Search Results (23)

International efforts are being made to reduce environmental pollution caused by microplastics (MPs). Microplastics are released into the environment through sewage treatment sludge, and the use of sludge as a soil improvement agent is increasing rapidly, emphasising the importance of controlling microplastics in sewage treatment facilities. The release of microplastics into the environment is an increasingly significant concern, with sources including sewage treatment sludge. This study focuses on the analysis of microplastics in sewage sludge using optical (Fourier-transform infrared spectroscopy, FTIR) and thermal (Thermo Extraction Desorption–Gas Chromatograph–Mass Spectroscopy, TED-GC-MS) processing-based analytical equipment. The average amount of MPs in the sewage sludge analysed using FTIR was 228.5 microplastics/g of sludge (MPs/g), primarily of the polypropylene type. Approximately 75% of the MPs were 0.1 mm in size or smaller. However, the average amount of MPs in the sewage sludge determined using TED-GC-MS was 95.79 µg-MPs/g. For the systematic management of microplastics, it is important to estimate the amount of microplastics generated by sewage treatment plants. Therefore, a microplastic generation calculation formula was proposed and used to estimate the potential microplastic generation in sewage treatment plants. The total amount of MPs generated from sewage treatment plants in South Korea, calculated using the equation, was approximately 364 ton/yr; we further divided the total amount by administrative regions. The findings of this study can be applied to assess global trends in MP research. Full article

Lysergic acid diethylamide (LSD) analogs, often referred to as new psychoactive substances, are synthesized to mimic controlled substances while evading drug regulations. This study emphasizes the challenges of identifying these compounds, particularly their isomeric forms. Gas chromatography–mass spectrometry (GC–MS) and UV spectroscopy were employed to analyze 13 LSD analogs. The effects of different solvents on the detection of these analogs were analyzed, demonstrating that solvents like diethyl ether, tert-butyl methyl ether, dichloromethane and acetone provided the best sensitivity and stability. Methanol, on the other hand, causes alcoholysis of many LSD analogs, which may lead to false results. Additionally, effective chromatographic separation of isomers was established, including LSD, MiPLA, LAMPA, 1P-LSD and 1P-MiPLA, as well as 1cP-LSD and 1cP-MiPLA, which is crucial for accurate identification. The elution order of the determined compounds with the use of developed chromatographic method was as follows: LSD, MiPLA, LAMPA, AL-LAD, LSZ, 2-Br-LSD, ALD-52, 1P-LSD, 1P-MiPLA, 1B-LSD, 1V-LSD, 1cP-LSD and 1cP-MiPLA. Differences in ion ratios observed in mass spectrometry (MS) were also analyzed to distinguish between closely related compounds. Several key ions for LSD analogs were able to be identified, including 221, 208, 207, 196, 194, 192, 181, 167, 154, 152 and 128 m/z. In analogs with an N-diethyl group (or variants like N-methyl-propyl in LAMPA or N-methyl-isopropyl in MiPLA), mass spectra showed fragments 100, 72 and 58 m/z. For LSZ, the cyclic group at R1 produces ions 98 and 70 m/z. Analogs with an N6 allyl group (e.g., AL-LAD) show a characteristic ion 247 m/z. This method allows for the correct differentiation of structural isomers based on their unique ion fragmentation patterns and relative intensities. UV spectroscopy was used as a supplementary tool for screening, though it has limitations in analyzing complex mixtures. This work contributes to the forensic identification of designer LSD analogs, ensuring reliable detection for legal and toxicological investigations. Full article

