Hasil untuk "Analytical chemistry"

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DOAJ Open Access 2024
Biobanks: Archives or Resources? Their Secondary Use for Forensic Purposes—A Systematic Review

Giulia Sguazzi, Giulia Fasani, Filippo Renò et al.

Since the biobanks’ inception in 1980, millions of human biological samples have been stored worldwide for medical research or treatment purposes. Today the secondary use of biobanks plays an increasingly important role in research projects because it allows large-scale research starting from professional collections of biospecimens and related clinical data. It would be limiting, in the “-omics” era, to not consider the enormous potential value to law enforcement of these biospecimens, where the availability of high-performance techniques makes it possible to obtain a large amount of data, even within a single session. Therefore, the quality of the sample, in addition to the associated clinical information, becomes of crucial importance to derive scientifically valid information, including for forensic research purposes. Proposing the introduction of the concept of “solidarity”, traditionally applied only to medical and research biobanks, led to public commitment to forensic medicine. Granting the forensic researcher this possibility certainly raises some questions regarding regulatory and ethical aspects of consent, privacy, confidentiality, transparency, and participant/donor trust. Since the debate has not stopped since the origin of biobanks, this review aims to explore the state of the art relating to the use of human biological material in medical biobanks for biomedical and forensic research.

Social pathology. Social and public welfare. Criminology, Analytical chemistry
DOAJ Open Access 2024
Comparing Warm and Cold Gutta-Percha Techniques for Root Canal Filling: An In Vitro Study

B Swathika, Syed Nahid Basheer, S Sriram et al.

Background: Gutta-percha is commonly used in endodontic therapy for obturating root canals after cleaning and shaping procedures. Warm and cold gutta-percha techniques are two common methods employed for obturation, each with its own advantages and limitations. Materials and Methods: Twenty extracted human teeth with single-rooted canals were selected and divided into two groups: warm gutta-percha obturation and cold gutta-percha obturation. In the warm gutta-percha group, gutta-percha was heated to a predetermined temperature using a warm gutta-percha heating device and injected into the root canal using a heated carrier. In the cold gutta-percha group, gutta-percha was applied directly to the root canal without prior heating. Root canal obturation quality was assessed using radiographic imaging to evaluate the presence of voids, completeness of obturation, and adaptation to the canal walls. Micro-computed tomography (micro-CT) analysis was also performed to quantify the volume of obturating material and assess the three-dimensional distribution of gutta-percha within the root canal space. Results: Both warm and cold gutta-percha techniques demonstrated effective obturation of root canals, with comparable outcomes in terms of void formation, completeness of obturation, and adaptation to canal walls. However, micro-CT analysis revealed differences in the volume and distribution of gutta-percha within the root canal space. Warm gutta-percha obturation exhibited more uniform distribution of gutta-percha material and higher volumetric filling compared to cold gutta-percha obturation. Additionally, the warm gutta-percha technique demonstrated superior flowability and adaptation to irregularities within the root canal system. Conclusion: In this in vitro study, warm gutta-percha obturation demonstrated advantages over cold gutta-percha obturation in terms of volumetric filling, distribution within the root canal space, and adaptation to canal irregularities.

Pharmacy and materia medica, Analytical chemistry
DOAJ Open Access 2024
Independent concentration extraction as a novel green approach resolving overlapped UV–Vis binary spectra and HPTLC-densitometric methods for concurrent determination of levocloperastine and chlorpheniramine

Ekram H. Mohamed, Hany A. Batakoushy, Adel Ehab Ibrahim et al.

