Gas Chromatography With Mass Spectrometry Research Articles

A Comparison between Bulgarian Tanacetum parthenium Essential Oil from Two Different Locations.

Tanacetum parthenium L. (Asteraceae) is a perennial herbaceous plant with a long-standing historical use in traditional medicine. Recently Tanacetum parthenium L. essential oil has been associated with a promising potential for future applications in the pharmaceutical industry, in the cosmetics industry, and in agriculture. Investigations on the essential oil (EO) have indicated antimicrobial, antioxidant, and repellent activity. The present study aimed to evaluate the chemical composition of Bulgarian T. parthenium essential oil from two different regions, to compare the results to those reported previously in the literature, and to point out some of its future applications. The essential oils of the air-dried flowering aerial parts were obtained by hydrodistillation using a Clevenger-type apparatus. The chemical composition was evaluated using gas chromatography with mass spectrometry (GC-MS). It was established that the oxygenated monoterpenes were the predominant terpene class, followed by the monoterpene hydrocarbons. Significant qualitative and quantitative differences between both samples were revealed. Camphor (50.90%), camphene (16.12%), and bornyl acetate (6.05%) were the major constituents in the feverfew EO from the western Rhodope Mountains, while in the EO from the central Balkan mountains camphor (45.54%), trans-chrysanthenyl acetate (13.87%), and camphene (13.03%) were the most abundant components.

Metabolomic Profile and Functional State of Oat Plants (Avena sativa L.) Sown under Low-Temperature Conditions in the Cryolithozone.

Oats are one of the most useful and widespread cereal crops in the world. In permafrost conditions (Central Yakutia), based on metabolic changes in late summer-sown oat plants (Avena sativa L.), the key processes involved in the cold acclimation of a valuable cereal species were identified. During the onset of low ambient temperatures, metabolites from leaf samples were profiled using gas chromatography with mass spectrometry (GC-MS) and were analyzed using principal component analysis (PCA). A total of 41 metabolites were identified in oat leaves. It was found that acclimation to suboptimal temperatures during the fall period leads to biochemical (accumulation of mono- and disaccharides and decrease in fatty acids and polyols) as well as physiological and biophysical changes (decrease in leaf PRI reflectance indices and chlorophyll a fluorescence). Therefore, the study contributes to a more holistic understanding of oat metabolism under low-temperature cryolithozone stress. It is believed that the analysis of changes in leaf reflection properties and JIP-test parameters of chlorophyll a fluorescence using leaf metabolomic profiling can be used in the selection of valuable varieties of cereal crops to obtain plant fodders with high nutrient contents under conditions of a sharply continental climate.

Microencapsulation by coacervation: Physicochemical and sensory properties of food flavorings

Coacervation is a low-energy method that is ideal for encapsulating heat-sensitive materials, e.g., limonene, citral, linalool, and isoamyl acetate. 
 This research used a simple coacervation method to prepare flavoring beads with alginate and Tween 80. The methods of scanning electron microscopy (SEM) and fourier transform infrared (FTIR) spectroscopy made it possible to study the morphology and structure of the flavoring beads. After the extraction, the flavor retention and structure were described using the method of gas chromatography with mass spectrometry (GC-MS). 
 The microcapsules demonstrated a retention rate of 99.07–99.73% while the encapsulation efficiency remained as high as 96.40–97.07%. The microcapsules had a mononuclear structure and ranged from spherical to elongated ellipsoids; they were sealed without agglomeration. The particle size was below 1000 µm. The GC-MS chromatograms detected neither structural changes nor any new compounds. The FTIR spectra were similar to the control but demonstrated slight shifts, which suggested fundamental structural changes caused by the coacervation. We also fortified sponge cake and jelly with flavoring beads. The sensory analysis of the sponge cake samples revealed no significant differences compared to the control. All the fortified jelly samples had higher scores for smell, taste, texture, and overall preference than the control. 
 The coacervation method proved to be an excellent solution for the problem of heat-sensitive flavorings that often lose quality or sensory attributes in food products that undergo extensive thermal treatment.

