Displaying publications 1 - 20 of 137 in total

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  1. Fulltext Ultrasound-assisted sequentially precipitated nickel-silica catalysts and its application in the partial hydrogenation of edible oil
    Lim MSW, Yang TC, Tiong TJ, Pan GT, Chong S, Yap YH
    Ultrason Sonochem, 2021 May;73:105490.
    PMID: 33609992 DOI: 10.1016/j.ultsonch.2021.105490
    Sequentially precipitated Mg-promoted nickel-silica catalysts with ageing performed under various ultrasonic intensities were employed to study the catalyst performance in the partial hydrogenation of sunflower oil. Results from various characterisation studies showed that increasing ultrasonic intensity caused a higher degree of hydroxycarbonate erosion and suppressed the formation of Ni silicates and silica support, which improved Ni dispersion, BET surface area and catalyst reducibility. Growth of silica clusters on the catalyst aggregates were observed in the absence of ultrasonication, which explained the higher silica and nickel silicate content on the outer surface of the catalyst particle. Application of ultrasound also altered the electron density of the Ni species, which led to higher activity and enhanced product selectivity for sonicated catalysts. The catalyst synthesised with ultrasonic intensity of 20.78 Wcm-2 achieved 22.6% increase in hydrogenation activity, along with 28.5% decrease in trans-C18:1 yield at IV = 70, thus supporting the feasibility of such technique.
    Matched MeSH terms: Chromatography, Gas
  2. A brief period of darkness induces changes in fatty acid biosynthesis towards accumulation of saturated fatty acids in Chlorella vulgaris UMT-M1 at stationary growth phase
    Cha TS, Yee W, Phua PSP, Loh SH, Aziz A
    Biotechnol Lett, 2021 Apr;43(4):803-812.
    PMID: 33438120 DOI: 10.1007/s10529-021-03077-2
    OBJECTIVE: The effects of a brief (3 days) and prolonged (6 days) period of incubation in darkness and light on the biomass content, lipid content and fatty acid profile in Chlorella vulgaris UMT-M1 were determined.

    RESULTS: Three days of incubation in darkness increased saturated fatty acid (SFA) content from 34.0 to 41.4% but decreased monounsaturated fatty acid (MUFA) content from 36.7 to 29.8%. Palmitic acid (C16:0) content was increased from 23.2 to 28.9%, whereas oleic acid (C18:1) content was reduced from 35.4 to 28.8%. Total oil content was slightly decreased from 20.4 to 18.7% after 3 days of darkness, without a significant reduction in biomass compared to 3 days of incubation in light. Biomass and oil content was highest in cultures incubated for 6 days in light, however the stimulatory and inhibitory effects of darkness (or light) on SFA and MUFA content was no longer present at 6 days of incubation.

    CONCLUSIONS: Findings from this study suggests that fatty acid composition in C. vulgaris could be modulated to favor either C16:0 or C18:1 by a brief period of either darkness or light incubation, prior to harvesting.

