Infrared Chemical Imaging Research Articles

Detection of microplastics in the human penis.

The proliferation of microplastics (MPs) represents a burgeoning environmental and health crisis. Measuring less than 5 mm in diameter, MPs have infiltrated atmospheric, freshwater, and terrestrial ecosystems, penetrating commonplace consumables like seafood, sea salt, and bottled beverages. Their size and surface area render them susceptible to chemical interactions with physiological fluids and tissues, raising bioaccumulation and toxicity concerns. Human exposure to MPs occurs through ingestion, inhalation, and dermal contact. To date, there is no direct evidence identifying MPs in penile tissue. The objective of this study was to assess for potential aggregation of MPs in penile tissue. Tissue samples were extracted from six individuals who underwent surgery for a multi-component inflatable penile prosthesis (IPP). Samples were obtained from the corpora using Adson forceps before corporotomy dilation and device implantation and placed into cleaned glassware. A control sample was collected and stored in a McKesson specimen plastic container. The tissue fractions were analyzed using the Agilent 8700 Laser Direct Infrared (LDIR) Chemical Imaging System (Agilent Technologies. Moreover, the morphology of the particles was investigated by a Zeiss Merlin Scanning Electron Microscope (SEM), complementing the detection range of LDIR to below 20 µm. MPs via LDIR were identified in 80% of the samples, ranging in size from 20-500 µm. Smaller particles down to 2 µm were detected via SEM. Seven types of MPs were found in the penile tissue, with polyethylene terephthalate (47.8%) and polypropylene (34.7%) being the most prevalent. The detection of MPs in penile tissue raises inquiries on the ramifications of environmental pollutants on sexual health. Our research adds a key dimension to the discussion on man-made pollutants, focusing on MPs in the male reproductive system.

Identification and quantification of microplastics in salts by complementary approaches using pyrolysis-gas chromatography/quadrupole-time of flight mass spectrometry (Py-GC/QTOFMS) and laser direct infrared (LDIR) chemical imaging analysis

Microplastics (MPs) and nanoplastics (NPs) have been suspected as contaminants in various foodstuffs, including salts, all over the world. Regarding the different sizes and polymer types, the mass concentrations of actual plastic particles in salt are not very clear. The purpose of this study is to develop a scalable method for qualitative and quantitative analysis of MPs and NPs by using Pyrolysis Gas Chromatography Quadrupole-Time of Flight mass spectrometry (Py-GC/QTOFMS) to detect their mass concentrations in salt samples. The targeted and suspected lists of polymers in salts were compiled based on the combined results of the high-resolution mass spectrometry (HRMS) full scanning with auxiliary MS dataset and the laser direct infrared (LDIR) chemical imaging analysis. The seven targeted MPs with polymer standards, i.e., polyvinyl chloride (PVC), polymethyl methacrylate (PMMA), polypropylene (PP), polystyrene (PS), polyethylene (PE), polyethylene terephthalate (PET), and polycarbonate (PC), were first subjected to a full MS scanning mode of the Py-GC/QTOFMS analysis. Subsequently, the parental masses of their pyrolysis compounds were used as the seeds to generate the related daughter masses. This process established both retention time and mass-pairs matching for the target MS/MS mode for enabling the identification and quantification of the particles. The suspected MPs with a matching degree >0.65 in the LDIR list were explored either by the full scan MS. Only PVC was identified, and PET was suspected. The Py-GC/QTOFMS result is complementary and comparable to the LDIR detection with the matching degree >0.85. We identified that PVC and PET (suspected) can be measured in both commercial and bulk sea salts, and their concentrations in sea salts are much higher than in rock salts, implying heavy contamination of the seawater.

Erosion of rigid plastics in turbid (sandy) water: quantitative assessment for marine environments and formation of microplastics.