The melon fruit fly, Bactrocera zonata (Coquillett) (Diptera: Tephritidae), is a notorious pest, posing a significant threat to a wide range of fruits and vegetables, leading to substantial agricultural losses worldwide. With growing concerns over chemical pesticide resistance and environmental safety, plant-based insecticides have emerged as eco-friendly and economically sustainable alternatives. In this context, the present study delves into the insecticidal potential of Ricinus communis extracts against B. zonata. The crude extract of R. communis was systematically fractionated using a series of organic solvents with increasing polarities. The fraction demonstrating the highest insecticidal activity was further purified for the isolation of bioactive compounds, employing advanced chromatographic techniques such as Column Chromatography, coupled with state-of-the-art analytical methods including Gas Chromatography-Mass Spectrometry (GC-MS) and Fourier Transform Infrared Spectroscopy (FTIR). Bioassays were conducted on B. zonata using the crude extract and its fractions in n-hexane, methanol, and ethyl acetate. Among the isolated compounds, 11,14,17-Eicosatrienoic acid was identified in both the methanol and ethyl acetate fractions. This compound exhibited remarkable insecticidal efficacy, with an LC₅₀ value of 1.36%, a linearity of R² = 0.64, and a statistically significant probability (p < 0.01). Particularly, 11,14,17-Eicosatrienoic acid emerged as the most potent bioactive agent against B. zonata highlighting its potential as a natural insecticide. These findings underscore the potential of R. communis as a valuable source of bioactive compounds for the sustainable management of B. cucurbitae. This study not only broadens the scope of plant-based pest control strategies but also opens avenues for further exploration of natural compounds in integrated pest management. Full article

Fusarium wilt caused by Fusarium oxysporum f. sp. pisi (Fop) poses significant threats to pea cultivation worldwide. Controlling this disease is mainly achieved through the integration of various disease management procedures, among which biological control has proven to be a safe and effective approach. This study aims to extract and identify antifungal secondary metabolites from Streptomyces alboflavus KRO3 strain and assess their effectiveness in inhibiting the in vitro growth of Fop. This bacterial strain exerts in vitro antagonistic activity against Fop, achieving highly significant inhibition over one week. The ethyl acetate extract, obtained from its ISP2 agar medium culture, also exhibited strong antifungal activity, maintaining an inhibition rate of approximately 90% at concentrations up to 250 µg/plug compared to the control. Thus, the organic extract has been fractionated using chromatographic techniques and its bioguided purification allowed us to isolate the main bioactive compound. This latter was identified as metacycloprodigiosin using nuclear magnetic resonance (NMR) spectroscopy, electrospray ionization mass spectrometry (ESI-MS), and specific optical rotation data. Metacycloprodigiosin demonstrates dose-dependent inhibitory activity against the phytopathogen with an effective concentration of 125 µg/plug. The other secondary metabolites present in the ethyl acetate extract were also identified by gas chromatography–mass spectrometry (GC-MS) and nuclear magnetic resonance (NMR). This study highlighted the potential of S. alboflavus KRO3 strain and its antimicrobial compounds for the management of the pea pathogen Fusarium oxysporum f. sp. pisi. Full article

Many naturally occurring chemical metabolites with significant cytotoxic activities have been isolated from medicinal plants and have become the leading hotspot of anti-cancer research in recent years. Hyptis rhomboidea Mart. et Gal is used as a folk medicine in South China to treat or assist in the treatment of liver disease, ulcers, and edema. But its chemical constituents have not been fully investigated yet. This study aimed to assess the cytotoxicity of H. rhomboidea, which was chemically characterized by chromatography–mass spectrometry methods. The results showed that the 95% ethanol extract of H. rhomboidea has marked inhibitory effects on five human cancer cell lines (HL-60, A549, SMMC-7721, MDA-MB-231, and SW480), with IC₅₀ values ranging from 15.8 to 40.0 μg/mL. A total of 64 compounds were identified by ultra-high-performance liquid chromatography with quadrupole time-of-flight mass spectrometry (UPLC-QTOF-MS) and gas chromatograph–mass spectroscopy (GC-MS) analysis of H. rhomboidea crude extract. Among them, kaempferol, quercetin, rosmarinic acid, squalene, and campesterol were found to be abundant and might be the major metabolites involved to its bioactivity. The cytotoxic characterization and metabolite profiling of H. rhomboidea displayed in this research provides scientific evidence to support its use as medicinal properties. Full article