    Matched MeSH terms: Chromatography, Gas
  3. Fulltext Electrodeposited Hybrid Biocathode-Based CO2 Reduction via Microbial Electro-Catalysis to Biofuels
    Anwer AH, Khan N, Umar MF, Rafatullah M, Khan MZ
    Membranes (Basel), 2021 Mar 22;11(3).
    PMID: 33810075 DOI: 10.3390/membranes11030223
    Microbial electrosynthesis is a new approach to converting C1 carbon (CO2) to more complex carbon-based products. In the present study, CO2, a potential greenhouse gas, was used as a sole carbon source and reduced to value-added chemicals (acetate, ethanol) with the help of bioelectrochemical reduction in microbial electrosynthesis systems (MES). The performance of MES was studied with varying electrode materials (carbon felt, stainless steel, and cobalt electrodeposited carbon felt). The MES performance was assessed in terms of acetic acid and ethanol production with the help of gas chromatography (GC). The electrochemical characterization of the system was analyzed with chronoamperometry and cyclic voltammetry. The study revealed that the MES operated with hybrid cobalt electrodeposited carbon felt electrode yielded the highest acetic acid (4.4 g/L) concentration followed by carbon felt/stainless steel (3.7 g/L), plain carbon felt (2.2 g/L), and stainless steel (1.87 g/L). The alcohol concentration was also observed to be highest for the hybrid electrode (carbon felt/stainless steel/cobalt oxide is 0.352 g/L) as compared to the bare electrodes (carbon felt is 0.22 g/L) tested, which was found to be in correspondence with the pH changes in the system. Electrochemical analysis revealed improved electrotrophy in the hybrid electrode, as confirmed by the increased redox current for the hybrid electrode as compared to plain electrodes. Cyclic voltammetry analysis also confirmed the role of the biocatalyst developed on the electrode in CO2 sequestration.
    Matched MeSH terms: Chromatography, Gas
  4. A review of gas chromatographic techniques for identification of aqueous amine degradation products in carbonated environments
    Saeed IM, Mazari SA, Alaba P, Ali BS, Jan BM, Basirun WJ, et al.
    Environ Sci Pollut Res Int, 2021 Feb;28(6):6324-6348.
    PMID: 33398750 DOI: 10.1007/s11356-020-11753-5
    Degradation of amines is a significant issue allied to amine-based carbon dioxide (CO2) absorption in post-combustion CO2 capture. It becomes essential to have a detailed understanding of degradation products for advanced post-combustion CO2 capture technology. Identification and quantification of degradation products of amines help in practicability and environmental assessment of amine-based technology. Gas, liquid, and ion chromatographic techniques are the benchmark tools for qualitative and quantitative analyses of the amines and their derivatives. Among others, gas chromatography has been more in use for this specific application, especially for the identification of degradation products of amines. This review focuses on the critical elucidation of gas chromatographic analysis and development of methods to determine the amine degradation products, highlighting preparation methods for samples and selecting columns and detectors. The choice of detector, column, sample preparation, and method development are reviewed in this manuscript, keeping in view the industry and research applications. Furthermore, obtained results on the quantitative and qualitative analyses using gas chromatography are summarized with future perspectives.
    Matched MeSH terms: Chromatography, Gas
  5. Analytical GC-FID Method for the Determination of Organic Solvents in Radiopharmaceuticals
    Hassan H, Othman MF, Zakaria ZA, Saad FFA, Abdul Razak HR
    Curr Radiopharm, 2021;14(2):131-144.
    PMID: 33115398 DOI: 10.2174/1874471013999201027215704
    BACKGROUND: Organic solvents play an indispensable role in most of the radiopharmaceutical production stages. It is almost impossible to remove them entirely in the final formulation of the product.

    OBJECTIVE: In this presented work, an analytical method by gas chromatography coupled with flame ionization detection (GC-FID) has been developed to determine organic solvents in radiopharmaceutical samples. The effect of injection holding time, temperature variation in the injection port, and the column temperature on the analysis time and resolution (R ≥ 1.5) of ethanol and acetonitrile was studied extensively.

    METHODS: The experimental conditions were optimized with the aid of further statistical analysis; thence, the proposed method was validated following the International Council for Harmonisation (ICH) Q2 (R1) guideline.

    RESULTS: The proposed analytical method surpassed the acceptance criteria including the linearity > 0.990 (correlation coefficient of R2), precision < 2%, LOD, and LOQ, accuracy > 90% for all solvents. The separation between ethanol and acetonitrile was acceptable with a resolution R > 1.5. Further statistical analysis of Oneway ANOVA revealed that the increment in injection holding time and variation of temperature at the injection port did not significantly affect the analysis time. Nevertheless, the variation in injection port temperature substantially influenced the resolution of ethanol and acetonitrile peaks (p < 0.05).

    CONCLUSION: The proposed analytical method has been successfully implemented to determine the organic solvent in the [18F]fluoro-ethyl-tyrosine ([18F]FET), [18F]fluoromisonidazole ([18F]FMISO), and [18F]fluorothymidine ([18F]FLT).