Mechanical degradation (erosion) of plastics in the marine environment has been reported in many literature studies but without quantitative information. This type of degradation is crucial as it accounts for most of the initial microplastic products, in marine environments (e.g., rivers and oceans). Here, we quantify the erosion of plastics by water-borne sediments under typical perpendicular water velocities and sand loads of turbid rivers and coastal oceans. Polypropylene (PP) shows the highest response to water-borne erosion, with a surface degradation rate of 5160 μm per year (4.44 mg per mm2 per year), compared with high-density polyethylene (HDPE) with a degradation rate of 1874 μm per year (1.79 mg per mm2 per year), resulting in the formation of microplastics (MPs). The rate of formation of such microplastic particles (>10 μm), as characterised by a laser direct infrared (LDIR) chemical imaging system, amounts to 669 particles per mm2 per year for PP and 187 particles per mm2 per year for HDPE, exhibiting average particle sizes of 60 μm and 23 μm in the same order. Furthermore, surface microscopy provided valuable insights into the dominant erosion mechanisms, revealing three distinct zones and the surface features reveal the brittle erosion behaviours. These results will enable a better assessment of degradation and lifetime prediction of plastics in turbid rivers and coastal oceans, allowing precise estimation of the rate of formation of MPs.

Detection of Various Microplastics in Patients Undergoing Cardiac Surgery.

Microplastics have been detected in human stool, lungs, and placentas, which have direct exposure to the external environment through various body cavities, including the oral/anal cavity and uterine/vaginal cavity. Crucial data on microplastic exposure in completely enclosed human organs are still lacking. Herein, we used a laser direct infrared chemical imaging system and scanning electron microscopy to investigate whether microplastics exist in the human heart and its surrounding tissues. Microplastic specimens were collected from 15 cardiac surgery patients, including 6 pericardia, 6 epicardial adipose tissues, 11 pericardial adipose tissues, 3 myocardia, 5 left atrial appendages, and 7 pairs of pre- and postoperative venous blood samples. Microplastics were not universally present in all tissue samples, but nine types were found across five types of tissue with the largest measuring 469 μm in diameter. Nine types of microplastics were also detected in pre- and postoperative blood samples with a maximum diameter of 184 μm, and the type and diameter distribution of microplastics in the blood showed alterations following the surgical procedure. Moreover, the presence of poly(methyl methacrylate) in the left atrial appendage, epicardial adipose tissue, and pericardial adipose tissue cannot be attributed to accidental exposure during surgery, providing direct evidence of microplastics in patients undergoing cardiac surgery. Further research is needed to examine the impact of surgery on microplastic introduction and the potential effects of microplastics in internal organs on human health.

Spatial–Temporal Distribution and Ecological Risk Assessment of Microplastics in the Shiwuli River

This study aimed to investigate the distribution of microplastics (MPs) within the Shiwuli River in Hefei, a Chinese inland city. Water and sediment samples were collected during flood season (from May to September) and non-flood season (from October to April) at 10 representative points along the truck stream. The electron microscope, the laser direct infrared chemical imaging system (LDIR), and the scanning electron microscope (SEM) were used to observe and quantify the colour and shape of the MPs, to identify the number, size, and polymer composition of the MPs, and to observe the microstructures of typical MP particles, respectively. The polymer risk index (RI) model and the pollution load index (PLI) model were used to assess the polymer-related risks and the overall extent of MP pollution in the river, respectively. Analysis of MP abundance for different sampling points showed that the water of Shiwuli River had an average abundance of MPs of 8.4 ± 2.5 particles/L during the flood season and 5.8 ± 1.7 particles/L during the non-flood season; the sediment had an average abundance of MPs of 78.9 ± 8.3 particles/kg during the flood season and 63.9 ± 7.1 particles/kg during the non-flood season. The abundance of MPs of different points was investigated. Result show that the more abundances of MPs were found at confluences with tributaries (S4, S5, and S6), where they are also close to the residential and industrial development, while lower values were found in agricultural areas (S8) and wetland ecological regions (S9 and S10). In water, the maximum appeared at S5 with 21.7 ± 4.6 particles/L during the flood season and 15.9 ± 4.2 particles/L during the non-flood season, respectively; the minimum appeared at S9 with 1.8 ± 1.0 particles/L during the flood season and 2.2 ± 0.4 particles/L during the non-flood season, respectively. In sediment, the maximum appeared at S5 with 174.1 ± 10.1 particles/kg during the flood season and 143.6 ± 10.4 particles/kg during the non-flood season, respectively; the minimum appeared at S8 with 10.3 ± 2.8 particles/kg during the flood season and at S9 with 12.1 ± 3.2 particles/kg during the non-flood season, respectively. MP characteristics were also studied. Results show that the MPs mainly exhibited a fibroid morphology (27.90–34%), and red-coloured particles (19.10%) within the smaller size less than 500 μm (38.60%) were more prevalent. Additionally, the result of LDIR scanning shows that a total of eleven types of MP polymers were found in the river water and sediment, including acrylates (ACR), chlorinated polyethylene (CPE), ethylene vinyl acetate (EVA), polyethylene (PE), polyethylene terephthalate (PET), polypropylene (PP), polystyrene (PS), polyurethane (PU), polyvinylchloride (PVC), polyamide (PA), and silicon. The most common particle was PE (19.3–21.6%). Furthermore, the environmental risk assessment demonstrated that the PS polymer posed a Level-III risk in the water samples and a Level-II risk in the sediment samples from the Shiwuli River. The remaining polymer types exhibited Level-I risk. The PLIzone value for water was 2.24 during the flood season, indicating heavy pollution, and 1.66 during the non-flood season, indicating moderate pollution. Similarly, the PLIzone value for sediments was 2.34 during the flood season and 1.91 during the non-flood season, both suggesting a heavy pollution. These findings highlight the potential risk posed by MP pollution in the Shiwuli River to the quality of drinking water sources in Chaohu Lake in Hefei. They provide valuable insights into management, pollution control, and integrated management strategies pertaining to MPs in urban inland rivers in Hefei.