Optimization and validation for identification of volatile organic com-pounds released from Trogoderma variabile Ballion using headspace solid-phase microextraction and GC-FID/MS

Volatile organic compounds (VOC) emitted by Trogoderma variabile at different life stages (larvae, female and male) can help us to understand the chemical signals that are released by the beetle which can serve as biomarkers for diagnostic purpose. There are several factors that effect on the optimization of VOC extraction including, temperature, jar size, number of insects, duration of extraction, and gas chromatography (GC) conditions. This study used headspace solid phase microextraction (HS-SPME) fibre coupled with flame ionization detection (FID) and gas chromatography with mass spectrometry (GC-MS) to determine the optimal method for accurate, rapid and cost-effective extraction and identification of VOC from different life stages of T. variabile. The HS-SPME technique and the analytical conditions with GC and GCMS were optimized and validated for the determination of VOCs released from T. variabile. Selection of the number of insects was based on the height and the number of peaks. Results showed that 15 and 20 larvae and adults respectively gave the best number of peaks. Sixteen hours were optimized as the best extraction time for larvae and adults to get maximum number of emitted VOCs. The number of compound released from T.variabile different stages was 7, 9 and 11 for male, female and larvae respectively. Furthermore, some compounds were identified in all stages such as oxime-, methoxy-phenyl, 2(3H)-furanone, 5-ethyldihydro- and nonanal. Also, most of the compounds were significantly different in peak area between different life stages.

Quality of New Domestic Hand Sanitizer Drug Product Manufacturers During COVID-19.

The FDA initiated a cross-sectional, statistically based sampling and testing study to characterize the quality of marketed alcohol-based hand sanitizer (ABHS) by evaluating the alcohol content and impurities present in ABHS products manufactured by establishments that registered with the FDA during March-April 2020. A stratified sampling design divided the population of manufacturers into independent groups based on each establishment's level of experience with FDA oversight and its geographic location. ABHS products were collected and analyzed by spatially offset Raman spectroscopy and gas chromatography with mass spectrometry (GC-MS). The GC-MS results for 310 products, from 196 newly registered domestic manufacturers, showed that 71.6% (± 5.7%) of these manufacturers had violative products. In 104 (33.5%) cases, the alcohol content did not meet label claim assay specifications but still fell within CDC efficacy ranges. Ethanol ABHS products failed more often overall (assay and impurities) (84.3%) and for impurities (84.3%), than isopropanol ABHS products (11.2% and 6.2%, respectively). Differences in test results across active ingredients were statistically significant. Ethanol ABHS products often (63.5% of cases) failed due to the presence of acetal or acetaldehyde, particularly in products with pH ≤ 6. Other impurities were also detected in several ABHS products, suggesting the use of low-grade alcohol in the manufacture of these products. Evidence was insufficient to conclude that having experience manufacturing FDA-regulated products, or lack thereof, influenced product-level violative results. This study highlights the importance of sourcing and testing active pharmaceutical ingredients to produce quality drug products.

Extraction of Active Compounds from Mixtures of Hemp (Cannabis sativa) with Plants of the Zingiberaceae Family

Hemp is probably one of the most studied plants for its health-promoting properties, with countless documented and patented extraction methods, but literature is scarce on the simultaneous extraction of mixture of raw materials. Hemp, along with other plant materials, could represent a potentially highly valuable source material with resulting reciprocal effects. In this study, hemp (Cannabis sativa) and three members of the Zingiberaceae family, ginger (Zingiber officinale), turmeric (Curcuma longa), and cardamom (Elettaria cardamomum), were extracted simultaneously, and their bioactive component values were investigated. Two extraction methods were used, namely ultrasound-assisted extraction with ethanol and supercritical fluid extraction with carbon dioxide. First, extracts were obtained from separate plant materials. Then, hemp was extracted in combination with ginger, turmeric, and cardamom in a 1:1 ratio. The extracts obtained were evaluated for their antioxidant activity and total phenolic content using UV/VIS spectrophotometry; cannabinoid content, 6-gingerol, and 6-shogaol were measured using liquid chromatography coupled with tandem mass spectrometry (LC-MS/MS); volatile components such as 1,8-cineole, alpha-terpinyl acetate, linalool, and aR-turmerone were measured using gas chromatography with mass spectrometry (GC/MS).