    Matched MeSH terms: Chromatography, Gas/methods*
  6. Fulltext Surface Thermo-Dynamic Characterization of Poly (Vinylidene Chloride-Co-Acrylonitrile) (P(VDC-co-AN)) Using Inverse-Gas Chromatography and Investigation of Visual Traits Using Computer Vision Image Processing Algorithms
    Kakani V, Kim H, Basivi PK, Pasupuleti VR
    Polymers (Basel), 2020 Jul 23;12(8).
    PMID: 32717780 DOI: 10.3390/polym12081631
    The Inverse Gas Chromatography (IGC) technique has been employed for the surface thermo-dynamic characterization of the polymer Poly(vinylidene chloride-co-acrylonitrile) (P(VDC-co-AN)) in its pure form. IGC attributes, such as London dispersive surface energy, Gibbs free energy, and Guttman Lewis acid-base parameters were analyzed for the polymer (P(VDC-co-AN)). The London dispersive surface free energy ( γ S L ) was calculated using the Schultz and Dorris-Gray method. The maximum surface energy value of (P(VDC-co-AN )) is found to be 29.93 mJ·m - 2 and 24.15 mJ·m - 2 in both methods respectively. In our analysis, it is observed that the γ S L values decline linearly with an increase in temperature. The Guttman-Lewis acid-base parameter K a , K b values were estimated to be 0.13 and 0.49. Additionally, the surface character S value and the correlation coefficient were estimated to be 3.77 and 0.98 respectively. After the thermo-dynamic surface characterization, the (P(VDC-co-AN)) polymer overall surface character is found to be basic. The substantial results revealed that the (P(VDC-co-AN)) polymer surface contains more basic sites than acidic sites and, hence, can closely associate in acidic media. Additionally, visual traits of the polymer (P(VDC-co-AN)) were investigated by employing Computer Vision and Image Processing (CVIP) techniques on Scanning Electron Microscopy (SEM) images captured at resolutions ×50, ×200 and ×500. Several visual traits, such as intricate patterns, surface morphology, texture/roughness, particle area distribution ( D A ), directionality ( D P ), mean average particle area ( μ a v g ) and mean average particle standard deviation ( σ a v g ), were investigated on the polymer's purest form. This collective study facilitates the researches to explore the pure form of the polymer Poly(vinylidene chloride-co-acrylonitrile) (P(VDC-co-AN )) in both chemical and visual perspective.
    Matched MeSH terms: Chromatography, Gas
  7. Poly(cyclodextrin-ionic liquid) based ferrofluid: A new class of magnetic colloid for dispersive liquid phase microextraction of polycyclic aromatic hydrocarbons from food samples prior to GC-FID analysis
    Yih Hui B, Mohamad Zain NN, Mohamad S, Varanusupakul P, Osman H, Raoov M
    Food Chem, 2020 Jun 01;314:126214.
    PMID: 31972404 DOI: 10.1016/j.foodchem.2020.126214
    Poly(β-cyclodextrin-ionic liquid) grafted magnetic nanoparticles combined with 1-octanol as supramolecular solvents (SUPRASs) presenting new ferrofluid was developed and successfully applied in the dispersive liquid-phase microextraction of seven representative polycyclic aromatic hydrocarbons. One variable at-a-time (OVAT) analysis and response surface methodology (RSM) were used for efficient optimization of the main variables. The calibration curves were found to be linear in the range of 0.1-150 ng mL-1 with correlation of determinations (R2) ranging from 0.9944 to 0.9986. Detection limits ranged at 0.02-0.07 ng mL-1 for all studied PAHs. The intra and inter-day precision values (RSD %) were in the range of 1.80%-7.56% and 2.97%-8.23%, respectively. The ferrofluid showed a satisfactory reproducibility between 1.72% and 5.90%, and acceptable recovery values at 84%-110% were obtained for the real samples analysis. The optimized method was successfully applied to access the content safety of the PAHs studied in a variety of commercial food and beverages available in Malaysia.
    Matched MeSH terms: Chromatography, Gas
  8. Fulltext Surface Energy Mapping of Modified Silica Using IGC Technique at Finite Dilution
    Ngeow YW, Williams DR, Chapman AV, Heng JYY
    ACS Omega, 2020 May 12;5(18):10266-10275.
    PMID: 32426583 DOI: 10.1021/acsomega.9b03920
