Gas Chromatographic Method Research Articles

Amino Acid Profile of Goat Milk Kefir with Lacticasei bacillus casei AP and Oat Milk during Storage

Background: Accurate and up-to-date information about amino acid profile is crucial in the production and promotion of dairy products and fermented milk because both components contribute to the nutritional and market value of the dairy products. Methods: This study aims to evaluate the amino acid profile of goat milk kefir supplemented with Lacticaseibacillus casei AP, oat milk or both during 14-day storage using the gas chromatography method. Result: The results demonstrated that Lacticaseibacillus casei AP and oat milk incorporated into kefir production significantly affected amino acids (aspartac acid, glutamic acid, tyrosine, valin, phenylalanine, ileusin and leucine).The dominant amino acids in the treatments were phenylalanine (46.66 ppm), glutamic acid (40.40 ppm) and lysine (23.91 ppm). The storage time only significantly reduced the amount of valine. Conclusively, incorporating Lacticaseibacillus casei AP, oat milk or both into goat milk kefir did not negatively affect the amino acid profile during storage time.

Solubilization of n-hexadecane by micellar solutions of trehalolipid - surfactants of biological origin

Objectives. To isolate biosurfactants of glycolipid nature produced by oil hydrocarbon degrading bacteria and to establish their ability to solubilize hydrophobic compounds in the case of n-hexadecane.Methods. Trehalolipids were isolated from bacteria Rhodococcus erythropolis X5 (VKM Ac-2532 D) and Rhodococcus erythropolis S67 (VKM Ac-2533 D) included in the MikroBak biopreparation for the bioremediation of oil-contaminated territories. The genome of R. erythropolis X5 is deposited in the National Center for Biotechnology Information database under GenBank accession numbers CP044283 and CP044284, BioSample – SAMN12818508, BioProject – PRJNA573614, and SRA – PRJNA573614. The content of trehalolipid biosurfactants was estimated by the amount of trehalose in aqueous solutions of biosurfactants using the phenolsulfur method. The surface tension of the obtained aqueous solutions of biosurfactants was determined by the du Noüy ring method using a Kruss K6 tensiometer (Kruss, Germany). The critical concentration of micelle formation was determined by the inflection point on the curves of surface tension dependence on the concentration of the biosurfactant solution. In order to establish the solubilizing ability of biosurfactants, the residual concentration of n-hexadecane in an aqueous sample of different concentrations was determined using a gas chromatographic method of analysis.Results. At a constant surface tension of 24.2 mN/m and 25.0 mN/m for R. erythropolis X5 and R. erythropolis S67, respectively, the critical micelle concentration for both strains was 33 mg/L (3.8 ∙ 10−5 mol/L). The solubilizing effect of Rhodococcus trehalolipid micellar solutions against hydrophobic n-hexadecane was demonstrated by gas chromatographic analysis. The solubilization process was characterized using molar solubilization capacity (Sm), molar solubilization ratio (MSR), micelle–water partition coefficient (Km), and solubilization energy 0 (ΔGS ). It was shown that the solubilization process of n-hexadecane proceeds spontaneously 0 (ΔGS = −35.5 kJ/mol) and more efficiently (Sm = 4.3 mol/mol, MSR = 4.7 mol/mol) than in comparison with other biosurfactants of glycolipid nature.Conclusions. Based on the value of the molar solubilization coefficient, it can be concluded that trehalolipids of the R. erythropolis X5 strain solubilize n-hexadecane in aqueous solutions to a greater extent than compared to other biosurfactants of a glycolipid nature, but are inferior to synthetic surfactants.

Trace-level quantification of NDMA in levosulpuride active pharmaceutical ingredient and tablet formulation Using UFLC-MS/MS

Nitrosamine impurities identified in several pharmaceuticals during recent times has raised concerns leading to product recalls worldwide and necessitating sensitive liquid and gas chromatographic methods for trace level detection of nitrosamine impurities. This study developed and validated a ultra-fast liquid chromatography-tandem mass spectrometry (UFLC-MS/MS) method for the quantification of NDMA in Levosulpuride drug substance and tablet formulation. Current method utilizes a triple quadrupole analyzer, atmospheric pressure chemical ionization (APCI) ionization source and multiple reaction monitoring (MRM) scan mode for the analysis. Chromatographic separation was achieved on a Gemini NX-C18 column (150 × 4.6 mm, 3 µm) maintained at 40 °C. The mobile phase consisted of a binary gradient of solvent A (0.1 % formic acid in water) and solvent B (methanol), with a total run time of 18 minutes. Current method achieved excellent linearity, recovery, precision, and sensitivity. Greenness of the developed method was evaluated using the GAPI, AGREE, and AES metrics. Current method is sensitive and selective for NDMA in levosulpuride drug substance and tablet formulations and can be employed for routine quality control analysis in pharmaceutical industry.

