Analytical Laboratory Research Articles

ВЛИЯНИЕ ТРИТИКАЛЕВОЙ МУКИ И ОТРУБЕЙ НА ПОКАЗАТЕЛИ КАЧЕСТВА ХЛЕБНЫХ ПАЛОЧЕК

The purpose of research is to study the influence of triticale grain processing products (flour and bran) on the quality indicators of breadsticks. Objectives: to determine the physicochemical parameters of wheat and triticale flour of the Bashkirskaya 3 variety; to study the quality indicators of triticale bran; to develop a recipe for bread sticks with partial replacement of wheat flour with triticale flour and triticale bran; to conduct a tasting assessment and examine the physical and chemical characteristics of the developed products; to study the content of protein, dietary fiber and vitamin B1 in the developed products. Research was carried out at the Department of Technology of Public Nutrition and Processing of Plant Raw Materials of the Federal State Budgetary Educational Institution of Higher Education "Bashkir State Agrarian University" and in the analytical laboratory of the Bashkir Research Institute of Agriculture UFITs RAS. The objects of the study were samples of premium wheat baking flour, triticale flour and triticale bran obtained from the Bashkirskaya 3 variety, added with different percentage replacements for wheat flour. The main research methods used: determination of the quantity and quality of raw gluten – according to GOST 27839-88; mass fraction of flour moisture according to GOST 9404-88; falling numbers – according to GOST 27676-88; mass fraction of ash – according to GOST 27494; vitamin B1 (thiamine) content – according to GOST 29138-91; mass fraction of protein – according to the Kjeldahl method, GOST 10846-91; soluble and insoluble dietary fiber by enzymatic-gravimetric method – GOST R 54014-2010 method. During research, breadsticks containing 60% triticale flour + 15 % triticale bran were identified as the most optimal in terms of organoleptic and physicochemical indicators (protein mass fraction 7.30 ± 0.05 % and vitamin B1 content 0.17 ± 0 .05) compared to the control from wheat flour (protein mass fraction 6.03 ± 0.84 % and thiamine content less than 0.1 %).

Interlaboratory Comparison for Analysis of Histamine in Fish as Per ISO/IEC 17043:2010 and ISO 13528:2015

Histamine is a significant food quality, safety, and trade issue in the fisheries sector. In the absence of adequate proficiency testing for histamine in India, it was important to organize a proficiency testing (PT) program among 22 food analytical laboratories for the external assessment of proficiency of the laboratories following ISO 17043:2010 and ISO 13528:2015. The test item (fish) prepared was sufficiently homogenous and stable for the entire duration of the PT program. The Grubbs test employed on the data showed the absence of any outlier result in the present testing scheme. The assigned value of 45.31 mg kg-1 was determined using the ‘consensus approach’ with a standard uncertainty of 1.33 mg kg-1. The robust standard deviation value was 5.02 mg kg-1. The z score for the participant results varied from -1.96 to +1.47, implying that the analytical performance of the participant laboratories was in agreement with the criteria mentioned in ISO 17043:2010. The HorRat value of 1.13, lay between the acceptable range of 0.5-2.0. The distribution of the results as depicted by the kernel density plot revealed a fairly normal distribution of the participants. All the participant laboratories were able to satisfy the proficiency testing requirements, as implied by the z score- -1.96 to +1.47. Further, proficiency testing can be carried out at various analyte levels and other matrices of commercial importance to allow for effective quality assurance.