    The reinforcing silica filler, which can be more than 40% of an elastomer composite, plays a key role to achieve the desired mechanical properties in elastomer vulcanizates. However, the highly hydrophilic nature of silica surface causes silica particle aggregation. It remained a challenge for many tire manufacturers when using silica-filled elastomer compounds. Here, the silica surface energy changes when the surface is modified with coupling or noncoupling silanes; coupling silanes can covalently bond the silica to the elastomers. The surface energy of silica was determined using inverse gas chromatography (IGC) at finite dilution (FD-IGC) and found to be reduced by up to 50% when the silica surface was silanized. The spatial distribution of silica aggregates within the tire matrix is determined by transmission electron microscopy (TEM) and a direct correlation between aggregate size (silica microdispersion) and work of cohesion from IGC is reported, highlighting surface energy and work of cohesion being excellent indicators of the degree of dispersion of silica aggregates.
    Matched MeSH terms: Chromatography, Gas
  9. New magnetic oil palm fiber activated carbon-reinforced polypyrrole solid phase extraction combined with gas chromatography-electron capture detection for determination of organochlorine pesticides in water samples
    Marsin FM, Wan Ibrahim WA, Nodeh HR, Sanagi MM
    J Chromatogr A, 2020 Feb 08;1612:460638.
    PMID: 31676087 DOI: 10.1016/j.chroma.2019.460638
    Magnetic solid phase extraction (MSPE) employing oil-palm fiber activated carbon (OPAC) modified with magnetite (Fe3O4) and polypyrrole (OPAC-Fe3O4-PPy) was successfully used for the determination of two organochlorine pesticides (OCPs), namely endosulfan and dieldrin in environmental water samples. Analysis was performed using gas chromatography with micro-electron capture detection (GC-μECD). The effects of three preparation variables, namely Fe3O4:OPAC ratio, amount of pyrrole monomer, and amount of FeCl3 oxidant were optimized using Box-Behnken design (BBD) (R2 < 0.99, p-value < 0.001%). The optimum conditions were as follows: Fe3O4:OPAC ratio of 2:1 w/w, 1 g of FeCl3 and 100 μL of pyrrole monomer. The experimental results obtained agreed satisfactorily with the model prediction (> 90% agreement). Optimized OPAC-Fe3O4-PPy composite was characterized using field emission scanning electron microscope, vibrating sample magnetometer and Fourier transform infrared spectroscopy. Four numerical parameters of MSPE procedure was optimized using BBD. The significance of the MSPE parameters were salt addition > sample solution pH > extraction time and desorption time. Under the optimized conditions (extraction time: 90 s, desorption time: 10 min, salt: 0%, and pH: 5.8), the method demonstrated good linearity (25-1000 ng L-1) with coefficients of determination, R2 > 0.991, and low detection limits for both endosulfan (7.3 ng L-1) and dieldrin (8.6 ng L-1). The method showed high analyte recoveries in the range of 98.6-103.5% for environmental water samples. The proposed OPAC-Fe3O4-PPy MSPE method offered good features such as sustainability, simplicity, and rapid extraction.
    Matched MeSH terms: Chromatography, Gas*
  10. Preparation of Medicinal Plants: Basic Extraction and Fractionation Procedures for Experimental Purposes
    Abubakar AR, Haque M
    J Pharm Bioallied Sci, 2020 01 29;12(1):1-10.
    PMID: 32801594 DOI: 10.4103/jpbs.JPBS_175_19
    Preparation of medicinal plants for experimental purposes is an initial step and key in achieving quality research outcome. It involves extraction and determination of quality and quantity of bioactive constituents before proceeding with the intended biological testing. The primary objective of this study was to evaluate various methods used in the preparation and screening of medicinal plants in our daily research. Although the extracts, bioactive fractions, or compounds obtained from medicinal plants are used for different purposes, the techniques involved in producing them are generally the same irrespective of the intended biological testing. The major stages included in acquiring quality bioactive molecule are the selection of an appropriate solvent, extraction methods, phytochemical screening procedures, fractionation methods, and identification techniques. The nitty-gritty of these methods and the exact road map