Development and Validation of a Gas Chromatography Method for Quantifying Metham Sodium in Diverse Plant Origin Foods

Development and Validation of a Gas Chromatography Method for Quantifying Metham Sodium in Diverse Plant Origin Foods

Fluxes of carbon dioxide gases (CO2) in the mangrove soil of Passo Village, Ambon City

Mangrove ecosystems play a significant role in carbon absorption. However, the accumulation of organic matter in mangrove sediments undergoes decomposition, which triggers the release of CO2 gas flux. This study aimed to analyze the CO2 gas flux in mangrove sediments of Negeri Passo, Ambon City. Gas data collection was performed using cylinder canopies at the three observation stations. Gas was passed through the syringe five times with an interval of 30s. Gas concentration analysis was carried out using the gas chromatography method, while CO2 flux was analyzed with flux equations referring to slope regression, volume and area of the scope, temperature, molecular weight of the gas, ideal gas settings, and time constants based on gas intake intervals. The results showed that the average CO2 concentration in St. 1 was 465.14 ± 96.52 ppm, and was the lowest compared to St. 2 and St. 3 with values of 638.60 ± 90.05 ppm and 630.98 ± 54.09 ppm, respectively. Meanwhile, the average CO2 flux was 50.44 mg/m2/hour. The largest CO2 gas flux was observed at St. 2 at 103.69 mg/m2/hour. Meanwhile, the lowest flux was found at St. 3, which was 16.24 mg/m2/hour. Based on this, it can be concluded that] the mangrove ecosystem in Negeri Passo has a higher concentration of CO2 gas than the average concentration of climate change stabilization scenarios. However, the CO2 flux was lower than that at other locations in the Ambon Dalam Bay area. In addition, the potential for significant carbon sequestration based on the Tier 1 model approach indicated that mangrove ecosystems in this location play an important role in climate change mitigation.

Fermented By-Products of Banana Wine Production Improve Slaughter Performance, Meat Quality, and Flavor Fingerprint of Domestic Chicken.

This study aimed to compare the effects of incorporating fermented feed into daily diets on the slaughter performance, meat quality, and flavor compounds of 120 domestic chickens over a 140-day period. A total of five groups (n = 24), including the control group (CK) of the Guangxi Partridge chickens received a standard base diet. The other four groups were provided with pellets that had been added with 10% fermented banana peel (Pe-10), 20% fermented banana peel (Pe-20), 10% fermented banana pulp residue (Pu-10), and 20% fermented banana pulp residue (Pu-20). The flavor compounds in the meat samples of the chickens in these groups were determined using the gas chromatographic method. The results demonstrated that the chickens in the Pe-10, Pe-20, Pu-10, and Pu-20 groups exhibited pectoral muscle percentages, thigh muscle percentages, and total fatty acid content of chest meat that were higher than those observed in the CK group. The moisture content, meat color, carcass weight, total net weight, and abdominal fat percentage of the meat samples in these experimental groups exhibited no notable differences. The flavor compounds in the meat samples of the chickens fed with the two concentrations of fermented banana peel and banana residue were found to be significantly different from those in the control group, with p-values less than 0.05. As the quantity of fermented banana peel incorporated into the daily ration was increased from 10% to 20%, a notable alteration in the flavor compounds present in the chicken samples was observed. The chickens that were provided with fermented banana peels and pulps in their diets exhibited superior slaughter performance and meat quality, particularly in the case of the Pu-10 group, in comparison to the control chickens.

End Column Reverse Chromatography as a Novel Approach for Enhanced Separation: A Pilot Study.