Exposure to microplastics in the upper respiratory tract of indoor and outdoor workers

The aim of this study was to determine the presence of microplastics (MPs) in the upper respiratory tract of indoor and outdoor workers, to assess the type and the extent of contamination. Sputum and nasal lavage fluid were collected, and plastic particles were quantitatively analyzed by polarizing microscopy and a laser direct infrared chemical imaging system. The polarized light microscopy results showed that suspicious MPs were found in the nasal lavage and sputum of both couriers and office staff, and the abundance of MPs in the nasal lavage of office staff was significantly higher than in couriers (P < 0.0001). The chemical imaging results showed that polycarbonate (24.2%) and polyvinylchloride (PVC) (23.0%) were the predominant plastic materials in the sputum of couriers, while polyamide (PA) (25.3%) and polyethylene (22.9%) were dominant in the nasal lavage fluid. The sputum and nasal lavage fluid of office staff were both dominated by PVC (39.1% and 41.1%, respectively) and PA (24.8% and 31.6%, respectively). Therefore, this study revealed that microplastic pollution was found in the respiratory tract of both indoor and outdoor workers, but the distribution of MP particles differed between the two populations.

A case study on small-size microplastics in water and snails in an urban river

Microplastic pollution has become pervasive in aquatic ecosystems. They readily interact with aquatic biota, potentially subjecting them to ecological and health risks. Urban rivers are also affected by microplastics due to intense anthropogenic activity. Nevertheless, relatively little is known about the physiocochemistry or ecotoxicology of microplastics in urban rivers. The present study used laser direct infrared chemical imaging to investigate microplastic pollution in a highly urbanized river in Beijing, China. Surface water was sampled at five sites along the river in March and July, and the benthic snail Bellamya aeruginosa was also collected at each location in July. Thirteen and fifteen different polymers were detected and identified in the surface water sampled in March and July, respectively. Thirteen different polymers were found and isolated in the snails. Of these, polypropylene, polyamide and polyethylene predominated in the microplastic particles. Moreover, the average abundance of the microplastic was significantly higher in the surface water sampled in July (39.55 ± 4.78 particles L−1) than in March (22.00 ± 4.87 particles L−1) (p < 0.05). The average microplastic abundance of snails across all sites was 28.13 ± 4.18 particles, among which the Q2 site has significantly higher microplastic abundance than station Q3-Q5 (p < 0.05). Microplastic particles 10–100 μm in size predominated in both the surface water and the snails. By contrast, the proportions of microplastic particles 200–500 μm in size were substantially smaller. The measured microplastic pollution load and microplastic pollution risk indices in the surface water indicated that the current microplastic pollution level in the Qing River was moderate from upstream to downstream. Moreover, the potential adverse effects of microplastic particles on snails remain unclear. Further research is required to elucidate small-size microplastics' environmental fate and potential ecological risks in urban rivers.