ХОЗЯЙСТВЕННО-БИОЛОГИЧЕСКАЯ И ТЕХНОЛОГИЧЕСКАЯ ОЦЕНКА СОРТОВ И ЛИНИЙ ГОРОХА СЕЛЕКЦИИ БАШКИРСКОГО НИИСХ УФИЦ РАН

The purpose of research is to study the economic, biological and technological properties of pea variety samples selected by the Bashkir Research Institute of Agriculture UFRC RAS. The object of study is the varieties Chishminskiy 95, Chishminskiy 229, Pamyati Khangildina, Pamyati Popova, included in the State Register of Breeding Achievements of the Russian Federation, and breeding lines L-30, L-118, L-31045. The standard is the variety Aksayskiy usatyy 55. The experiments were carried out in 2020–2022 in the fields of the Chishminskiy plant breeding center. The evaluation of the studied variety samples was carried out in accordance with the methods of state variety testing. Grain yield was determined by the gravimetric method. Technological indicators of grain quality were assessed in the laboratory of selection and primary seed production of leguminous and cereal crops and in the analytical laboratory of the BRIA UFRC RAS. As a result of a comparative study, sources for a number of economically valuable traits were identified for use in breeding. Sources of early ripening can be the varieties Chishminskiy 95, Chishminskiy 229, Pamyati Khangildina, L-31045 with a growing season of 64–65 days, high grain yields – Chishminskiy 229, Pamyati Popova, L-30 (17.7–18.8 c/ha). As a source material with high technological indicators of grain quality, the varieties Chishminskiy 229, Pamyati Khangildina, L-30 with a weight of 1000 seeds over 190 g can be used; Chishminskiy 95, Chishminskiy 229, In Pamyati Khangildina, In Pamyati Popova, L-118, L-31045 with seed uniformity of 85.7–87.7 % and digestibility of 97.3–102.3 min; Chishminskiy 95, Pamyati Khangildina, Pamyati Popova, L-31045 with a grain yield of 83.1–84.2 %. Intervarietal coefficients of variation for the traits we studied were low, which is due to the genetic proximity of varieties and local breeding lines.

P0167 Circular extrachromosomal DNA (eccDNA): a potential diagnostic and prognostic tool to be introduced into the clinical practice of Inflammatory Bowel Disease

Abstract Background The diagnosis of Inflammatory Bowel Disease, which continues to increase year by year, is complex; these disorders can be confirmed by investigations such as fecal calprotectin, endoscopy, histology of biopsies, and CT scan; despite this, there is a lack of highly specific and minimally invasive techniques that allow not only diagnosis but also determination of the severity of the disease and its evolution. Given these challenges, the search for reliable and specific predictors that can direct the clinician toward personalized patient care is very important. In this context, can help extrachromosomal circular DNA (eccDNA) that are eukaryotic nuclear circle DNA molecules, independent from chromosomes, with a length ranging from a few hundred to a few thousand base pairs. In addition to its already known role in cancer, in IBD increased levels of eccDNA have been found compared with healthy controls. Circular DNA could represent a potential biomarker that can be isolated from peripheral blood or intestinal mucosa and is useful for making early diagnoses and assessing disease status. Methods We examined peripheral blood, collected by blood sampling . "Technical Tests" were performed in order to determine the right procedure for storing blood samples and optimize the results obtained in terms of eccDNA extraction . The samples will be divided into two groups, for the first group the procedure is to centrifuge the blood at 2000g for 15 minutes at different timepoints with or without storing the plasma at 4° C; for the second group the sample is centrifuged immediately after blood collection and the plasma is stored in the refrigerator at different timepoints [Table 1]. Then for both groups we proceed with eccDNA extraction by the "Circle-Seq" analysis. Results No significant differences are shown between the two groups in terms of the amount of eccDNA [Figure 1]. In particular, the non-immediate centrifugation and separation of plasma from whole blood does not negatively affect the extraction yield, highlighting that degradative factors are not present in whole blood. In addition, refrigerated storage for a longer period of time is a positive factor for eccDNA concentration, probably because in this way circular DNA found within microvesicles has time to be extruded, increasing its concentration in plasma. Conclusion Circulating eccDNAs could represent potential biomarkers to be detected in plasma by liquid biopsy, as the method is minimally invasive and easily reproducible in analytical laboratories, becoming a diagnostic and prognostic tool to be brought into clinical practice. References Fundings: European Union’s Horizon 2020 Research and Innovation Programme (899417)

A study to Determine the Antibiotic Sensitivity of Microbes Causing Cervical Infections in Women in Zawia Western Libya