Currently, the most popular technique in gas chromatography (GC) is the "temperature programming", where the temperature increases from the start of the injection. This leads to faster elution of analytes compared to isothermal methods. However, isothermal methods are considered optimal for separating compounds with similar retention times. Another interesting technique that provides higher resolution is the dynamic thermal gradient gas chromatography (TGGC), where separations are achieved as a decreasing thermal gradient. This gradually decreases the positive gas velocity. Nevertheless, it was proven that GC techniques with negative velocity gradients don't improve the resolution of compounds with nearly identical retention times. Optimizing a new GC approach to combine both the short time from positive temperature ramps programming, and the enhanced separation of the negative ramps of the TGGC, a model under the name of "end column reverse chromatography". The process simply consists of two steps, the first is a normal positive ramp from the start of the injection, the second step is a negative thermal ramp at a time that is around the retention time of the first eluting peak. This will decrease the solute velocity almost solely for the second compound leading to relatively enhanced separation. Optimized ECRC method increased the resolution of two isomers (trans and cis chlordane) from 1 (slightly overlapping) in case of temperature programming to 2.78 as shown in this study. This comes in expense of the width and intensity of the peaks, where the intensity decreased about 17% and 12% for cis and trans chlordane, and the peak width increased with 37% and 77% for the same compounds respectively. ECRC is a novel model for enhanced separation that comes with some drawbacks. It can be an alternative approach to get a fast GC method with enhanced separation for isomers.

Reference Material for the Composition of Fuel Oil

Electrical transformers are a key element in the process of distributing electricity from the producer to the final consumer. The reliability of electrical transformers is ensured through systematic monitoring of the structural condition using chemical analysis of fuel (transformer) oil used for electrical insulation and cooling of transformers. The working life of energy oil and paper insulation can be assessed by evaluating the content of antioxidant additive (ionol) and furan derivatives (furfuryl alcohol, furfural, 2-acetylfuran and 5-methylfurfural). The article provides a critical analysis of methods for measuring ionol and furan derivatives in oils. In particular, it has been established that the most widely used methods for the identification of ionol and furan derivatives are liquid and gas chromatography methods with preliminary isolation of analytes based on the principles of liquid/solid-phase extraction. At the same time, the need for matrix reference materials with established metrological traceability was identified for metrological support of methods for measuring the content of ionol and furan derivatives in oils. Therefore, the purpose of this study was the development of a certified reference material (CRM) for the composition of fuel oil. The technology for producing such a CRM makes it possible to prepare the material with the required concentrations of analytes. The article describes the sequence of preparation of a CRM batch and presents the conclusions of studying the stability and between-bottle homogeneity of the material. The given calculation of the standard uncertainty for the certified value of the CRM from the characterization method, heterogeneity, and instability of the material in accordance with GOST ISO Guide 35–2015 deserves attention. The metrological traceability of certified values of the CRM to the unit of value «mass fraction of a component» reproduced by the State Primary Standard of units of mass (molar) fraction and mass (molar) concentration of organic components in liquid and solid substances and materials based on liquid and gas chromatography-mass spectrometry with isotope dilution and gravimetry (GET 208–2019). The competence of the study is confirmed by the fact that the CRM was recognized as GSO 12232–2023.

Oxidation of Geraniol on Vermiculite—The Influence of Selected Parameters on the Oxidation Process

Geraniol is a compound belonging to the group of monoterpenes that finds many applications in organic syntheses, medicine and cosmetics. The following properties of geraniol and its derivatives are of particular interest in medicine: its anti-inflammatory, antioxidant, antimicrobial and anticancer effects. The geraniol oxidation process was carried out using a mineral of natural origin—vermiculite. Vermiculite is a catalyst that perfectly fits into modern trends in the organic industry, where the aim is to use cheap, renewable and relatively easily available catalytic materials (vermiculite is found on continents including Africa, North America, South America, Australia and Asia). Preliminary studies on the oxidation process of geraniol on vermiculite was carried out in a glass apparatus using molecular oxygen supplied by means of a bubbler and magnetic stirrer with a heating function. During the oxidation process of geraniol on vermiculite, the influence of the following parameters was examined: the temperature, amount of catalyst and reaction time. The main parameters of the process, on the basis of which the most favorable process conditions were selected, were the selectivity of the transformation to 2,3-epoxygeraniol, citral and 2,3-epoxycitral, and the conversion of geraniol. The composition of the post-reaction mixtures was determined qualitatively and quantitatively using the gas chromatography method. In addition, vermiculite was subjected to instrumental tests, such as XRD, SEM, EDX, FTIR and UV-VIS. Moreover, the specific surface area, pore volume and pore volume distribution were estimated on the basis of N2 sorption at −196 °C and also the acid-site concentration in vermiculite was established.