Abstract Background The proposed research study introduces independent concentration extraction (ICE) as a novel UV–Vis spectrophotometric approach. The approach can be used for extracting the concentration of two analytes with severely overlapped spectra from their binary mixtures. ICE is based on spectral extraction platform involving simple smart successive methods that can directly extract the original zero order spectra of the analytes at their characteristic (λmax). Chlorpheniramine maleate (CPM) and Levocloperastine fendizoate (LCF) are two commonly co-formulated drugs in cough preparations. The combined mixture was used to confirm the validity of the developed ICE tool. Another less green HPTLC was developed for the first time to separate both drugs and help also in confirming the proposed tool. Methods For the simultaneous determination of CPM and LCF, two ecologically friendly techniques were employed. The first approach encompasses the use of the ICE spectrophotometric method that could be successively applied for extracting the concentration of two analytes with severely overlapped unresolved spectra in their binary mixtures. Other complementary methods aiming at original spectral extraction; including spectrum subtraction (SS) and unity subtraction (US) were also successfully employed to resolve the zero order spectra of the combined drugs with all their characteristic features and peaks. The second technique used, a high-performance TLC-densitometric one, was performed on silica plates with silica plates F254 and a mobile phase with a ratio of 3:3:3:1 by volume of toluene, ethanol, acetone, and ammonia as a developing system at 230 nm. Results The presented extraction approach was executed without any optimization steps or sample pretreatment for the simultaneous determination of CPM and LCF. The method was found to be valid for their determination within concentration range of 3.0–30.0 μg mL−1 for both drugs. For HPTLC method, the resulting Rf values of CPM and LCF were 0.37 and 0.78, within concentration ranges of 0.3–4.0 μg/spot and 0.8–10.0 μg/spot, respectively. Greenness assessment of both developed methodologies showed that the HPTLC method is less green than the spectrophotometric method, yet with comparable sustainability when it comes to the used technique. Conclusion The procedures were found to be selective, accurate, and precise for analysis of the studied binary mixture. Furthermore, the environmental impact of the introduced methods was assessed using novel greenness metrics, namely AGREE and Green Analytical Procedure Index (GAPI) to prove their ecological safety. In addition, white analytical chemistry (WAC) evaluation metric was employed to ensure the synergy and coherence of analytical, practical, and ecological attributes.

DOAJ Open Access 2024
Crystallization of molecular layers produced under confinement onto a surface

Jincheng Tong, Nathan de Bruyn, Adriana Alieva et al.

Abstract It is well known that molecules confined very close to a surface arrange into molecular layers. Because solid-liquid interfaces are ubiquitous in the chemical, biological and physical sciences, it is crucial to develop methods to easily access molecular layers and exploit their distinct properties by producing molecular layered crystals. Here we report a method based on crystallization in ultra-thin puddles enabled by gas blowing, which allows to produce molecular layered crystals with thickness down to the monolayer onto a surface, making them directly accessible for characterization and further processing. By selecting four molecules with different types of polymorphs, we observed exclusive crystallization of polymorphs with Van der Waals interlayer interactions, which have not been observed with traditional confinement methods. In conclusion, the gas blowing approach unveils the opportunity to perform materials chemistry under confinement onto a surface, enabling the formation of distinct crystals with selected polymorphism.

DOAJ Open Access 2023
Aroma Component Analysis Using HS/SPME-FID Gas Chromatograph in Basmati Rice Varieties of Punjab, Pakistan

Farah Shamim, Mohsin Ali Raza, Syed Sultan Ali et al.

Aroma is a promising quality factor for rice grain that impacts consumer acceptability. The principal volatile compound that adds Basmati rice fragrance is 2-acetyl-1-pyrroline (2AP). Milled White rice of 04 promising varieties i.e., Super Basmati, Basmati-515, Basmati 2000and Basmati 370 were evaluated for volatile compounds by gas chromatography (GC) coupled with Solid Phase Micro Extraction unit (SPME) using Flame Ionizing Detector (FID). Six volatile compounds (nonanal, decanal, and alcohols such as benzyl alcohol, indole) were identified in the tested varieties, among them 2-AP is only present in aromatic rice varieties. This study confirmed the occurrence of 2-AP in all studied varieties with highest concentration in Super Basmati followed by Basmati-515, Basmati 2000 and Basmati 370.