Sustainable and safe food is an important issue worldwide, and it depends on cost-effective analysis tools with good sensitivity and reality. However, traditional standard chemical methods of food safety detection, such as high-performance liquid chromatography (HPLC), gas chromatography (GC), and tandem mass spectrometry (MS), have the disadvantages of high cost and long testing time. Those disadvantages have prevented people from obtaining sufficient risk information to confirm the safety of their products. In addition, food safety testing, such as the bioassay method, often results in false positives or false negatives due to little rigor preprocessing of samples. So far, food safety analysis currently relies on the enzyme-linked immunosorbent assay (ELISA), polymerase chain reaction (PCR), HPLC, GC, UV-visible spectrophotometry, and MS, all of which require significant time to train qualified food safety testing laboratory operators. These factors have hindered the development of rapid food safety monitoring systems, especially in remote areas or areas with a relative lack of testing resources. Surface-enhanced Raman spectroscopy (SERS) has emerged as one of the tools of choice for food safety testing that can overcome these dilemmas over the past decades. SERS offers advantages over chromatographic mass spectrometry analysis due to its portability, non-destructive nature, and lower cost implications. However, as it currently stands, Raman spectroscopy is a supplemental tool in chemical analysis, reinforcing and enhancing the completeness and coverage of the food safety analysis system. SERS combines portability with non-destructive and cheaper detection costs to gain an advantage over chromatographic mass spectrometry analysis. SERS has encountered many challenges in moving toward regulatory applications in food safety, such as quantitative accuracy, poor reproducibility, and instability of large molecule detection. As a result, the reality of SERS, as a screening tool for regulatory announcements worldwide, is still uncommon. In this review article, we have compiled the current designs and fabrications of SERS substrates for food safety detection to unify all the requirements and the opportunities to overcome these challenges. This review is expected to improve the interest in the sensing field of SERS and facilitate the SERS applications in food safety detection in the future. Full article

Reliable interpretation of the changes occurring in the samples during their heating is ensured by using more than one measurement technique. This is related to the necessity of eliminating the uncertainty resulting from the interpretation of data obtained by two or more single techniques based on the study of several samples analyzed at different times. Accordingly, the purpose of this paper is to briefly characterize thermal analysis techniques coupled to non-thermal techniques, most often spectroscopic or chromatographic. The design of coupled thermogravimetry (TG) with Fourier transform infrared spectroscopy (FTIR), TG with mass spectrometry (MS) and TG with gas chromatography/mass spectrometry (GC/MS) systems and the principles of measurement are discussed. Using medicinal substances as examples, the key importance of coupled techniques in pharmaceutical technology is pointed out. They make it possible not only to know precisely the behavior of medicinal substances during heating and to identify volatile degradation products, but also to determine the mechanism of thermal decomposition. The data obtained make it possible to predict the behavior of medicinal substances during the manufacture of pharmaceutical preparations and determine their shelf life and storage conditions. Additionally, characterized are design solutions that support the interpretation of differential scanning calorimetry (DSC) curves based on observation of the samples during heating or based on simultaneous registration of FTIR spectra and X-ray diffractograms (XRD). This is important because DSC is an inherently non-specific technique. For this reason, individual phase transitions cannot be distinguished from each other based on DSC curves, and supporting techniques are required to interpret them correctly. Full article