Application of straw-derived biochar: a sustainable approach to improve soil quality and crop yield and reduce N2O emissions in paddy soil.

The burning of agricultural straw is a pressing environmental issue, and identifying effective strategies for the rational utilization of straw resources is decisive for achieving sustainable development. Owing to its high carbon content and exceptional stability, straw biochar produced via pyrolysis has emerged as a key focus in multidisciplinary research. However, the efficacy of biochar in mitigating nitrous oxide (N2O) emissions from paddy soils is not consistent. A 2-year field experiment was conducted and investigated the impact of biochar derived from two feedstocks (rice straw and wheat straw, pyrolyzed at 450°C) on N2O emissions, global warming potential (GWP), greenhouse gas intensity (GHGI), nitrogen use efficiency (NUE), crop yield, and soil quality. The static chamber technique was used for collecting N2O gas samples, and concentrations were analyzed through gas chromatography methods. The treatment combinations included BR0 (control), BR1 (NPK at the recommended dose, 120:60:40kgha-1), BR2 (wheat straw biochar, 5 t ha-1), and BR3 (rice straw biochar, 5 t ha-1). The results exhibited that cumulative N2O emissions from BR2 and BR3 treatments decreased by 10.55% and 13.75% respectively, compared to BR1. Lower GWP and GHGI were observed under both biochar treatments compared with BR1. The highest rice grain yield (3.48Mgha-1) and NUE (76.72%) were recorded from BR3, which also exhibitedthe lowest yield-scaled N2O emission. We observed positive correlations between soil nitrate, ammonia and water-filled pore spaces, while NUE showed negative correlations with N2O emissions. Significant (p < 0.05) improvements in soil quality were also detected in both the biochar treated plots, indicated by increased soil pH, water holding capacity, porosity, and nutrient contents. Overall, the results suggest that applying biochar at a rate of 5 t ha-1 in paddy soil is a viable nutrient management strategy with the potential to reduce reliance on inorganic fertilizers, mitigate N2O emissions, and contribute to sustainable food production.

Inter-laboratory study for extraction testing of medical devices

Biocompatibility evaluation of medical devices often relies on chemical testing according to ISO 10993–18 as a critical component for consideration. However, the precision associated with these non–targeted chemical characterization assessments has not been well established. Therefore, we have conducted a study to characterize intra–laboratory (repeatability) and inter–laboratory (reproducibility) variability associated with chemical testing of extractables from polymeric materials. To accomplish this, this study focused on two polymers, each with nine chemicals that were intentionally compounded into the materials. Eight different laboratories performed extraction testing in two solvents and subsequently characterized the extracts using gas chromatography and liquid chromatography methods. Analysis of the resulting data revealed the central 90 % range for the repeatability and reproducibility relative standard deviations are (0.09, 0.22) and (0.30, 0.85), respectively, for the participating laboratory methods. This finding implies that if the same sample was tested by two different laboratories using the same extraction conditions, there is 95 % confidence for 95 % of systems that the test results could exhibit differences up to 240 %. While the study was not designed to evaluate the relative impact of specific underlying factors that may contribute to variability in quantitation, the data obtained suggest the variability associated with analytical method alone is a substantial contribution to the overall variability. The relatively large reproducibility limits we observed may have significant implications where variability in extraction measurements can impact aspects of biocompatibility risk evaluation, such as exposure dose estimation and chemical equivalence assessments.