Purpose: Bacterial vaginosis (BV) infections in women are typically caused by living organisms, making it one of the most significant health issues related to the vagina. Bacterial vaginitis occurs when the normal bacteria in the vagina decrease in number. Aim: This study aimed to determine the prevalence of vaginal infections and the antibiotic susceptibility of different types of bacteria among women attending Al-Zawia Medical Hospital. Methods: The study was conducted at Al-Zawia Medical Hospital from January to March 2024. Vaginal smear samples were collected from women and tested for sensitivity to antibiotics. All isolated vaginal samples were cultured using standard methods in the analytical sciences laboratory. Microbial sensitivity to antibiotics was determined using the disk diffusion technique based on the Kirby-Bauer method. Results: were analyzed descriptively. Results: Between January and March 2024, 36 vaginal swabs were collected at Al-Zawia Medical Hospital, Libya. These samples were tested at the Al-Zawia Medical Analysis Laboratory for antibiotic sensitivity. Approximately 200 women aged 10 to 54 participated in the study. Overall, 18% of women had a vaginal infection, with higher rates seen in women aged 25 to 39. Streptococcus bacteria showed 100% susceptibility to ciprofloxacin, indicating its effectiveness in inhibiting the bacteria, including Staphylococcus aureus. E. coli bacteria had a lower sensitivity in this study, with an inhibition rate of 50%. Conclusion: Bacterial vaginal infections are common among women and should be monitored regularly. Women should undergo periodic examinations for vaginal infections, and antibiotic treatment should be followed accordingly.

Characterization of 53 Multiplexed Targeted Proteomics Assays for Verification Studies in Cancer Cell Lines.

The National Cancer Institute's Clinical Proteomics Tumor Analysis Consortium (CPTAC) was established to address the need for improved design, standardization, and validation of proteomics assays to enable better translation of biomarkers from the analytical lab to the clinic. Here, we applied CPTAC guidelines to characterize quantitative mass spectrometry (MS) assays in a new multiple reaction monitoring (MRM) proteomics panel. The panel of 50 proteins was developed in response to a previous study that identified a proteomic profile of altered translational control associated with response to a new cancer drug. MRM-MS assays for 53 peptides of interest were developed, optimized, and characterized on a UPLC system coupled to a triple-quadrupole mass spectrometer (QQQ-MS) using synthetic proteotypic peptides and corresponding stable-isotope labeled internal standard (SIS) peptides. Most of the assays were found to be fit-for-purpose for biomarker verification in that they precisely and reproducibly quantify the peptides at levels corresponding to the endogenous concentration in the desired cancer cell lines. Of these, 28 peptide assays represent to proteins that previously had no associated assays published in the CPTAC database. The targeted proteins in this publicly deposited validated multiplexed panel may be of use for research applications in cancer, cellular stress, neurology, cardiology, and metabolism.

Development and validation of a liquid chromatography-tandem mass spectrometry (LC-MS/MS) assay for the quantification of oximes in KIKO mouse plasma.

Chemical warfare nerve agents (CWNAs) are potent and irreversible inhibitors of acetylcholinesterase (AChE). Oxime reactivators are an important part of the standard treatment for CWNA exposure as they can reactivate inhibited AChE. Evaluating the oxime candidates of interest in biological samples requires analytical detection methods and oxime reactivators as a class of compounds have historically been notoriously difficult to isolate, detect and analyze in an analytical laboratory, and there are currently no sensitive or robust analytical detection methods in the literature. The goal of this study was to develop reliable and robust novel extraction and liquid chromatography-tandem mass spectrometry (LC-MS/MS) methods to detect and quantitate 2-PAM, HI-6, HLö-7, and MMB-4 in a human AChE knock-in, mouse carboxylesterase knock-out (KIKO) mouse in vivo model. This study identified an LC column that achieved retention for all four oxime compounds which is a major advancement over past oxime methods. A unique extraction and chromatographic method was developed for each oxime. The developed methods were sensitive down to 0.5ng/mL for 2-PAM, 50ng/mL for HI-6, and 15ng/mL for both HLö-7 and MMB-4. These methods were validated to meet the Food and Drug Administration (FDA) bioanalytical method validation requirements under Good Laboratory Practice (GLP) conditions. The 4 methods were validated for performance by assessing linearity, sensitivity, precision, accuracy, selectivity, specificity, carryover, extraction recovery, dilution analysis, and stability.