Voltammetric analysis of mephenoxalone drug in pharmaceutical and biological samples using novel screen-printed sensor with boron-doped diamond electrode

A novel screen-printed sensor (SPE) with boron-doped diamond electrode (BDDE) for determination of a muscle relaxant and mild anxiolytic mephenoxalone (MNL) was developed. The sensor utilizes the electrochemical oxidation of MNL, which was firstly studied in aqueous solution using oxygen terminated BDDE. MNL provided an irreversible anodic signal at a potential of + 1380 mV (vs. Ag/AgCl/KCl sat.) over a wide pH range. Britton-Robinson buffer (pH 9) was selected as a suitable electrolyte and the square-wave voltammetric method (SWV) was developed. The low detection limit (55 nmol L–1), wide linear dynamic range (0.1–30 µmol L−1), and good recovery in the analysis of model and pharmaceutical samples (RSD < 1.77%) were attained. Subsequently, the new method was successfully transferred to SPE, which can find application in point-of-care testing. These sensors proved excellent sensitivity and reproducibility in the analysis of biological samples (RSD < 4.94%) without pretreatment and no need of electrolyte. Based on gas chromatography with mass spectrometry (GC-MS) analysis of preparative electrolysis products, a mechanism of the electrochemical oxidation of MNL was proposed, describing the oxidative cleavage of the alkoxybenzene ring. These results were supported with HOMO spatial distribution calculations and atomic charges calculations for arising radical cations, and with spectroelectrochemical measurements.

Mechanism, Kinetics and Simulation of Electrocatalytic Oxidation of Dimethylamine Borane (DMAB) on Electroless Gold

Dimethylamine borane ((CH3)2NHBH3) or DMAB, is broadly used as a reducing agent in electroless autocatalytic platings like gold and nickel-boron, hydrogen storage, and reductive amination. However, the mechanism of its DMAB oxidation procedure remains unclear. This project is based on the hypothesis that a multi-step electron transfer mechanism exists for oxidizing the reducing agent DMAB on gold in alkaline media. According to this mechanism, the active species produced when DMAB is used at high hydroxide content is the BH3OH-. This species is created through a series of irreversible electrochemical oxidation producing the following intermediates BH2(OH)2-, BH(OH)3- and B(OH)4-, which is the final product. Multiple electrochemical methods have been used to uncover the properties of DMAB oxidation progress and verify above-mentioned hypothesis. Electrochemical Impedance Spectroscopy (EIS) was used to test the uncompensated resistance between the working electrode and reference electrode and calibrated in the following experiments: Cyclic voltammetry (CV) showed that DMAB in hydroxide electrolytes have three half-wave potentials with E_(1/2) of -0.778, -0.174 and 0.248 V. Kinetic current values obtained from the Koutecky-Levich plot decreased with temperature with -4.065, -3.62 and -1.45 mA/cm2 at 25°C, 41°C and 52°C, respectively. Rotating Disk Electrode (RDE) and Chronoamperometry (CA) were used to determine the Diffusion Coefficient of BH3(OH)-; BH2(OH)2- and BH(OH)3- 1.38E-05, 3.31E-05 and 1.01E-04, respectively. Tafel analysis was used in obtaining the transfer coefficient, whereas Klingler and Kochi’s method evaluated the constant. These kinetic parameters were used in KISSA-1D software to simulate the CVs. Gas Chromatography with Mass Spectrometry (GC/MS) was used to verify the existence of B(OH)4- and a peak at m/z 78.8 was recorded. All of this provided evidence that the three intermediates are involved in the proposed mechanism. In the future, simulated and experimental approaches will be investigated for other amine boranes compounds such as Sodium cyanoborohydride (NaBH3CN), Sodium triacetoxyborohydride (NaBH(O2CCH3)3), and Sodium borohydride (NaBH4). This work will have far-reaching consequences in enhancing the practical applications of gold and nickel in microelectronics and fuel cells.