Greenhouse Gas Emissions Characteristics and Driving Factors Analysis in the Eutrophic Saline Lake Daihai Lake

To investigate the greenhouse gas emission characteristics and driving factors of eutrophic saline lakes in northern China, considering Daihai Lake in Inner Mongolia as an example, 10 monitoring sites were selected based on hydrological distribution characteristics in April, July, and October 2023. Using headspace gas chromatography and modeling methods, dissolved concentrations and exchange fluxes of carbon dioxide （CO2）, methane （CH4）, and nitrous oxide （N2O） were determined in the nearshore zone, open lake area, and lake center surface water. During the study period, Daihai Lake exhibited significant seasonal variations in greenhouse gas concentration and flux. The average concentrations of CO2, CH4, and N2O in surface water were （26.52 ± 17.58） μmol·L-1, （282.30 ± 172.30） nmol·L-1, and （9.09 ± 1.64） nmol·L-1, respectively. The average fluxes were （5.29 ± 11.98） mmol·（m2·d）-1, （178.24 ± 63.34） μmol·（m2·d）-1, and （-0.74 ± 1.28） μmol·（m2·d）-1, with cumulative emissions of 50 770.77, 543.52, -4.21 kg·km-2 and a global warming potential （expressed in CO2-equivalent） of 50 770.77, 15 218.49, -1 254.48 kg·km-2. Daihai Lake acted as a source of atmospheric CO2 and CH4 but a sink for N2O during the study period. Correlation and stepwise regression analyses revealed that pH and total dissolved solids （TDS） influenced CO2 concentration and flux, while the factors affecting CH4 were water temperature （WT）, water depth （WD）, wind speed （WS）, oxidation-reduction potential （ORP）, and total nitrogen （TN）. For N2O, the influencing factors were WT, WS, and TN. Additionally, Daihai Lake's eutrophication and salinity characteristics influenced the generation and emission of greenhouse gases. This study provides insights into the greenhouse gas dynamics and environmental factors in eutrophic saline lakes like Daihai Lake.

Modern problems of Ukraine's ecology: agricultural pollutants and the quality of drinking water in the city of Kyiv

Considered modern problems of Ukraine's ecology. The problem “influence of agriculture on the quality of underground water” is considered in detaile. In 1998-2002, 163 analyzes of underground waters of the aquifer of Cenomanian sediments and the aquifer of Jurassic sediments in the city of Kyiv for the content of persistent chlorine-organic pesticides: DDT and its metabolites, hexachlorocyclohexane (HCCH) and its isomers, aldrin, heptachlor and the fluor-containing pesticide treflane were carried out by the gas-chromatographic method. In the water of the aquifer of Cenomanian sediments and the aquifer of Jurassic sediments of the city of Kyiv, the average concentration of DDT was at the level of 10-5 mg/dm3. According to our calculations for the year 2024, the concentration of the amount of DDT in the drinking groundwater of the city of Kyiv has decreased by 2-3 orders of magnitude, depending on natural conditions. This indicates that there no new inputs of DDT to natural ecosystems, and retrospective contamination is gradually decreasing. The need to conduct fundamental research of establishing concentrations of new pesticides in groundwater, developing criteria for assessing the danger of co-presence of pesticides of various classes of chemical compounds in groundwater and other natural objects remains relevant. In 2023-2024, 58 wells were examined for the quality of drinking water in Kyiv.

Development of a Low-Temperature Purification Method for Gas Chromatography–Mass Spectrometry Quantification of Three Cresol Isomers in Smoked Bacon

Development of a Low-Temperature Purification Method for Gas Chromatography–Mass Spectrometry Quantification of Three Cresol Isomers in Smoked Bacon

Simultaneous multianalyte trace-level quantification of eight genotoxic nitrosamine impurities in valsartan Active Pharmaceutical Ingredient and tablet formulation using UFLC-MS/MS and greenness assessment

Valsartan, a widely prescribed antihypertensive drug, was identified for the presence of carcinogenic nitrosamine impurities in 2018, leading to product recalls worldwide and necessitating sensitive liquid and gas chromatographic methods for trace level detection of nitrosamine impurities. This study developed and validated an ultra-fast liquid chromatography-tandem mass spectrometry (UFLC-MS/MS) method for the quantification of eight genotoxic nitrosamines (NDMA, NDEA, NDPA, NEIPA, NDIPA, NMBA, NDBA, and NMPA) in valsartan drug substance and tablet formulations. The method employed a triple quadrupole analyzer, atmospheric pressure chemical ionization (APCI) ionization source and multiple reaction monitoring (MRM) scan mode for the analysis. Chromatographic separation was achieved on a Phenomenex biphenyl column (150 × 4.6 mm, 3 µm) maintained at 55 °C. The mobile phase consisted of a binary gradient of solvent A (0.1 % formic acid in water) and solvent B (0.1 % formic acid in methanol), with a total run time of 20 min for the sensitive and specific detection of the analytes. Method validation demonstrated excellent linearity, recovery, precision, and sensitivity. The greenness of the developed analytical method was critically assessed through comprehensive evaluations using the GAPI, AGREE, and AES metrics and the results obtained are compared with the reported methods in the literature. This novel UFLC-MS/MS method offers a reliable and sensitive approach for routine quality control analysis of nitrosamine impurities in Valsartan drug substance and tablet formulations.