In-Situ Implant Formulation of Laurate and Myristate Prodrugs of Dolutegravir for Ultra-Long Delivery

The focus of present work was to synthesize prodrugs of dolutegravir (DTG) for ultra-long delivery purpose. The prodrug was synthesized by esterification of hydroxyl group with carboxyl group of fatty acid (lauric or myristic acid). The prodrugs were characterized by differential scanning calorimetry, X-ray powder diffraction, nuclear magnetic resonance, Fourier transformed infrared, near infrared-chemical imaging, pH-solubility, partition coefficient, and stability (solid and liquid). Stability studies were performed by exposing the powder drugs to 40°C/75% RH for three months and buffer solutions at room temperature for 72 h. The prodrugs and drug were formulated into in-situ implant using biodegradable polymer. Thermal, spectral, and diffractometric data indicated formation of new chemical and solid forms. Formation of prodrugs resulted in lowering of melting point of DTG from 191.1°C to 163.7 and 140.7°C for DTG-Laurate and DTG-Myristate prodrugs, respectively. A decrease in solubility of 18.2-115.9 and 124.5-1594.9 folds was observed for DTG-Laurate and DTG-Myristate, respectively compared to DTG. Similarly, the prodrugs were highly lipophilic compared to DTG. Solid-state and pH-stability profiles of DTG and prodrugs were comparable. Implant formulation released 60.1% in 77 days compared to 95.6% in 35 days in the case of DTG-Myristate and DTG, respectively. In summary, combining prodrug and drug delivery approaches can be utilized for delivering drug for ultra-long period.

Targeted Analysis of Microplastics Using Discrete Frequency Infrared Imaging.

An analytical strategy to improve sample throughput with discrete frequency infrared image-based targeted analysis of microplastics using a laser direct infrared chemical imaging system was successfully developed and implemented. Leveraging a quantum cascade laser as a light source, the system could lock the frequency at predetermined wavelengths and use a discrete frequency infrared imaging technique to identify particles with absorption at desired wavelengths. In this way, targeted analysis can be achieved by selectively characterizing these particles. In the concept demonstration study, the targeted analysis was able to identify 87.7% of spiked polyethylene particles by scanning only 20% of the particles in the sample. The technique substantially improves sample throughput by at least a factor of 4 under conditions used. In the tests performed with real environmental samples, the targeted analysis workflow correctly identified eight types of common microplastics by only investigating around 60% of the particles and less than 30% of the sample area. Results obtained demonstrated that this scanning strategy is a game changer to enhance sample throughput in microplastic analysis. The technique has the potential of being applied to other infrared-based analytical platforms.

A novel composite anode via immobilizing of Ce-doped PbO2 on CoTiO3 for efficiently electrocatalytic degradation of dye

The exploitation of efficient electrocatalyst is significantly important for degradation of refractory organic pollutants. Herein, a novel Ti/CoTiO3/Ce-PbO2 composite electrocatalyst (abbreviated as CTO/CP) is successfully constructed via facile consecutive immersion pyrolysis and electro-deposition method and then systematically characterized by scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS), X-ray diffraction (XRD), Fourier Transform infrared spectroscopy (FT-IR), energy dispersive spectroscopy (EDS) and near infrared chemical imaging (NIR-CI). Importantly, the electrochemical measurements demonstrate that the CTO/CP possesses numerous prominent properties such as lower charge transfer resistance, larger electroactive area, higher oxygen evolution potential than those of the pristine Ti/CoTiO3 (CTO) and Ti/Ce-PbO2 (CP). Thereby, the CTO/CP exhibits an enhanced electrocatalytic degradation performance with the degradation efficiency as high as 90.0% and COD removal rate of 88.3% at 180 min for the optimal CTO/CP (denoted as 10 layers of CTO and 1 h electrodeposition of CP), in which the ·OH is the major reactive species. Additionally, the optimal CTO/CP also shows a higher ICE/ACE together with lower EEC and desirable stability, universal applicability for many different dyes and reusability. Overall, this work offers a promising approach for enhancing the electrocatalytic properties of CTO via introducing CP.