Applying a Green Solvent with Microwave, Ultrasound, and Soxhlet Extraction Techniques to Quantify the Slip Additive cis-1,3-Docosenamide and Nine Oxidative Degradation Byproducts in Polypropylene Samples.

Erucamide is used as an important slip agent for polymers. However, erucamide can degrade during processing and long-term storage, forming various oxidation products. These degradation products can affect the recovery rates of erucamide. In this study, investigated different solid-liquid extraction methods (Soxhlet, microwave, and ultrasound) and used gas chromatography with mass spectrometry (GC-MS) to quantify erucamide and its degradation byproducts in polypropylene (PP). A multivariable experiment was designed, and a mixed-effect approach was used to analyze the results. Various extraction variables were examined, such as temperature, time, solvents, and PP pretreatments. Using a mixed-effect model with a Kenward-Roger approximation, an R2 of the model of 97% and p values of 0.168, 0.000, and 0.000 were obtained for the technical, solvent, and type of PP pretreatment variables, respectively. The highest average recoveries of erucamide were found with the microwave technique and were 96.4% using dichloromethane, 94.57% using cyclohexane, and 93.05% using limonene. With ultrasound, recoveries ranged between 85 and 92% for dichloromethane and limonene. In addition, it was observed that the extraction method had better recovery results in ground PP than in films and in pellets. Nine oxidative degradation byproducts of erucamide were identified and semi-quantified by GC-MS. The reaction mechanisms for forming each byproduct were proposed. The byproducts that experienced a higher rate of degradation of erucamide were erucamide with a hydroxyl group at position one and 12-amino-6-12-oxo-dodecanoic acid, showing more prominent peaks using the Soxhlet method with cyclohexane and dichloromethane as solvents and polypropylene (PP) films as the type of material used.

Effectiveness of Ozonation for Improving the Microbiological Safety of Fresh-Cut Parsley (Petroselinum crispum) Leaves

In the last decade, fresh-cut plants have become a more popular flavoring additive in food. It is important to find an effective method for ensuring the safety and quality of plant materials used as food additives. Ozonated water is being considered by the EFSA for approval as a cidal agent for plant protection. The objective of this study was to evaluate the effectiveness of ozonated water in improving the microbial safety of fresh-cut parsley leaves, with a particular focus on mesophilic and psychrotrophic bacteria and fungi. The yeasts and bacteria were identified with the MALDI-TOF MS system. Color changes on the surface of the parsley samples were measured in the CIE L*a*b trichromatic color model. The chemical composition of the essential oil was evaluated via gas chromatography with mass spectrometry (GCMS). The microbial level of the fresh leaves varied and depended on the season. The highest microbial levels were found in the leaves picked in the summer and autumn, at 104 to 106 CFU/g for fungi and 106 to 108 CFU/g for bacteria. Among the isolates with the highest isolation frequency, bacteria belonging to Pseudomonas fluorescens, Staphylococcus warneri, and Bacillus megaterium dominated. The dominant yeasts and molds were Candida sp., Rhodotorula sp., Cladosporium sp., and Fusarium sp. The conditions for water ozonation (ozone dose and time) were established for both mono- and mixed cultures. Time of 3 min, ozone content of 0.5, O3 mg/L or 1 min, and 1.5 mg of O3 mg/L were sufficient for a 90% reduction in the number of living microorganisms. Yeasts and bacteria were sensitive to ozone treatment, excluding P. fluorescens rods. The tested mold strains were the most resistant. However, it was noted that organic matter might reduce the decontamination effect. The effectiveness of ozonation was negatively influenced by organic compound content above 1%. Spectrophotometric measurements of parsley leaves after ozonation, especially after 3 min treatment at 1.5 O3 mg/L, revealed morphological changes. The CIELAB color space (L*a*b*) changed in the direction of lightness and yellowness; however, ΔE showed no statistically significant differences in comparison with the untreated leaves. In preliminary studies, no differences were noted in GLC-MS chromatograms for essential oils of parsley leaves before and after ozonation. The aroma of parsley treated with ozonated water was more intensely herbal than the control sample, probably due to the higher content of α and β phellandrene. The results of this study show that decontamination of parsley leaves by ozonated water containing 1.5 O3 mg/L in a closed 5 min process can effectively ensure the microbiological quality of fresh-cut parsley leaves. It can be concluded that ozone treatments in aqueous form appear to provide promising qualitative and quantitative results for the decontamination of this fresh-cut plant material. However, more work is necessary to study chemical and volatilome changes. Especially the sensory analyses should be conducted before and after ozone treatment.