Analysis of Intact In Vivo Peroxidized Phospholipids from Bovine Retina via LC-MS/MS and GC-MS/MS Using Autoxidized Retina Reference Standards.

Highly unsaturated fatty acids (HUFAs) are vulnerable to oxygen attack, thus making HUFA-rich, high metabolic rate/reactive oxygen species (ROS)-generating neurological tissue particularly susceptible to increased oxidative stress. Lipid oxidation is a putative early stage marker of neurodegenerative diseases, suggesting that reliable monitoring of oxidized neural lipids in vivo reveals early pathogenesis. Here, we present a novel methodology to detect and quantify intactin vivo ROS-driven peroxidized phospholipids (LPOx-PLs) in bovine retina extract. A protocol for preparing autoxidized pure phospholipids (PLs) and complex retinal extracts served as reference standards and was adapted to enable analytical parameter development. Fatty acid profiles of bovine retinas were first established with routine gas chromatography (GC) methods and used to customize mass spectrometry scanning for major HUFA-carrying PLs in the retinal extract. Targeted multiple reaction monitoring (MRM) scanning via triple quadrupole tandem mass spectrometry detected native (unoxidized) and oxidation-damaged PL regardless of the position of the O or O2 addition along the acyl chains and enabled quantification of relative signals from intact native and oxidized PL (5%-10% CV). MRM-triggered information-dependent acquisition (IDA) spectra confirmed the structure of peroxidized PLs, revealing that peroxidized species (+O-OH) dominated over single O-added species in vitro and in vivo. Positive identification and relative quantification are reported for 12 selected in vivo native and peroxidized phosphatidylcholines and phosphatidylethanolamines. These results enable future studies of the initial peroxidation due to toxins, genetics, or other initiating events influencing in vivo oxidation levels and potentially the effectiveness of strategies to mitigate this mechanism of action.

Controlling Methane Ebullition Flux in Cascade Reservoirs of the Upper Yellow River by the Ratio of mcrA to pmoA Genes

Reservoirs are an important source of methane (CH4) emissions, but the relative contribution of CH4 ebullition and diffusion fluxes to total fluxes has received little attention in the past. In this study, we systematically monitored the CH4 fluxes of nine cascade reservoirs (Dahejia, Jishixia, Huangfeng, Suzhi, Kangyang, Zhiganglaka, Lijiaxia, Nina, and Longyangxia) in the upper reaches of the Yellow River in the dry (May 2023) and wet seasons (August 2023) using the static chamber gas chromatography and headspace equilibrium methods. We also simultaneously measured environmental physicochemical properties as well as the abundance of methanogens and methanotrophs in sediments. The results showed the following: (1) All reservoirs were sources of CH4 emissions, with an average diffusion flux of 0.08 ± 0.05 mg m−2 h−1 and ebullition flux of 0.38 ± 0.41 mg m−2 h−1. Ebullition flux accounted for 78.01 ± 7.85% of total flux. (2) Spatially, both CH4 diffusion and ebullition fluxes increased from upstream to downstream. Temporally, CH4 diffusion flux in the wet season (0.09 ± 0.06 mg m−2 h−1) was slightly higher than that in the dry season (0.08 ± 0.04 mg m−2 h−1), but CH4 ebullition flux in the dry season (0.38 ± 0.48 mg m−2 h−1) was higher than that in the wet season (0.32 ± 0.2 mg m−2 h−1). (3) qPCR showed that methanogens (mcrA gene) were more abundant in the wet season (5.43 ± 3.94 × 105 copies g−1) than that in the dry season (3.74 ± 1.34 × 105 copies g−1). Methanotrophs (pmoA gene) also showed a similar trend with more abundance found in the wet season (7 ± 2.61 × 105 copies g−1) than in the dry season (1.47 ± 0.92 × 105 copies g−1. (4) Structural equation modeling revealed that the ratio of mcrA/pmoA genes, water N/P, and reservoir age were key factors affecting CH4 ebullition flux. Variation partitioning further indicated that the ratio of mcrA/pmoA genes was the main factor causing the spatial variation in CH4 ebullition flux, explaining 35.69% of its variation. This study not only reveals the characteristics and influencing factors of CH4 emissions from cascade reservoirs on the Qinghai Plateau but also provides a scientific basis for calculating fluxes and developing global CH4 reduction strategies for reservoirs.