Validated LC-MS/MS methodology for the quantification of CBD, trace level THCA and UK controlled cannabinoids (Δ9-THC, Δ8-THC, CBN and THCV) in food samples.

Products containing cannabidiol (CBD) have become increasingly popular due to consumer-perceived benefits of improving health and well-being. More specifically in the United Kingdom (UK), CBD food products are categorised as novel foods. For these products to remain on the market, they must have authorisation from the Food Standards Agency on the basis that they are safe, correctly labelled, and do not contain substances classified under controlled drugs legislation in accordance with any existing or future Home Office guidance. This demands for analytical laboratories to be able to accurately measure the CBD concentration using validated methods to confirm correct labelling, as well as the controlled cannabinoid content to ensure the products comply with legislation. To address some of these challenges, this work describes two similar liquid chromatography tandem mass spectrometry (LC-MS/MS) methods which were developed and validated for measuring CBD and trace level controlled cannabinoids in CBD containing foods. The accuracy of the methods developed were tested for the first time through an interlaboratory comparison involving expert laboratories. The methods were applied to a comprehensive study of 148 CBD edible products. In 13 of the products tested (9% of the total) CBD was found below the limit of quantification. Of the remaining 135 products (91% of the total), 66% were found to have detectable amounts of one or more controlled cannabinoids. Of the 13 samples that did not contain detectable levels of CBD, two did contain quantifiable levels of controlled cannabinoids. The validation and sample analysis results reveal intriguing sets of data which help gauge the ongoing narrative surrounding CBD analysis and CBD products available in the UK. The research contributes to the global effort to keep unsafe products off the market.

Data Processing and Reporting System for Chemical Analytical Laboratories of Environmental Control

The relevance of environmental monitoring and environmental pollution control is justified in the introduction of the article in order to monitor the state of the environment and its protection, on the basis of existing regulatory legal acts. Fundamental principles of these types of environmental activities are given. In order to justify the task, a brief description of chemical analytical laboratories (hereinafter referred to as HAL) activities and the tasks of their information systems is provided. Having analyzed a number of HAL information systems operating in the Russian Federation the authorscame to the conclusion that they mainly perform the functions of automated collecting, storing and processing information. The availability of decision-making support systems (DSS) function in the systems has not been established, for example, none of the software systems issues recommendations on changing the measurement regulations in cases of exceeding permissible values. An information system for data collection, processing and analysis from a chemical analytical laboratory with the DSS functions (monitoring changes in measurement regulations and monitoring the timing of metrologicaldevice verification) is proposed. The article describes the main functions of the proposed system available to the user and the administratorin detail. An example and a detailed description of the regulation changing process based on the MPC excess in samples are given. Regulations, the main blocks of the system, their functions and capabilities are described. The program structure and the system algorithm are presented. All system functions have been successfully tested. The figures show the algorithms of user’s and system administratoractivity when testing the database function, the function of reporting on specified parameters to obtain information about the discrepancy between samplenumbers and devices to the specified parameters, the function of automatic sampling and adding samples from the selected device and the function 'Changing the rules'. In conclusion, it is emphasized that this information system allows not only data processing from research results of chemical analytical laboratories in an automated mode, but also to perform certain functions of decision-making support systems.

Immunomonitoring in bladder cancer: a short report on stability of leukocytes and proteins in refrigerated urine samples

BackgroundUrine biomarkers are crucial for monitoring patient responses in treating urological pathologies, including non-muscle invasive bladder cancer (NMIBC). Yet, analysing urine biomarkers poses several challenges, including ensuring specimen stability during transportation and analytical processing. This prospective feasibility study aimed to investigate how urinary leukocytes and proteins are impacted by storing and refrigerating urine.MethodsStability of leukocytes from four healthy donors (HD) spiked into urine supernatants was analyzed for up to 72 h at 4°C. Urine samples from five NMIBC patients undergoing BCG treatment were divided into two portions, followed by either immediate processing or overnight refrigeration. Urinary cell content and soluble factors were analyzed by multiparameter flow cytometry and Luminex®, respectively.ResultsWe confirmed the stability of healthy donor peripheral blood leukocytes spiked into cell-free urine supernatants from healthy donors or untreated bladder cancer patients for up to 72 h under refrigeration at + 5℃. Additionally, we conducted immune cell and proteomic analysis from urine samples obtained from five NMIBC patients receiving Bacillus Calmette-Guérin (BCG) therapy either processed immediately or after overnight refrigeration. We successfully demonstrated that leukocyte and protein composition remain stable in refrigerated urine from BCG-treated NMIBC for 24 h. This included granulocytes, monocytes, and T cells, as well as total protein, creatinine and 46 additional individual immune-related mediators.ConclusionsThis work demonstrates the compatibility of refrigerated urine shipment from the collection sites to analytical laboratories with both immunophenotyping and proteomic analysis and establishes clear logistical benefits for numerous clinical settings focused on monitoring patient immune responses in the urine matrix.