Development and Validation of Gas Chromatography–Mass Spectrometry Method for Quantification of Sibutramine in Dietary Supplements

The use of dietary supplements (DSs) has dramatically increased in recent decades. However, around 20% of these products are reported to contain pharmacologically active undeclared compounds, most of which could expose consumers to serious side effects. According to recent data, some of the most commonly detected undeclared compounds are also considered doping and are prohibited by the World Anti-Doping Agency (WADA). One of the most frequently detected undeclared substances in DSs used for promoting weight loss is sibutramine. In 2011, all medicines containing sibutramine were urgently withdrawn from Europe and US markets because of serious side effects. In the present study, in order to detect and quantify sibutramine in DSs, a rapid, sensitive, and reliable gas chromatography with mass spectrometry (GC-MS) method was developed. The method was validated according to the ICH guidelines and demonstrated good linearity, accuracy, precision, and robustness. The limits of detection and quantification were 0.181 μg/mL and 0.5488 μg/mL, respectively. The method was applied to analyze 50 DSs promoting weight loss, fat burning, and performance enhancement. Sibutramine was detected in six of them in a range of 16.59–14,854.94 μg/per capsule. The high concentrations of sibutramine detected in some samples raise concerns about the potential health risks associated with the use of adulterated DSs. The proposed GC-MS method could be used successfully in the quality control of DSs or in different research programs, contributing to safety and the prevention of associated side effects.

Comparison of recirculation and drain-to-waste hydroponic systems in relation to medical cannabis (Cannabis sativa L.) plants

Rising temperatures, higher water consumption for irrigation, and the discharge of agricultural wastewater may soon adversely affect water resources across the entire planet and its people. Agriculture consumes large amounts of water, and there is a pressing need to explore possibilities for recirculation and reuse of nutrient solutions to reduce the associated environmental and economic costs of hydroponics. This study compared two different nutrient systems for hydroponic cultivation (recirculation, RS, and drain-to-waste system, DS), and assessed their effect on the growth and concentration of elements and secondary metabolites in medical cannabis (Cannabis sativa L.) plants. The dry decomposition method with flame atomic absorption spectroscopy (FAAS) and inductively coupled plasma optical emission spectroscopy (ICP-OES) were used for the elemental analysis of plant organs. Nitrogen content was measured using the Kjeldahl method. A high-performance liquid chromatograph equipped with a diode array detector (HPLC-DAD) was used to analyze the phytocannabinoid profile in ethanolic flower extracts. Gas chromatography with flame ionization detection (GC-FID) and gas chromatography with mass spectrometry (GC-MS) were employed to determine the content of terpenic compounds in hexane extracts. Cultivation of plants with the RS system, achieved an 87% higher maximum yield of the main cannabinoid of medical cannabis chemotype I, tetrahydrocannabinolic acid (THCA), with lower total water and nutrient consumption, but with a longer cultivation time and a lower concentration of the sesquiterpene, β-caryophyllene. In contrast, the DS system enabled better control over the nutrient solution with stable delivery of the exact concentrations of nutrients. DS accelerated plant maturation, but at the cost of higher water and fertilizer consumption and a significantly lower total yield of THCA and monoterpenes.