Method of Gas Chromatography–Mass Spectrometry for the Determination of Free Bisphenol A in Ethanol Extracts

Method of Gas Chromatography–Mass Spectrometry for the Determination of Free Bisphenol A in Ethanol Extracts

Development and validation of a gas chromatography method for analysing polychlorinated biphenyls in fish roe

A method for determining polychlorinated biphenyls (PCBs) in fish roe by gas chromatography (GC) has been developed. The suitability (validation) of the process for the determination of 14 PCBs (PCB 18, PCB 31, PCB 28, PCB 52, PCB 44, PCB 101, PCB 149, PCB 118, PCB 153, PCB 138, PCB 180, PCB 170, PCB 194, PCB 209) in fish roe by GC using an electron capture detector (ECD) was evaluated according to the following criteria: selectivity, linearity, limits of detection (LOD), limits of quantification (LOQ), accuracy and precision. Automated Soxhlet extraction and sample clean-up by solid phase extraction (SPE) were proposed for extracting PCBs from fish roe. The results of the method selectivity study showed that the determination of PCBs in fish roe is not affected by other components in the sample. The correlation coefficients for fourteen PCBs ranged from 0.9962 to 0.9999 (R2 ≥0.995). The limits of detection (LOD) and limits of quantification (LOQ) of PCBs are below the maximum permissible levels set by the European Union (EU). The recovery percentage ranged from 81.5% to 107%, indicating the PCB extraction procedure's acceptability (R, 80 – 120%). The relative standard deviation (RSD, %) of the measurement results under convergence conditions ranged from 1.02% to 9.43% (RSD ≥15%). The obtained method suitability (validation) data meets the Commission Regulation (EU) No 589/2014 criteria.

The use of liquid and gas chromatography in combination with mass spectroscopy and the method of capillary electrophoresis to study hydroxycinnamic acids in plants growing in Russia

BACKGROUND: Recently, the volume of research and publications devoted to the study of the class of phenylpropanoids in plants, in particular, hydroxycinnamic acids and their derivatives, has been steadily growing. This is due to the diverse range of their pharmacological activity and the possibility of using them in medicine. The reliability and reliability of identification of this group of compounds is significantly expanding with the improvement of analytical methods: gas and liquid chromatography in combination with mass spectroscopy, as well as the use of capillary electrophoresis. The study of the proposed approaches to the analysis of this group of compounds can be interpolated to new plant objects. AIM: A comparative analysis of the use of liquid and gas chromatography methods in combination with mass spectroscopy, as well as the capillary electrophoresis method for the study of hydroxycinnamic acids in plants growing and cultivated in the Russian Federation. MATERIALS AND METHODS: Results published in domestic periodical scientific journals and conference proceedings, based on information and analytical studies. RESULTS: Data on the study of the conditions of extraction, structure and content of hydroxycinnamic acids and their derivatives in plants growing on the territory of the Russian Federation have been systematized. The review presents the advantages and limitations of gas and liquid chromatography in combination with the method of mass spectroscopy in the analysis of this group of compounds, using various conditions for their extraction from plant materials. The prospects of using the capillary electrophoresis method for these purposes are shown due to the ease of implementation and highly efficient separation of hydroxycinnamic acids and their derivatives in plant materials. It has been established that there is a lack of information on studying the dynamics of their accumulation depending on climate-forming factors, regions of growth, as well as their stability in plant materials. CONCLUSION: analysis of the methods presented in the review allows us to create a methodological basis for further improvement and development of new methods for the analysis of hydroxycinnamic acids and their derivatives in plant objects.