study, we aimed to replicate F-T synthesis using electrochemical CO2 reduction and CO reduction reactions on a stainless steel (SS) support with a gold (Au) overlayer. Under CO2-saturated conditions, the presence of Au on the SS surface led to the formation of CH4 and a range of hydrocarbons (CnH2n and CnH2n+2, n = 2-7), while bare SS primarily produced hydrogen. The Au(10 nm)/SS exhibited the highest hydrocarbon production in CO2-saturated phosphate, indicating a synergistic effect at the Au-SS interface. In CO-saturated conditions, bare SS also produced long-chain hydrocarbons, but increasing Au thickness resulted in decreased production due to poor CO adsorption. Hydrocarbons were formed through both direct and indirect CO adsorption pathways. Anderson-Schulz-Flory analysis confirmed surface CO hydrogenation and C-C coupling polymerization following conventional F-T synthesis. The C2 hydrocarbons exhibited distinct behavior compared to C3-5 hydrocarbons, suggesting different reaction pathways. Despite low reduction product levels, our EC method successfully replicated F-T synthesis using the Au/SS electrode, providing valuable insights into C-C coupling mechanisms and electrochemical production of long-chain hydrocarbons. Depth-profiling X-ray photoelectron spectroscopy revealed significant changes in surface elemental compositions before and after EC reduction.

Synergistic inhibition effect of ultraviolet irradiation and benzalkonium chloride on the corrosion of 316L stainless steel caused by Aspergillus terreus.

Microbiologically influenced corrosion (MIC) is a key factor that damages engineering materials in marine environments. One of the major concerns in this regard is the corrosion protection of stainless steel (SS) caused against fungal attacks. This study investigated the effect of ultraviolet (UV) irradiation and benzalkonium chloride (BKC) on the corrosion of 316L stainless steel (316L SS) induced by marine Aspergillus terreus in 3.5 wt% NaCl solution. This was accomplished by employing microstructural characterisations and electrochemical analysis to analyse the synergistic inhibition behaviour of the two methods. The results indicated that while UV and BKC demonstrated individual abilities to suppress the biological activity of A. terreus, their inhibitory effects were not significant. The combination of UV light and BKC was found to cause a further decline in the biological activity of A. terreus. The analysis revealed that the combination of BKC and UV significantly decreased the sessile cell counts of A. terreus by more than three orders of magnitude. The fungal corrosion inhibition effect of individual application of UV light or BKC did not yield satisfactory results owing to the low intensity of UV and low concentration of BKC. Furthermore, the corrosion inhibition of UV and BKC occurred mainly during the early stages. The corrosion rate of the 316L SS declined rapidly when the combination of UV light and BKC were used, indicating that UV light and BKC exert a good synergistic inhibitory effect on the corrosion of the 316L SS caused by A. terreus. Therefore, the results suggest that the combination of UV light and BKC can be an effective approach to control the MIC of 316L SS in marine environments.

Temporal dynamics of adhesion of oral bacteria to orthodontic appliances.

Adhesion of the most common dental biofilm bacteria to alloys used in orthodontics in relation to surface characteristics was analyzed. Streptococcus mutans (S. mutans), Streptococcus oralis (S. oralis), Veillonella parvula (V. parvula), and Aggregatibacter actinomycetemcomitans (A. actynomicetemcomitans) were incubated for 4 h with nickel-titanium (NiTi) and stainless-steel (SS) wires. The surface roughness and free energy of the alloys, as well as the hydrophobicity of the alloys and bacteria, were assessed. NiTi had higher surface free energy and rougher (p<0.001) and more hydrophilic surfaces than SS (p<0.001). The hydrophobic properties of the bacteria decreased in the following order: V. parvula>S. oralis>S. mutans>A. actynomicetemcomitans. Bacterial adhesion generally increased over time, though this pattern was influenced by the type of alloy and the bacteria present (p<0.001). In a multiple linear regression, the principal predictor of adhesion was bacterial hydrophobicity (p<0.001), followed by time (p<0.001); alloy surface characteristics had a low influence.

Advanced micro- & nanostructuring for enhanced biocompatibility of stainless steel by multi-beam and beamshaping technology.

Biocompatibility is one of the key issues for implants, especially in the case of stainless steel with medium to low biocompatibility, which may lead to a lack of osseointegration and consequently to implant failure or rejection. To precisely control preferential cell growth sites and, consequently, the biocompatibility of prosthetic devices, two types of surfaces were analyzed, containing periodic nanogrooves laser induced periodic surface structure (LIPSS) and square-shaped micropillars. For the fast and efficient production of these surfaces, the unique combination of high energy ultrashort pulsed laser system with multi-beam and beamshaping technology was applied, resulting in increased productivity by 526% for micropillars and 14 570% for LIPSS compared to single beam methods.In vitroanalysis revealed that micro and nanostructured surfaces provide a better environment for cell attachment and proliferation compared to untreated ones, showing an increase of up to 496% in the number of cells compared to the reference. Moreover, the combination of LIPSS and micropillars resulted in a precise cell orientation along the periodic microgroove pattern. The combination of these results demonstrates the possibility of mass production of functionalized implants with control over cell organization and growth. Thus, reducing the risk of implant failure due to low biocompatibility.

Titanium Dioxide/Graphene Oxide Composite Coatings for 316 Stainless Steel Dental Implants.