Gas chromatography with mass spectrometry analysis of 4,4-dimethylsterols and 4-methylsterols in edible oils after their enrichment by means of solid phase extraction

4-Methylsterols (4-M-sterols) and 4,4-dimethylsterols (4,4-D-sterols) are a group of underexplored minor sterols that occur in almost all living organisms. Here, we developed a strategy for the determination of the biochemical precursors of the predominant 4-desmethylsterols in edible oils. Due to their low contribution to the sterol content in the samples, a solid phase extraction (SPE) method was developed for the enrichment of 4-M- and 4,4-D-sterols in the hexane extracts of saponified oils. In a two-fold SPE procedure, the bulk of 4,4-D-sterols was collected in one fraction. The residual sample was subjected to a second SPE step which targeted all 4-M-sterols and low shares of 4,4-D-sterols in one fraction and the predominant 4-desmethylsterols in another one. After silylation of the SPE fractions, gas chromatography with mass spectrometry (GC/MS) was used to analyze 4,4-D- and 4-M-sterols. The results were used to define eight subgroups whose characteristic structural features could be linked with the presence of specific m/z values. These m/z values were measured sensitively by GC/MS operated in selected ion monitoring (SIM) mode. Application of the GC/MS method to eighteen edible oils enabled the detection of 55 mostly very low abundant 4-M- and 4,4-D-sterols. Twenty-four of the 4-M- and 4,4-D-sterols could be assigned and the remaining 31 unknown sterols could be traced back to their basic structures.

Correlation of the Diffusion Parameters and the Biological Activities in the Formulation of Pinus halepensis Essential Oil in Phosphogypsum Material

The use of natural biopesticides, specifically essential oils, is being explored as an alternative solution to protect stored foodstuffs. This study focuses on a formulation of phosphogypsum–Pinus halepensis essential oil as a pesticidal product. First, the essential oil chemical composition was determined using gas chromatography with mass spectrometry (GC-MS), while the phosphogypsum (waste from the phosphate mining industry) was analyzed using scanning electron microscopy, X-ray fluorescence, X-ray diffraction, Fourier-transform infrared spectroscopy, and thermogravimetric–differential thermal analysis; thus, physico-chemical properties and heavy metal contents were determined. In a second step, the preparation of the formulation consists in grafting the essential oil on the phosphogypsum (adsorption) in a cylindrical geometric shape adapted to the models applied in the bioprocesses of storage. The study of essential oil transfers in the material in the case of desorption along the axis (Oz) was carried out using analytical and numerical models of the Fickian diffusion process to understand the behavior of the oil and determine physicochemical parameters such as diffusivity (D) and evaporation flux (F). By using statistical methods such as experimental design and principal component analysis, these parameters can help explain the mechanisms involved in the insecticidal activities against the primary pest of lentils (Bruchus signaticornis) and in the parameters of lentil seed germination.

Serum polybrominated diphenyl ether exposure and influence factors in blood donors of Wuxi adults from 2013 to 2016

Polybrominated diphenyl ethers (PBDEs) have been used as brominated flame retardants worldwide and are correlated with extensive environmental pollution and human health concerns. This study is aimed at analyzing the concentrations of PBDEs and at evaluating their temporal trends among a population of blood donors (n = 33) over a 4-year period. A total of 132 serum samples were used for PBDE detection. Nine PBDE congeners were quantified in serum samples by gas chromatography with mass spectrometry (GC-MS). The median concentrations of Σ9PBDEs in each year were 33.46, 29.75, 30.85, and 35.02ng/g lipid, respectively. Most of the PBDE congeners showed a downward trend from 2013 to 2014 and then increased after 2014. No correlations between age and PBDE congener concentrations were observed, while concentrations of each congener and Σ9PBDE were nearly always lower in females than in males, especially in BDE-66, BDE-153, BDE-183, BDE-190, and Σ9PBDE. We also found that the intake of fish, fruit, and eggs in the daily diet was related to the exposure level of PBDEs. Our results suggest that, as deca-BDE is still produced and used in China, diet is an important exposure pathway for PBDEs, and follow-up studies will be required to improve our understanding of the behaviors of PBDE isomers in humans and the exposure levels.