Environmental sciences, Analytical chemistry
DOAJ Open Access 2022
Rapid Screening of 352 Pesticide Residues in Chrysanthemum Flower by Gas Chromatography Coupled to Quadrupole-Orbitrap Mass Spectrometry with Sin-QuEChERS Nanocolumn Extraction

Yuanyuan Wang, Zhijuan Meng, Chunyan Su et al.

To analyze pesticide residues, GC coupled with quadrupole-Orbitrap MS (GC-Orbitrap-MS) has become a powerful tool because of its unique characteristics of accurate mass full-spectrum acquisition, high resolution, fast acquisition rates, and overcoming matrix interference. This paper presents an efficiency evaluation of GC-Orbitrap-MS for identification and quantitation in the 352 pesticide residues analysis of chrysanthemum flowers in full-scan mode. A streamlined pretreatment approach using one-step extraction and dilution was used, which provided high-throughput processing and excellent recovery. The samples were extracted using acetonitrile. The extracted solution was purified by a Sin-QuEChERS Nano column to suppress the matrix in chrysanthemum flowers and determined by GC-Orbitrap-MS. The calibration curves for the 352 pesticides obtained by GC-Orbitrap-MS were linear in the range of 0.5–200 μg·kg−1, with the correlation coefficients higher than 0.99. The limits of detection (LODs) and the limits of quantification (LOQs) for the 352 pesticide residues were 0.3–3.0 μg·kg−1 and 1.0–10.0 μg·kg−1, respectively. The average recoveries in chrysanthemum flower at three levels were 95.2%, 88.6%, and 95.7%, respectively, with relative standard deviations (RSDs) of 7.1%, 7.5%, and 7.2%, respectively. Lastly, the validated method and retrospective analysis was applied to a total of 200 chrysanthemum flower samples bought in local pharmacies. The proposed method can simultaneously detect multipesticide residues with a good performance in qualitative and quantitative detection.

Analytical chemistry
DOAJ Open Access 2022
Essential Mineral Content (Fe, Mg, P, Mn, K, Ca, and Na) in Five Wild Edible Species of <i>Lactarius</i> Mushrooms from Southern Spain and Northern Morocco: Reference to Daily Intake

Alejandro R. López, Marta Barea-Sepúlveda, Gerardo F. Barbero et al.

Mushroom consumption has increased in recent years due to their beneficial properties to the proper functioning of the body. Within this framework, the high potential of mushrooms as a source of essential elements has been reported. Therefore, the present study aims to determine the mineral content of seven essential metals, Fe, Mg, Mn, P, K, Ca, and Na, in twenty samples of mushrooms of the genus <i>Lactarius</i> collected from various locations in southern Spain and northern Morocco, by FAAS, UV-Vis spectroscopy, and ICP-OES after acid digestion. Statistics showed that K was the macronutrient found at the highest levels in all mushrooms studied. ANOVA showed that there were statistically significant differences among the species for K, P, and Na. The multivariate study suggested that there were differences between the accumulation of the elements according to the geographic location and species. Furthermore, the intake of 300 g of fresh mushrooms of each sample covers a high percentage of the RDI, but does not meet the recommended daily intake (RDI) for any of the metals studied, except for Fe. Even considering these benefits, the consumption of mushrooms should be moderated due to the presence of toxic metals, which may pose health risks.

Biology (General)
DOAJ Open Access 2021
Simplified Point-of-Care Full SARS-CoV-2 Genome Sequencing Using Nanopore Technology

Anton Pembaur, Erwan Sallard, Patrick Philipp Weil et al.