Cladanthus mixtus (L.) Chevall., Asteraceae, also known as Moroccan chamomile, is a spontaneous, annual plant growing wild in North-Western Morocco. Economically, the essential oil of C. mixtus is of high interest, Morocco being the only supplier on the international market. Two essential oil samples (EO) were isolated from aerial parts of Cladanthus mixtus (L.) Chevall., and analyzed by a combination of chromatographic and spectroscopic techniques (gas chromatography (GC) in combination with retention indices (RI), gas chromatography-mass spectrometry (GC/MS), and ¹³C NMR spectroscopy). Computer matching against the in-house ¹³C NMR library allowed the identification of the eight components at appreciable contents, namely 3,6,6,9-bis-epoxy-farnesa-1,7(14),10-triene, and its 3-epi, 9-epi, and 3,9-diepi epimers, and 6,9-epoxy-farnesa-1,7(14),10-trien-3-ol and its 3-epi, 6-epi, and 3,6-diepi epimers. Our results confirm the tremendous chemical variability of Moroccan C. mixtus essential oil and the usefulness of ¹³C NMR analysis, in combination with GC(RI), for the identification of uncommon oxygenated sesquiterpenes that induce an original composition. Full article

Chlorpyrifos^® (Thaion Agro Chemical CO., Ltd. Yannawa, Bangkok 10120, Thailand) (an almost water insoluble organophosphate insecticide) has been extensively used, resulting in the presence as a surface contaminant in foodstuffs, surface streams and soils. It is thus critically essential to develop methods to degrade or remove and eliminate this pollutant from environments. Chlorpyrifos^® has very limited solubility and so it is primarily a contaminant of the surfaces of foodstuffs. We present the effect of magnetically treated water (MTW) to remove Chlorpyrifos^® contaminating in Brassica chinensis Linn., a commonly eaten vegetable in Thailand and globally. Samples were washed with magnetically treated water (MTW) prior to detection of Chlorpyrifos^® with GC-MS (Gas Chromatograph-Mass Spectroscopy). Chlorpyrifos^® was removed by a factor of 413 times (−99.7%) by MTW compared to the un-washed sample, whereas the removal factor for tap water washing was only 9.6 (−89%). The MTW washed material easily passed safety criteria (Maximum Residue Load—MRL), but the tap water washed vegetables did not do so reliably. Although Chlorpyrifos^® may be banned in many countries, the binding properties of replacement organophosphates are likely to be similar, and so our results should generalize to pesticides in the organophosphate chemical class that are not readily water soluble. Full article

The present work deals with the production of hydrocarbons in the C5–C12 range obtained from the fast micropyrolysis of a laboratory-grown Desmodesmus sp. microalgae. It compares the properties of this specific fraction of hydrocarbons using or not using transition alumina catalysts during pyrolysis in experiments with both pure dried microalgae and its n-hexane extract. The microalgae were characterised using thermogravimetry (TG) and CHN analysis; the n-hexane extract was analysed through Fourier transform infrared spectroscopy (FTIR). The pyrolysis experiments were performed in a multi-shot pyrolyser connected online with a gas chromatograph coupled to a mass spectrometer (GC/MS). The composition of the C5–C12 fraction was compared to that of an industrial pyrolysis gasoline. The results of pyrolysis at 600 °C show that the alumina catalyst increases the quantity of C5–C12 hydrocarbon families when compared to purely thermal pyrolysis, representing about 40% of all the dry microalgae pyrolysis products. In the case of n-hexane extract, the C5–C12 area fraction corresponds to 33.5% of the whole products’ area when pyrolysis is conducted with an alumina catalyst. A detailed analysis shows that linear molecules, mainly unsaturated, are predominant in the products. Dry biomass formed more aromatic but less cyclic and alkylated molecules in relation to the n-hexane extract. Nitrogen products, essentially alkylated pyrroles, were produced in large quantities when dry biomass was used but were below the detection limit when pyrolysing the extracts. Thus, the extraction with hexane proved to be an effective way to remove nitrogen compounds, which are undesirable in fuels. The estimated low heating values of the present C5–C12 pyrolysis hydrocarbon fractions (between 43 and 44 MJ/kg) are quite comparable to the reported values for reformulated and conventional industrial gasolines (42 and 43 MJ/kg, respectively). Full article