Development of the QuEChERS Extraction Method for the Determination of Polychlorinated Biphenyls (Aroclor 1254) in Soil Samples by Using GC-MS

Polychlorinated biphenyls (PCBs) have been found in soil, which has typically been the result of industrial pollution in the past two decades. Although they are banned, PCBs can still be found in soils and other environmental media. For this reason, it is critical to develop an analytical method that can reliably identify and monitor their sources. This study describes a gas chromatography with mass spectrometry (GC-MS) technique, which was used to detect PCBs in soil samples by using a fast extraction method. Using the QuEChERS (quick, easy, cheap, effective, rugged, and safe) method, PCBs were more effectively extracted from soil. Different related parameters, such as time of shaking and centrifuging, type of solvent, and clean-up adsorbents, were compared and optimized. As the extraction solvent, acetonitrile/water produced the best results, and as the dispersive solid-phase extraction sorbent, diatomaceous earth produced the best results. Procedures allowed recovery values between 95.3% and 103.2%. A limit of detection of 1.9 µg/kg was determined with relative standard deviations (n = 3) of 2.1–4.0% for intra-day assays and 3.6–5.8% for inter-day assays. It was demonstrated that the method was simple, sensitive, efficient, and environmentally friendly when applied to soil samples. To our knowledge, an integrated approach based on QuEChERS for the determination of Aroclor 1254 in soil has not been published before. It is believed that this approach will eliminate the significant challenge of sample extraction in GC-MS processing, which was considered to be a procedural challenge in previous analyses.

A novel dynamic proteomics approach for the measurement of broiler chicken protein fractional synthesis rate.

The study of protein synthesis in farm animals is uncommon despite its potential to increase knowledge about metabolism and discover new biomarkers of health and growth status. The present study describes a novel dynamic proteomics approach for the measurement of protein fractional synthesis rate (FSR) in broiler chickens. Chickens received a 10g/kg oral dose of 2 H2 O at day 21 of their life. Body water 2 H abundance was measured in plasma samples using a portable Fourier transform infrared spectrometer. Free and protein-bound amino acids (AAs) were isolated and had their 2 H enrichment measured by gas chromatography with mass spectrometry (GC/MS). Peptide 2 H enrichment was measured by proteomics analysis of plasma and muscle samples. Albumin, fibrinogen and muscle protein FSR were calculated from GC/MS and proteomics data. Ala appeared to be more enriched at the site of protein synthesis than in the AA free pools. Glu was found to be the AA closest to isotopic equilibrium between the different AA pools. Glu was used as an anchor to calculate n(AA) values necessary for chicken protein FSR calculation in dynamic proteomics studies. FSR values calculated using proteomics data and GC/MS data showed good agreement as evidenced by a Bland-Altman residual plot. A new dynamic proteomics approach for the measurement of broiler chicken individual protein FSR based on the administration of a single 2 H2 O oral bolus has been developed and validated. The proposed approach could facilitate new immunological and nutritional studies on free-living animals.

Comparative Production of Bio-Oil from In Situ Catalytic Upgrading of Fast Pyrolysis of Lignocellulosic Biomass