Effect of Hemolysis on Routine Blood Gas and Whole Blood Analytes.

Hemolysis is a major pre-analytical concern for many laboratory analytes; however, instruments utilized for whole blood chemistries and blood gas measurements lack the ability to detect and measure the degree of hemolysis. This study evaluated the effect of hemolysis on 13 routine whole blood and blood gas analytes and compared visual assessments of hemolysis to measured hemolysis (H-index). Remnant whole blood samples (n = 85) were split into 2 portions and aspirated through a syringe one or more times. To induce hemolysis, a needle was affixed to the end of the syringe to provide shear stress, and a mock procedure without syringe was used as a control. Samples were analyzed on a Radiometer ABL800 series instrument, centrifuged, and the H-index of the plasma portion was measured. Two medical technologists recorded a visual categorization of the specimens as slightly, moderately, or severely hemolyzed. Hemolysis had a modest effect on metabolites and most cooximetry components, with percent bias within ±5% at all levels of hemolysis. Methemoglobin exhibited a larger overall negative bias, up to 13.3%. The absolute pH bias was fairly consistent (within 0.1 pH units) across all levels of hemolysis. As expected, potassium displayed a significant positive bias with increasing hemolysis. Sodium and ionized calcium displayed overall linear trends with a significant negative bias. Hemolysis can falsely increase or decrease certain blood gas analytes and lead to misinterpretation of results. Therefore, hemolysis detection capabilities are crucial for mitigating this effect and ensuring accurate results for patient care.

Increasing Authenticity of the Laboratory through the MICRO Project: Analysis of Analytical Chemistry Laboratory Experiments for Their Level of Inquiry.

Inquiry-based laboratory experiments, in comparison to traditional "cookbook" style laboratory experiments, more accurately model the work scientists do and engage students in the skills they use. Students who participate in inquiry-based laboratory experiments engage in science practices and develop skills such as critical thinking and argumentation. Despite the abundance of literature surrounding the benefits of inquiry-based laboratory learning approaches, adoption of these instructional approaches has been slow. The MICRO project was designed with the goal of supporting analytical chemistry faculty in adopting inquiry-based laboratory experiments. Laboratory experiments representing those used by institutions prior to the project and during the project were collected and analyzed for their level of inquiry. We saw a decrease in the percentage of laboratory experiments that were traditional, "cookbook" style laboratory experiments and an increase in laboratory experiments that are higher levels of inquiry during the semester of implementation of MICRO laboratory experiments, indicating faculty were adopting some inquiry-based instructional practices.

TLC densitometric approach for concurrent determination of quinary mixture for treatment of migraine with appraisal to method greenness and whiteness