Medicinal plants play important role in the public health sector worldwide. Natural products from medicinal plants are sources of unlimited opportunities for new drug leads because of their unique chemical diversity. Researchers have focused on exploring herbal products as potential sources for the treatment of cancer, cardiac and infectious diseases. Arisaema flavum (Forssk.) is an important medicinal plant found in the northwest Himalayan regions of Pakistan. It is a poisonous plant and is used as a remedy against snake bites and scorpion stings. In this study, two bioactive compounds were isolated from Arisaema flavum (Forssk.) and their anticancer activity was evaluated against human breast cancer cell line MCF-7 using an MTT assay. The crude extract of Arisaema flavum (Forssk.) was subjected to fractionation using different organic solvents in increasing order of polarity. The fraction indicating maximum activity was then taken for isolation of bioactive compounds using various chromatographic and spectroscopic techniques such as column chromatography, thin-layer chromatography (TLC), gas chromatography–mass spectrometry (GC-MS), Fourier transform infrared spectroscopy (FTIR) and nuclear magnetic resonance spectroscopy (NMR). Crude extract of Arisaema flavum (Forssk.), as well as various fractions extracted in different solvents such as n-hexane, chloroform and ethyl acetate, were tested against human breast cancer cell line MCF-7 using an MTT assay. The crude extract exhibited significant dose-dependent anticancer activity with a maximum activity of 78.6% at 500 µg/mL concentration. Two compounds, hexadecanoic acid ethyl ester with molecular formula C₁₈H₃₆O₇ and molar mass 284 and 5-Oxo-19 propyl-docosanoic acid methyl ester with molecular formula C₂₆H₅₀O₃ and molecular mass 410, were isolated from chloroform fraction. These compounds were tested against the MCF-7cell line for cytotoxic activity and exhibited a significant (p < 0.00l) decrease in cell numbers for MCF-7 cells with IC₅₀ of 25 µM after 48 h of treatment. Results indicated that Arisaema flavum (Forssk.) possesses compounds with cytotoxic activity that can further be exploited to develop anticancer formulations. Full article

(1) Background. The aim of this work is to combine non-invasive imaging with chemical characterization analyses to study original and restoration materials of a late 16th-century painting on a canvas representing the “Coronation of the Virgin with the Saints Ambrose and Jerome”, preserved in the Diocesan archive of Orte, a town in the district of Viterbo (Italy). The diagnostic campaign was addressed to support the restoration activities and the choice of the most suitable cleaning operations. (2) Methods. Both traditional analytical techniques and innovative multispectral imaging were applied to solve the diagnostic issues and best address the restoration of the painting. Specifically, hypercolorimetric multispectral imaging (HMI), X-ray fluorescence spectroscopy (XRF), Fourier transform infrared spectroscopy (FT-IR), optical microscopy, and gas chromatography coupled with mass spectrometry (GC-MS) were combined to obtain information on the general conservation state of the artwork and the characterization of pigments, organic binders, and superimposed materials, these last being particularly important to identify ancient and not-documented restoration intervention, enabling the correct choice of the most suitable and effective cleaning intervention. (3) Results. Multispectral data allowed us to differentiate and map original materials through infrared and ultraviolet false color images and spectral reflectance-based similarity maps, suggesting pigment attribution and focusing point analysis for characterization. This approach was particularly successful to identify and locate the presence of unaltered smalt blue in the first painting coat, which had been covered with other pigments, and to suggest the use of organic dye in mixtures with cinnabar and ochres. Spectroscopic and chromatographic techniques enabled us to identify the painting palette and confirm the use of oil-based binder for the pigments and characterize the altered top layers, made with a natural resin and an animal glue. (4) Conclusions. The characterization of the artwork’s materials was essential to select the most suitable methods and materials for the bio-cleaning, based on bacteria, experimented with during the restoration activities. Full article