Design Considerations for Discrete Frequency Infrared Microscopy Systems.

Discrete frequency infrared chemical imaging is transforming the practice of microspectroscopy by enabling a diversity of instrumentation and new measurement capabilities. While a variety of hardware implementations have been realized, design considerations that are unique to infrared (IR) microscopes have not yet been compiled in literature. Here, we describe the evolution of IR microscopes, provide rationales for design choices, and catalog some major considerations for each of the optical components in an imaging system. We analyze design choices that use these components to optimize performance, under their particular constraints, while providing illustrative examples. We then summarize a framework to assess the factors that determine an instrument's performance mathematically. Finally, we provide a validation approach by enumerating performance metrics that can be used to evaluate the capabilities of imaging systems or suitability for specific intended applications. Together, the presented concepts and examples should aid in understanding available instrument configurations, while guiding innovations in design of the next generation of IR chemical imaging spectrometers.

Preparation and characterization of dicarboxylic acids salt of aripiprazole with enhanced physicochemical properties

The focus of present work was to prepare salt of aripiprazole (APZ) with dicarboxylic acids to improve physicochemical properties the drug. Dicarboxylic acids used in the study were malonic acid, maleic acid and succinic acid. The salts were prepared with solubilization-crystallization method. The salts were characterized for pH-solubility, dissolution, and stabilities. The Fourier infrared spectroscopy, X-ray powder diffraction, differential scanning calorimetry and near infrared chemical imaging indicated formation of new solid phase. pH-solubility profiles of the salts were similar to the drug except higher solubility were observed in the salts at all tested pH. The highest solubility was observed for APZ-Malonate salt among all the prepared salts. The solubility curve was inverted ‘V’ shape for APZ-maleate and APZ-succinate while it was inverted ‘U’ shape for APZ-malonate. The water solubility of APZ, APZ-malonate, APZ-maleate and APZ-succinate were 0.07 ± 0.02, 3503.9 ± 37.4, 269.3 ± 6.9 and 729.4 ± 9.4 µg/mL, respectively. The dissolution was 2.9 ± 0.4, 18.4 ± 3.9, 19.5 ± 1.4 and 36.6 ± 4.0% in 45 min for APZ, APZ-maleate, APZ-malonate, and APZ-succinate. The stabilities of the salts were similar to the drug. Thus, salts improved the physicochemical properties of the drug, and have similar stability profiles as that of APZ.

Antibacterial porous xanthan‐based films containing flavoring agents evaluated by near infrared chemical imaging technique

AbstractXanthan gum (XG) is a widely applied natural polysaccharide in food industry as thickening agent. Nowadays, one of the major problems is that some food products are found to be contaminated by pathogenic bacteria such as Escherichia coli and Staphylococcus aureus reducing so, their shelf life. This research aims to demonstrate the antibacterial activity of some biodegradable formulation XG‐lignin hydrogel films and their potential application as carriers for controlled release of flavoring compounds. The XG‐lignin films containing an aspen wood lignin type showed a high antibacterial activity against Salmonella Typhymurium ATCC 14028, E. coli ATCC 25922 and Listeria monocytogenes ATCC 25922 bacteria compared with those containing softwood lignin, or lignin from annual plants. Surface morphology indicated a homogeneous distribution of both components within the hydrogel network and the generation of a porous structure after swelling and lyophilization. Additionally, near infrared chemical imaging technique was used as nondestructive method to observe the spatial distribution of the polymeric components and vanillin into the hydrogel films as well as its release profile. The vanillin release rate dependence on the lignin type was also evidenced, a retarded release of vanillin being observed. These results give an important insight into the use of XG, lignin, and vanillin for the development of new edible films for active packaging materials.