A new accurate, precise thin layer chromatographic (TLC densitometric) approach was developed for the simultaneous analysis of ergotamine tartrate (ERG), phenobarbital sodium (PHEN), caffeine anhydrous (CAF), dipyrone sodium (DIP) and meprobamate (MEP) in their pure form and in their combined formulation; (MIGRANIL tablets). TLC separation depended on using a stationary phase of TLC plates F254 (20 × 10 cm) and using a developing system of ethyl acetate: methanol: n- hexane (8:2:3, by volume) with UV scanning at 254 nm for ERG, PHEN, CAF and DIP. For MEP, detection was done at 560 nm after spraying with 0.3% ethanolic solution of para -dimethylaminobenzaldehyde (PDAB) and heating at 110 ºC for 30 min. Analysis was performed in the concentration intervals of 0.06-2, 0.15–5 µg/band for ERG and PHEN, respectively; while for CAF, DIP and MEP it was done in the ranges of 0.3-9, 0.5–10, 1–100 µg/band, respectively. Moreover, the method was used for the quantitation of the five studied drugs in their unique formulation and the recovery% was calculated and found to be 102.04, 100.73, 100.65, 99.91, 1nd 101.77% for ERG, PHEN, CAF, DIP, and MEP, in order and all these outcomes proved excellent selectivity of the method. Other validation parameters were tested following ICH guidelines. Accuracy ranged from 98.02 to 100.53% while the obtained %RSD of interday day precision ranged from 1.215 to 1.940%. The environmental impact and performance of the method was tested with several tools; Analytical eco-scale, green analytical procedure index (GAPI), Analytical GREEnness Metric Approach (AGREE), Blue applicability grade index (BAGI), and RGB additive color model. Results ensured minimum hazardous effect on health and environment. This is the first analytical approach developed for simultaneous analysis of the quinary mixture which can be easily applied in any analytical laboratory.

Occupational exposure to respirable crystalline silica at an underground copper mine in Zambia.

Overexposure to respirable crystalline silica (RCS) can lead to the development of silicosis and other respiratory diseases. The mine under study was reported to have the highest number of certified cases of pneumoconiosis in Zambia in 2015, and in 2008, a study revealed that 56% of the RCS samples exceeded 0.05mg/m3. This study aims to assess occupational exposure to RCS at this underground copper mine. In this cross-sectional study, personal exposure monitoring was conducted using National Institute for Occupational Safety and Health's methods 0600 and 7602 (KBr pellet), and 114 samples were collected. Gravimetric analysis of respirable dust (RD) samples and quantification of RCS were performed at an ISO 17025:2005 accredited analytical laboratory. BOHS-NVvA 2022 standard was used for determining activity areas' overexposure. The median, 95th percentile (P95), and maximum (Max) RD concentrations were 0.279, 1.650, and 3.7mg/m3, respectively. For the RCS exposure, the median, P95, and Max RCS exposure concentrations were 0.02, 0.179, and 0.548mg/m3, respectively. Thirteen (11.7%) of the 111 samples had exposure exceeding the Republic of South Africa (RSA) TWA-OEL of 0.1mg/m3, and 11 out of 18 activity areas were statistically overexposed to RCS when applying the BOHS-NVvA 2022 standard. The number of RCS samples exceeding 0.05mg/m3 reduced from the 67% recorded in 2008 to 32.4% in this study. One factor that could have led to this reduction is the mine not working at full capacity during the sampling period. However, the lack of adherence to the occupational health and safety (OHS) guidelines by the miners still leads to personal exposure above the limits set by various countries. Exposure to RCS in more than half of the activity areas was not under control. Routine RCS monitoring in Zambian mines should be mandatory, as this is not an isolated case, though it is more of a challenge at this mine because of the high percentage of RCS in RD samples (18.5%). Miners should be continuously trained on the importance of adhering to the OHS guidelines. Furthermore, Zambia should consider adopting the RSA occupational exposure limit for RCS and the BOHS-NVvA 2022 standard for exposure level compliance testing.

Modernizing USP Melatonin Liquid Chromatographic Analyses for Increased Throughput and Reduced Environmental Impact.

Melatonin supplements are often used to alleviate jetlag and other sleep-depletion related disorders. Recent studies found large inconsistencies between labeled values and actual contents of melatonin within products, which has led to concerns over the quality of melatonin supplements. In order to facilitate the quality control testing of melatonin supplements, an improved and more modern approach to the liquid chromatographic analysis of melatonin is required. In addition, growing public concern over the environmental footprint of analytical laboratories exacerbates the need to modernize legacy analytical procedures with more eco-friendly or greener approaches. This study aims to optimize the routine liquid chromatographic analyses that are prescribed in the US Pharmacopeia (USP) melatonin monograph on a High Performance Liquid Chromatography (HPLC) system without fundamentally modifying the methods. The melatonin assay and the melatonin related compounds (impurities) test were optimized on a C18 column packed with 2.5 µm particles. The column length and the gradient elution parameters were adjusted following the guidelines on Adjustment of Chromatographic Conditions in USP General Chapter <621>. The mobile phase compositions were optimized to meet the system suitability requirements that were specified in the USP melatonin monograph. The flow rate was optimized for better separation efficiency. The optimized HPLC methods not only met the USP system suitability requirements in relative retention time (RRT), resolution, and relative standard deviation (RSD), but also demonstrated excellent linearity, sensitivity, accuracy, precision (repeatability), and would have a lower environmental impact. The optimized HPLC methods for assay of melatonin and test of its related compounds achieved significantly increased throughput and a reduced environmental impact, without fundamentally modifying the methods. The optimized HPLC methods are significantly faster and more eco-friendly. These methods can be implemented on HPLC systems without a full re-validation.