A phosphorous-based bi-functional compound HPDAl was used as a reactive-type flame retardant (FR) in an epoxy thermoset (EP) aiming to improve the flame retardant efficiency of phosphorus-based compounds. HPDAl, consisting of two different P-groups of aluminum phosphinate (AHP) and phosphophenanthrene (DOPO) with different phosphorous chemical environments and thus exerting different FR actions, exhibited an intramolecular P-P groups synergy and possessed superior flame-retardant efficiency compared with DOPO or AHP alone or the physical combination of DOPO/AHP in EP. Adding 2 wt.% HPDAl made EP composites acquire a LOI value of 32.3%, pass a UL94 V-0 rating with a blowing-out effect, and exhibit a decrease in the heat/smoke release. The flame retardant modes of action of HPDAl were confirmed by the experiments of the scanning electron microscope (SEM), X-ray photoelectron spectroscopy (XPS), and thermogravimetry–Fourier transform infrared spectroscopy–gas chromatograph/mass spectrometer (TG-FTIR-GC/MS). The results indicate that the phosphorous-based FRs show different influences on the flame retardancy of composites, mainly depending on their chemical structures. HPDAl had a flame inhibition effect in the gas phase and a charring effect in the condensed phase, with a well-balanced distribution of P content in the gas/condensed phase. Furthermore, the addition of HPDAl hardly impaired the mechanical properties of the matrix due to the link by chemical bonds between them. Full article

The historical monuments of the ‘City of Temples’ (Kathmandu) represent an intrinsic component of Nepal’s cultural heritage. The 2015 devastating Gorkha earthquake, besides human casualties, has led to a widespread demolition or partial damage of monuments at UNESCO World Heritage Sites, including the ones in Durbar squares. This study, through an integrated material characterization of masonry binders, used in four case monuments from Hanuman Dhoka and Patan Durbar squares, intends to contribute to the knowledge of the technological know-how of the past in order to maintain as much as possible the original traditions and to provide appropriate conservation strategies. The analytical characterization of the ancient mortars was carried out by means of X-ray Diffraction (XRD), Attenuated Total Reflectance–Fourier Transform-Infrared Spectroscopy (ATR-FTIR), Thermogravimetric Analysis (TGA), petrographic analysis, X-ray Fluorescence spectroscopy (XRF) and Pyrolysis–Gas Chromatography–Mass Spectrometry (Py-GC-MS). The composition of the mortars has been determined and is in accordance with previous research in traditional materials used in the Nepalese architecture. Chromatographic techniques proved to be particularly important in the analysis of mortars with organic binders as they revealed the possible composition of the binding media, providing additional information valuable for the future conservation/restoration of the stone monuments of the ‘City of Temples’. Full article

The formosolv fractionation process has been demonstrated to be an effective approach toward lignin recovery as an antioxidant from lignocellulosic biomass. In this study, four lignin fractions, FL-88%, FSL-70%, FIL-70% and FL-EtAc, were isolated from Phragmites australis biomass through two-step formosolv fractionation (88% formic acid delignification followed by 70% aqueous formic acid fractionation). To better understand the structural properties of the lignin obtained from this fractionation process, four isolated lignins were successfully characterized by gel permeation chromatography (GPC), Fourier transform infrared (FT-IR), two-dimensional heteronuclear single quantum coherence nuclear magnetic resonance (2D-HSQC NMR) spectroscopy, thermogravimetric analysis (TGA) and gas chromatograph-mass spectroscopy (GC/MS). It was found that lignin depolymerization via β-O-4 cleavage occurred via a formylation, elimination and hydrolysis mechanism, accompanied by a competitive condensation reaction. Noteworthily, two-step formosolv fractionation can produce specific lignin fractions with different ABTS and DPPH radical scavenging activities. The FL-EtAc fraction with low molecular weight (M_w = 2748 Da) and good homogeneity (PDI = 1.5) showed excellent antioxidant activity, compared with the other three isolated lignin fractions, even equal to that of commercial antioxidant BHT at the same concentration of 2.0 mg·mL⁻¹. These findings are of great help for specific lignin from biomass as a natural antioxidant in the future. Full article