Process quality control of the manufacturing of Chinese Materia Medica by process analysis technology

Process quality control is essential for the manufacturing of Chinese Materia Medica. Non-destructive monitoring is still a challenge for the quality control of Chinese Materia Medica manufacturing. As the commonly used non-destructive process analysis technology, near infrared spectroscopy, near infrared chemical imaging, and laser-induced breakdown spectroscopy have been applied to the quality control of Chinese Materia Medica manufacturing. The characteristic near infrared bands of 29 natural chemical components have been assigned. Ten spectral pre-processing methods and five variable selection methods have been optimized, respectively. Given the interrelationship among modeling parameters, a system modeling concept was put forward to establish a global model. Accuracy Profile was further proposed as the validation method of models. In addition, the homogeneity of chlorpheniramine maleate tablets from six brands was successfully visualized by near infrared-chemical imaging. As and Hg variation in An-Gong-Niu-Huang Wan have been rapidly monitored by laser-induced breakdown spectroscopy. A systematic modeling method (model establishment, evaluation, and validation) and the non-destructive technology of homogeneity visualization and toxic element detection have been developed for quality control of Chinese Materia Medica manufacturing, which is shown in Figure 1 of the article. These achievements have greatly promoted the research and application of process analysis technology in Chinese Materia Medica manufacturing, laying a solid foundation for the development of intelligent Chinese pharmaceutical industry.

An On-Chip Quad-Wavelength Pyroelectric Sensor for Spectroscopic Infrared Sensing.

Merging photonic structures and optoelectronic sensors into a single chip may yield a sensor‐on‐chip spectroscopic device that can measure the spectrum of matter. In this work, an on‐chip concurrent multiwavelength infrared (IR) sensor, which consists of a set of narrowband wavelength‐selective plasmonic perfect absorbers combined with pyroelectric sensors, where the response of each pyroelectric sensor is boosted only at the resonance of the nanostructured absorber, is proposed and realized. The proposed absorber, which is based on Wood's anomaly absorption from a 2D plasmonic square lattice, shows a narrowband polarization‐independent resonance (quality factor – Q of 73) with a nearly perfect absorptivity as high as 0.99 at normal incidence. The fabricated quad‐wavelength IR sensors exhibit four different narrowband spectral responses at normal incidence following the predesigned resonances in the mid‐wavelength infrared region that corresponds to the atmospheric window. The device can be applied for practical spectroscopic applications such as nondispersive IR sensors, IR chemical imaging devices, pyrometers, and spectroscopic thermography imaging.

Surface-enhanced infrared absorption

Infrared spectroscopy is a powerful tool for the detection and identification of molecules. However, its application is limited by the low infrared absorption cross-sections of molecules. Localized surface plasmon resonances in metal and highly-doped semiconductor nanomaterials can produce large localized electromagnetic field enhancements. When molecular vibrations are in resonance with localized surface plasmon resonances, molecular vibrations are able to be largely amplified. The detection of minute amounts of target molecules can be realized in this way. Surface-enhanced infrared absorption (SEIRA) spectroscopy has recently attracted extensive attention owing to its enormous potential in molecular detection in chemistry, biology and medicine. In this review article, the enhancement mechanism and theoretical models of SEIRA are first introduced. The preparation methods and enhancement effects of various infrared-responsive nanomaterials are then discussed. The applications of SEIRA in diverse areas, such as hyperspectral infrared chemical imaging, detection of biomolecules, monitoring of pollutants in the environment, and on-chip gas sensing, are finally summarized.

Feasibility of attenuated total reflection-fourier transform infrared (ATR-FTIR) chemical imaging and partial least squares regression (PLSR) to predict protein adhesion on polymeric surfaces.

Predicting the degree to which proteins adhere to a polymeric surface is an ongoing challenge in the scientific community to prevent non-specific protein adhesion and drive favourable protein - surface interactions. This work explores the potential of multivariate PLSR modelling in conjunction with Attenuated Total Reflection - Fourier Transform Infrared (ATR-FTIR) chemical imaging to investigate whether experimentally characterised surface chemistry can be used to predict surface protein adhesion. ATR-FTIR spectra were collected on dry and wetted polymeric surfaces, followed by evaluation of adhered fibrinogen on surfaces using the micro bicinchoninic (BCA) protein assay as a reference method. Partial Least Squares Regression (PLSR) models were built using IR spectra as the predictor variable. Overall the models built with 'wetted polymer' IR spectra performed better as compared to the models built using 'dry polymer' IR spectra (average coefficient of determination, R2P 0.998, 0.996 respectively), with the lowest error in prediction (4 ± 0.6 μg) for ultra-high molecular weight polyethylene (UHMPE) as a test surface. This indicates the potential of this method to predict the degree to which protein adhesion occurs on polymeric surfaces using experimentally determined surface chemistry.