Stainless steel has been used in orthopedics and orthodontic fields. However, it cannot be used for fabrication of dental implants due to its inertness, low biocompatibility and weak resistance to corrosion. A composite coating of titanium oxide /graphene oxide has been prepared for stainless steel to improve its biological properties. Stainless steel discs were polished, cleaned and pre-treated with a mixture of HNO3 and HF acid for 15 min. The composite coating composed of TiO2 produced by sol-gel technique and doped with 0.75 wt% graphene oxide. XRD, SEM-EDX and AFM were employed to characterize the composite coating. The anti-bacterial action of the composite coating was investigated against S. aureus and E. coli. The corrosion resistance of coated and noncoated samples was assessed in SBF using electrochemical technique. Cytotoxicity was assessed using osteoblast-like cells. The wettability was determined by contact angle, and bioactivity assessed by immersion in SBF. The results revealed that the composite coating was dense with few micro-cracks, and was not cytotoxic to osteoblast-like cells. The composite coating reduced bacterial colonies and the corrosion rate of the steel was improved. The wettability of the sample was increased with the composite coating and apatite formation appeared after 21 days.

Carbon nanotubes-assisted solid-phase microextraction for the extraction of gasoline in fire debris samples.

Gasoline is one of the most encountered ignitable liquids (IL) in fire debris analysis. The extraction of gasoline from fire debris samples presents challenges due to the complicated nature of multicomponent mixtures. This research work proposed a novel carbon nanotube-assisted solid phase microextraction (CNT-SPME) fiber coupled with gas chromatography and mass spectrometry (GC/MS) to determine gasoline residues for fire debris analysis. The CNT-SPME fiber was prepared by a sequential coating of polydopamine, epoxy, and CNTs on a stainless-steel wire. The extraction capabilities of the CNT-SPME fiber for gasoline and its major aromatic groups (xylenes, alkylbenzenes, indanes, and naphthalenes) from neat and spiked samples were promising, with linear dynamic ranges of 0.4-12.5 and 3.1-12.5 µg 20-mL-1 headspace vial, respectively. The average relative standard deviations and accuracies for all concentration ranges in this work were lower than 15%. The relative recovery of the CNT-SPME fiber for all aromatic groups ranged from 28 ± 3% to 59 ± 2%. Additionally, the CNT-SPME fiber showed a higher selectivity for the naphthalenes group in gasoline, as indicated by the experimental outcome using a pulsed thermal desorption process of the extracts. We envision the nanomaterial-based SPME offers promising opportunities for extracting and detecting other ILs to support fire investigation.

In-situ growth of covalent organic framework on stainless steel needles as solid-phase microextraction probe coupled with electrospray ionization mass spectrometry for rapid and sensitive determination of tricyclic antidepressants in biosamples.

Tricyclic antidepressants (TCAs) including amitriptyline (AT), doxepin (DOX) and nortriptyline (NT) are the first-line drugs for the clinical treatment of depression; however, monitoring TCA concentrations in biological fluids and tissues is necessary to improve therapeutic effect and determine the cause of death in patients. It is of great significance to develop a rapid and sensitive method for real-time monitoring of TCAs in various biosamples. In this work, we fabricated a novel covalent organic framework (COF) based solid-phase microextraction (SPME) probe by an in-situ step-by-step strategy, which was obtained by sequentially modifying 1,3,5-tri (4-aminophenyl) benzene (TPB) and 2, 5-divinylbenzaldehyde (DVA) on the surface of polydopamine layer. The TPB-DVA-COF-SPME probe possessed high specific surface area (1244 m2·g - 1), regular pores (3.23 nm), good hydrophobicity and stability, resulting in efficient enrichment for TCAs. Furthermore, the combination of TPB-DVA-COF-SPME probe and ambient electrospray ionization mass spectrometry system (ESI/MS) was firstly proposed for rapid and sensitive determination of TCAs in biosamples. As a result, the developed method exhibited low limits of detection (LODs) (0.1-0.5 µg∙L - 1), high enrichment factors (39-218), and low relative standard deviations (RSDs) for one probe (1.2-3.8%) and probe-to-probe (2.0-3.7%). Benefiting from these outstanding performance, TPB-DVA-COF-SPME probe was further successfully applied to biosamples (i.e., serum, liver, kidney, and brain) with excellent reusability, indicating the promising applicability of the TPB-DVA-COF-SPME-ESI/MS as a powerful tool for drug monitoring.

Modified stainless steel wires with superwettability for highly efficient in-tube solid-phase microextraction.

Construction of different surface wettability is meaningful for the interaction between the sorbent surface and target components. In the current study, four kinds of stainless-steel wires (SSWs) with different hydrophobic/hydrophilic property were prepared and used as the absorbents to enrich the target compounds with different polarity. Comparative extraction of six non-polar polycyclic aromatic hydrocarbons (PAHs) and six polar estrogens was carried out by in-tube solid phase microextraction (IT-SPME). The results showed that two SSWs with the superhydrophobic surfaces exhibited high extraction capacity to the non-polar PAHs with the superior enrichment factor (EF) in the range of 29-672 and 57-744, respectively. In contrast, the superhydrophilic SSWs demonstrated higher enrichment efficiency for the polar estrogens than other hydrophobic SSWs. On the basis of optimized conditions, a validated analysis method was established using six PAHs as model analytes for IT-SPME-HPLC. Acceptable linear ranges (0.5-10 µg L-1) and low detection limits (0.0056-0.32 µg L-1) were achieved using the superhydrophobic wire modified by perfluorooctyl trichlorosilane (FOTS). The relative recoveries spiked at 2, 5 and 10 µg L-1 in the lake water samples were in the range of 81.5%-113.7%. The relative standard deviation (RSD) of intraday (≤0.8%, n = 3) and interday (≤5.3%, n = 3) tests demonstrated the good extraction repeatability for the same extraction tube. Satisfactory repeatability for the preparation of extraction tubes (n = 3) was also obtained with the RSD values in the range of 3.6%-8.0%.