Evaluation of Biological Activity of Essential Oil from Teucrium polium L.

Background: Teucrium polium L. has an essential place in traditional medicine throughout the world. Their use, based on empirical knowledge passed down from generation to generation, has helped to treat a multitude of illnesses and relieve a variety of symptoms. These traditional practices have laid the foundations for modern research, which seeks to understand the significant antibacterial properties. The bioactive compounds present in the plant, such as essential oils and polyphenols, have demonstrated antimicrobial activity against a wide range of pathogenic bacteria. This includes bacteria responsible for gastrointestinal, skin and respiratory infections. Methods: The focus of this study was the extraction of essential oils from the aerial portions of Teucrium polium L. via the hydrodistillation method, their anti-oxidant effect using the 2,2-diphenyl-1-picrylhydrazyl (DPPH) free radical scavenging assay method and iron reduction and antimicrobial activity of these essential oils was evaluated against seven ATCC bacterial strains: Staphylococcus aureus ATCC25923, Escherichia coli ATCC25922, Salmonella typhimurium ATCC10428, Pseudomonas aeruginosa ATCC27853, Enterococcus faecalis ATCC29212, Klebsiella pneumoniae ATCC700603 and Bacillus subtilis ATCC7033. In addition, the minimum inhibitory concentrations (MICs) were determined by incorporation method. These tests were carried out at the Laboratoires de the analytical chemistry laboratory at the Department of Pharmacy, Badji Mokhtar University, Annaba, Algeria. Result: The hydro distillation method yielded an essential oil of 0.45%. Antimicrobial activity was tested by the sensitivity test, which revealed inhibition zone diameters ranging from 11.5 mm to £20 mm. In addition, minimum inhibitory concentrations (MICs) were determined, showing variations between bacterial strains, suggesting potential therapeutic importance for some strains. Additionally, the antioxidant activity of the essential oils was assessed using the iron-reducing capacity assay and the DPPH free radical scavenging assay. Although the results indicated notable antioxidant potential, the IC50 values obtained were relatively high when compared to ascorbic acid, registering 107.38 mg/ml for iron reduction and 91.62 mg/ml for DPPH reduction. These findings contribute to the exploration of the therapeutic potential of Teucrium polium L. essential oils for their antimicrobial and antioxidant properties.

A Review of Principles, Applications, and Recent Developments in HPTLC and HPLC

High-Performance Thin Layer Chromatography (HPTLC) and High-Performance Liquid Chromatography (HPLC) represent fundamental analytical techniques in modern chemical analysis. These sophisticated separation methods have revolutionized the field of analytical chemistry through their precision, reliability, and versatility. HPTLC, an enhancement of traditional thin-layer chromatography, offers advantages such as minimal sample preparation, simultaneous analysis of multiple samples, and cost-effectiveness. It has found extensive applications in pharmaceutical analysis, natural product research, and food quality assessment. HPLC, characterized by its high resolution, sensitivity, and automation capabilities, has become an indispensable tool in various industries, including pharmaceutical, environmental, and biochemical analyses. The technique employs different modes such as reverse phase, normal phase, and ion exchange, enabling the separation of complex mixtures with remarkable accuracy. Recent technological advancements have led to the development of ultra-high-performance liquid chromatography (UHPLC), offering enhanced speed and resolution. Both HPTLC and HPLC complement each other in analytical laboratories, with HPTLC providing rapid screening and HPLC offering detailed quantitative analysis. The continuous evolution of these techniques through technological innovations ensures their pivotal role in modern analytical chemistry.