Hybrid collagen/pNIPAAM hydrogel nanocomposites for tissue engineering application

The present work explores new hybrid bioactive, enzymatically degradable hydrogel nanocomposites. They are composed by stimuli-sensitive semi-interpenetrating collagen/poly(N-isopropyl acrylamide) polymeric matrix, Dellite® 67G and Cloisite® 93A nanoclays, and hydroxyapatite particles. Morphology of the hybrid hydrogel nanocomposites was examined by near infrared chemical imaging, X-ray diffraction, scanning electron microscopy, and transmission electron microscopy techniques. It has been found that the porous hydrogel nanocomposites showed a mix between intercalated and exfoliated structure, with interconnected pores and the inorganic material was evenly distributed in the polymeric matrix because of specific interactions between components. The collagen resistance against enzymatic degradation and the thermal stability were improved due to the protein encapsulation in the synthetic polymer matrix. The hydrogel nanocomposites showed suitable swelling characteristics for tissue engineering. In vitro cytocompatibility and cell viability revealed that the hybrid nanocomposites were non-cytotoxic for rat osteoblasts. These hybrid nanocomposites were designed as potential synthetic bone tissue engineering.

Concentration monitoring with near infrared chemical imaging in a tableting press

Monitoring powder potency and homogeneity is important in achieving real-time release testing in a continuous tablet manufacturing operation. If quality related issues are encountered, monitoring powder potency inside a feed frame offers a last opportunity to intervene in the process before tablet compression. Feed frame monitoring methods based on near infrared (NIR) spectroscopy have been increasingly reported in recent years. New process analytical tools with the potential of being deployed alone or in combination with NIR spectroscopy for feed frame monitoring are now available commercially. The present study evaluated the potential of near infrared chemical imaging (NIR CI) for in-line monitoring of a prototype pharmaceutical composition containing ascorbic acid (AA), microcrystalline cellulose and dicalcium phosphate. NIR spectroscopy was the reference method. In-line calibration models based on partial least square regression were developed and validated with a range of AA concentrations. The ability of NIR spectroscopy and NIR CI to predict concentrations in test runs was ascertained both independently and in combination. NIR CI, with a single bandpass filter, predicted AA concentrations—present at commercially relevant concentrations—with acceptable accuracy. Comparative results showed that NIR CI has the potential for in-line monitoring of blend concentrations inside feed frames. In addition to the advantage of increased sample size, it also has the potential to detect segregation inside feed frames.

Nanoantenna-Enhanced Infrared Spectroscopic Chemical Imaging.

Spectroscopic infrared chemical imaging is ideally suited for label-free and spatially resolved characterization of molecular species, but often suffers from low infrared absorption cross sections. Here, we overcome this limitation by utilizing confined electromagnetic near-fields of resonantly excited plasmonic nanoantennas, which enhance the molecular absorption by orders of magnitude. In the experiments, we evaporate microstructured chemical patterns of C60 and pentacene with nanometer thickness on top of homogeneous arrays of tailored nanoantennas. Broadband mid-infrared spectra containing plasmonic and vibrational information were acquired with diffraction-limited resolution using a two-dimensional focal plane array detector. Evaluating the enhanced infrared absorption at the respective frequencies, spatially resolved chemical images were obtained. In these chemical images, the microstructured chemical patterns are only visible if nanoantennas are used. This confirms the superior performance of our approach over conventional spectroscopic infrared imaging. In addition to the improved sensitivity, our technique provides chemical selectivity, which would not be available with plasmonic imaging that is based on refractive index sensing. To extend the accessible spectral bandwidth of nanoantenna-enhanced spectroscopic imaging, we employed nanostructures with dual-band resonances, providing broadband plasmonic enhancement and sensitivity. Our results demonstrate the potential of nanoantenna-enhanced spectroscopic infrared chemical imaging for spatially resolved characterization of organic layers with thicknesses of several nanometers. This is of potential interest for medical applications which are currently hampered by state-of-art infrared techniques, e.g., for distinguishing cancerous from healthy tissues.