Catalytic upgrading of fast pyrolysis bio-oil from two different types of lignocellulosic biomass was conducted using an H-ZSM-5 catalyst at different temperatures. A fixed-bed pyrolysis reactor has been used to perform in situ catalytic pyrolysis experiments at temperatures of 673, 773, and 873 K, where the catalyst (H-ZSM-5) has been mixed with wood chips or lignin, and the pyrolysis and upgrading processes have been performed simultaneously. The fractionation method has been employed to determine the chemical composition of bio-oil samples after catalytic pyrolysis experiments by gas chromatography with mass spectroscopy (GCMS). Other characterization techniques, e.g., water content, viscosity, elemental analysis, pH, and bomb calorimetry have been used, and the obtained results have been compared with the non-catalytic pyrolysis method. The highest bio-oil yield has been reported for bio-oil obtained from softwood at 873 K for both non-catalytic and catalytic bio-oil samples. The results indicate that the main effect of H-ZSM-5 has been observed on the amount of water and oxygen for all bio-oil samples at three different temperatures, where a significant reduction has been achieved compared to non-catalytic bio-oil samples. In addition, a significant viscosity reduction has been reported compared to non-catalytic bio-oil samples, and less viscous bio-oil samples have been produced by catalytic pyrolysis. Furthermore, the obtained results show that the heating values have been increased for upgraded bio-oil samples compared to non-catalytic bio-oil samples. The GCMS analysis of the catalytic bio-oil samples (H-ZSM-5) indicates that toluene and methanol have shown very similar behavior in extracting bio-oil samples in contrast to non-catalytic experiments. However, methanol performed better for extracting chemicals at a higher temperature.

Sustainable production of nanolime using plant extracts by fermentation: A traditional approach towards conservation of heritage structures

Nanolimes have emerged as efficient consolidants for the conservation of historic and heritage structures. This research investigates an effective, economical, and sustainable way of synthesizing nanolimes using hydraulic lime and natural plant extracts. The lime is fermented with aqueous organic extract for 14 days to produce nanolimes. The fermented compounds in liquid phases and the organic extract were identified using high-performance liquid chromatography (HPLC) and gas chromatography with mass spectrometry (GC-MS). Alcohols, which are substantial fermentation byproducts, were found to aid the nanoscale dispersion of portlandite particles. The narrow size distribution and mean particle size of 130–290 nm in seven-day fermented samples were able to penetrate deeper into treated surface strata for better conservation of structures. The presence of portlandite and calcite nanoparticles observed by X-ray diffraction in nanolime assisted to fill the pores that are too big for nano-portlandite alone and intensifies its ability to hold the grains of the treated surface. The biomineralization process resulted in the development of carbonate compounds ranging in size from 0.4 to 50 nm, thus rendering nanolime as more effective and facilitating the filling of nanopores smaller than 100 nm, which eventually signifies the durability of structure. Ultimately, this research emphasizes importance of nanotechnology in resurrecting tangible heritage.

Degradation Products Assessment of the Wooden Painted Surfaces from a XVIIth Heritage Monastery

Currently, approximately 70% of paintings in museum collections are affected by the presence of metallic soaps, evidenced by spherical globules visible on the surface of the paintings. They are responsible for altering the paintings’ surface through processes such as exfoliation and cracking, or even in the form of surface “skins” that appear in the pictorial layers. The objective of this study is the investigation of the icon paintings from Saint Mary Monastery, Techirghiol, Romania, which underwent some restoration procedures. This study is so important/significant, due to the presence of efflorescence that is correlated with the conversion of some fatty acids, as palmitic acid, stearic acid and azelaic acid, in the so-called metallic soaps through the reaction of the metals contained in the pigments from the painting layer and the binder. The investigated paintings are strongly affected by zinc carboxylate aggregation, and for this, the sample was embedded in polyester resin and the obtained cross-section, after polishing, was investigated by microscopic techniques (optical microscopy (OM), stereomicroscopy, and scanning electron microscopy with electronic dispersion spectroscopy (SEM-EDS), Fourier-transform infrared spectroscopy (FTIR), Raman spectroscopy, and gas-chromatography with mass spectrometry (GC-MS) in good agreement with data from the literature. The potential result of this study is the identification and quantification of the metallic soap generated as a white deposit (probably salts, a kind of white efflorescence), from the binding medium of the metal carboxylate ionomer, by the crystallization of saturated fatty acids, through polymerization in oil. Six pigments (calcite, lithopone, carbon black, red ochre, vermilion, and ultramarine), present in the sublayers of the samples were identified.