The scale of the ongoing SARS-CoV-2 pandemic warrants the urgent establishment of a global decentralized surveillance system to recognize local outbreaks and the emergence of novel variants of concern. Among available deep-sequencing technologies, nanopore-sequencing could be an important cornerstone, as it is mobile, scalable, and cost-effective. Therefore, streamlined nanopore-sequencing protocols need to be developed and optimized for SARS-CoV-2 variants identification. We adapted and simplified existing workflows using the ‘midnight’ 1200 bp amplicon split primer sets for PCR, which produce tiled overlapping amplicons covering almost the entire SARS-CoV-2 genome. Subsequently, we applied Oxford Nanopore Rapid Barcoding and the portable MinION Mk1C sequencer combined with the interARTIC bioinformatics pipeline. We tested a simplified and less time-consuming workflow using SARS-CoV-2-positive specimens from clinical routine and identified the CT value as a useful pre-analytical parameter, which may help to decrease sequencing failures rates. Complete pipeline duration was approx. 7 h for one specimen and approx. 11 h for 12 multiplexed barcoded specimens. The adapted protocol contains fewer processing steps and can be completely conducted within one working day. Diagnostic CT values deduced from qPCR standardization experiments can act as principal criteria for specimen selection. As a guideline, SARS-CoV-2 genome copy numbers lower than 4 × 10<sup>6</sup> were associated with a coverage threshold below 20-fold and incompletely assembled SARS-CoV-2 genomes. Thus, based on the described thermocycler/chemistry combination, we recommend CT values of ~26 or lower to achieve full and high-quality SARS-CoV-2 (+)RNA genome coverage.

Biology (General)
DOAJ Open Access 2021
Thioredoxin-dependent system. Application of inhibitors

Anna Jastrząb, Elżbieta Skrzydlewska

One of the systems responsible for maintaining cellular redox homeostasis is the thioredoxin-dependent system. An equally important function of this system is the regulation of the expression of many proteins by the transcription factor NF-κB or the apoptosis regulating kinase (ASK-1). Since it has been shown that the Trx-dependent system can contribute to both the enhancement of tumour angiogenesis and growth as well as apoptosis of neoplastic cells, the search for compounds that inhibit the level/activity of Trx and/or TrxR and thus modulate the course of the neoplastic process is ongoing. It has been shown that many naturally occurring polyphenolic compounds inactivate elements of the thioredoxin system. In addition, the effectiveness of Trx is inhibited by imidazole derivatives, while the activity of TrxR is reduced by transition metal ions complexes, dinitrohalobenzene derivatives, Michael acceptors, nitrosourea and ebselen. In addition, research is ongoing to identify new selective Trx/TrxR inhibitors.

Therapeutics. Pharmacology
DOAJ Open Access 2021
Assessment of Pb, Cd, As and Hg concentration in edible parts of broiler in major metropolitan cities of Tamil Nadu, India

Mathaiyan M, Natarajan A, Xavier Rajarathinam et al.

The risk of heavy metals contamination in meat and meat products is of great concern for both food safety and from human health point of view. The present study was carried out to assess the heavy metal residues such as Pb, Cd, As and Hg in broiler chicken meat, neck and edible organs (liver and kidney). In the present study, 150 samples were randomly collected from major cities (Chennai, Coimbatore, Madurai, Trichy, and Salem) of Tamil Nadu state, India and analyzed for Pb, Cd, As and Hg residues (mg/kg) using inductively coupled plasma-mass spectrometry (ICP-MS) technique. The results revealed that lead (Pb) concentration was higher in meat and liver samples of all cities and the highest concentration was detected in Chennai followed by Coimbatore, whereas in kidney and neck samples, Chennai metropolitan alone exceeded the MRL value of 0.5 and 0.1 mg/kg respectively. The residues of cadmium and mercury in meat and meat samples were within the permissible limit in all the metropolitans. Arsenic was found exceeding the MRL of 0.1 mg/kg in the breast samples of all the metropolitans (0.2141–2.2285 mg/kg, the highest being in Trichy), except for Madurai, which recorded very low value (0.0239 mg/kg). Arsenic was found in the range of 0.1110–1.0850 mg/kg in liver samples thus exceeding MRL value. Neck and kidney samples did not contain any Arsenic. Thus it can be concluded that the lead concentration in meat and edible organ samples collected from all the metropolitans exceeded the MRL values and is an indication of contamination. Appropriate precautions are warranted to minimize the heavy metal consumption contamination especially of Pb and As.

Toxicology. Poisons

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