A Review of Liquid Chromatography-Mass Spectrometry and its Applications in Chemical Analysis

Liquid Chromatography-Mass Spectrometry (LC-MS) has emerged as a powerful analytical technique combining the separation capabilities of liquid chromatography with the high sensitivity and selectivity of mass spectrometry. This sophisticated instrumentation enables precise identification and quantification of complex chemical mixtures across diverse fields including pharmaceuticals, environmental monitoring, food safety, and biological research. Modern LC-MS systems offer enhanced resolution, improved ionization methods, and sophisticated mass analyzers that facilitate accurate molecular weight determination and structural elucidation of compounds. Recent technological advancements have led to the development of ultra-high-performance liquid chromatography (UHPLC) systems coupled with high-resolution mass spectrometers, enabling faster analysis times and improved detection limits. The versatility of LC-MS is demonstrated through its applications in proteomics, metabolomics, drug development, and quality control processes. Integration of artificial intelligence and machine learning algorithms has further enhanced data processing capabilities, allowing for automated peak identification and complex mixture analysis. The continuous evolution of LC-MS technology has addressed previous limitations in ionization efficiency, matrix effects, and quantification accuracy. This analytical technique has revolutionized chemical analysis by providing comprehensive molecular information, making it an indispensable tool in modern analytical laboratories.

A prospective evaluation of microscale thermophoresis coupled with mass spectrometry using the “RGB_ex-ante” model

The evaluation of greenness and whiteness is usually made retrospectively (ex-post) – for a developed and validated methodology ready for use. However, it can also be made ex-ante, i.e. taking into account the potential pros and cons that have not yet been experimentally confirmed. The RGB_ex-ante model presented here is a simple assessment framework to help determine whether developing a new specific methodology is worth investing effort. We used it for a prospective evaluation of a new foreseen technique – microscale thermophoresis (MST) coupled online with mass spectrometry (MST-MS). Concurrently, it was demonstrated that biophysical techniques dedicated to the analysis of biomolecular interactions, such as MST, can and should be assessed in terms of greenness and whiteness on an equal footing with chromatography, spectroscopy and other quantitative analysis techniques. We report the original preliminary research results confirming the possibility of combining online MST and MS instruments, which, however, do not yet constitute evidence for analyzing equilibrium processes in this system. For that reason, an ex-ante evaluation was performed. The obtained greenness and whiteness scores suggest that the MST-MS technique would likely be greener than the conventional offline approach, but not whiter. Despite some potential benefits related to all attributes (red, green and blue criteria), the implementation of MST-MS coupling would entail a number of limitations that overall offset the expected merits. The proposed evaluation model turned out to be a simple and helpful tool that is worth using prior developing new methods, procedures and experimental techniques in analytical laboratory and beyond.

Continuous fiber printing of a modular heater for ion mobility spectrometry

Ion mobility spectrometry (IMS) is a powerful analytical method for separating and detecting gaseous substances like volatile organic compounds (VOCs). It is highly versatile, used both as a standalone technique and in combination with chromatographic methods for pre-separation or mass spectrometry for complex matrix analysis. This study explores the use of an advanced 3D printing technology to print a heater for an IMS-device.A continuous fiber printer, commonly used to enhance the mechanical properties of printed objects, was used to create a customized heating element by embedding a copper wire within the polymer matrix during the printing process. Cyclic olefin copolymer (COC) was chosen as the matrix material due to its analytical properties, such as low off-gassing and higher thermal stability, compared to the more commonly used polylactic acid (PLA).The 3D printed heater was incorporated into a drift tube ion mobility spectrometer, and its performance was evaluated by analyzing the separation of various ketones. The results show that the 3D printed heater effectively controlled the temperature within the drift tube, improving the resolving power of overlapping peaks.This study shows the potential of 3D printing technology to improve fabrication and functionality of IMS devices. The flexibility in design and material selection afforded by 3D printing not only enhances the analytical performance of IMS but also allows for customization and rapid prototyping of other analytical instruments or laboratory devices.