followed solely depends on the research design. Solvents commonly used in extraction of medicinal plants are polar solvent (e.g., water, alcohols), intermediate polar (e.g., acetone, dichloromethane), and nonpolar (e.g., n-hexane, ether, chloroform). In general, extraction procedures include maceration, digestion, decoction, infusion, percolation, Soxhlet extraction, superficial extraction, ultrasound-assisted, and microwave-assisted extractions. Fractionation and purification of phytochemical substances are achieved through application of various chromatographic techniques such as paper chromatography, thin-layer chromatography, gas chromatography, and high-performance liquid chromatography. Finally, compounds obtained are characterized using diverse identification techniques such as mass spectroscopy, infrared spectroscopy, ultraviolet spectroscopy, and nuclear magnetic resonance spectroscopy. Subsequently, different methods described above can be grouped and discussed according to the intended biological testing to guide young researchers and make them more focused.
    Matched MeSH terms: Chromatography, Gas
  11. Fulltext Microwave-Assisted Brine Extraction for Enhancement of the Quantity and Quality of Lipid Production from Microalgae Nannochloropsis sp
    Zghaibi N, Omar R, Kamal SMM, Biak DRA, Harun R
    Molecules, 2019 Oct 04;24(19).
    PMID: 31590304 DOI: 10.3390/molecules24193581
    Toward attaining a sustainability and eco-friendly process, a green and low-cost solvent-brine (NaCl solution) is proposed, as microwave-assisted extraction (MAE) technique solvent to extract lipids from microalgae Nannochloropsis sp. The effect of NaCl concentration on the quantity and quality of the extracted lipid was assessed, while MAE parameters were optimized using response surface methodology (RSM). The content of fatty acid methyl esters (FAMEs) in the lipid was analyzed by using a gas chromatography-flame ionization detector (GC/FID). The highest lipid yield (16.1%) was obtained using 10% (w/v) brine at optimum extraction parameters of 5% (w/v) solid loading, 100 °C, and 30 min. The lipid extraction yield via optimized MAE-brine technique was thrice better than that Soxhlet extraction did and only 2% less than Bligh and Dyer (B&D) lipid extraction, which utilized harmful solvents. The proposed MAE-brine technique offered better quality lipids containing the highest amount of polyunsaturated fatty acids (PUFA) (44.5%) and omega-3 fatty acids (FAs) (43%). Hence, the MAE-brine solvent technique appears to be a promising extraction method for cheaper, greener, and faster extraction of a high-quality lipid for specialty food applications.
    Matched MeSH terms: Chromatography, Gas
  12. Magnetic poly(β-cyclodextrin-ionic liquid) nanocomposites for micro-solid phase extraction of selected polycyclic aromatic hydrocarbons in rice samples prior to GC-FID analysis
    Boon YH, Mohamad Zain NN, Mohamad S, Osman H, Raoov M
    Food Chem, 2019 Apr 25;278:322-332.
    PMID: 30583379 DOI: 10.1016/j.foodchem.2018.10.145
    Poly(β-cyclodextrin functionalized ionic liquid) immobilized magnetic nanoparticles (Fe3O4@βCD-Vinyl-TDI) as sorbent in magnetic µ-SPE was developed for the determination of selected polycyclic aromatic hydrocarbons (PAHs) in rice samples coupled with gas chromatographic-flame ionization detector (GC-FID). The nanocomposite was characterized by various tools and significant parameters that affected the extraction efficiency of PAHs were investigated. The calibration curves were linear for the concentration ranging between 0.1 and 500 μg kg-1 with correlation determinations (R2) from 0.9970 to 0.9982 for all analytes. Detection limits ranged at 0.01-0.18 μg kg-1 in real matrix. The RSD values ranged at 2.95%-5.34% (intra-day) and 4.37%-7.05% (inter-day) precision for six varied days. The sorbents showed satisfactory reproducibility in 2.9% to 9.9% range and acceptable recovery values at 80.4%-112.4% were obtained for the real sample analysis. The optimized method was successfully applied to access content safety of selected PAHs for 24 kinds of commercial rice available in Malaysia.
    Matched MeSH terms: Chromatography, Gas
  13. Complete fatty acid analysis data of flaxseed oil using GC-FID method
    Danish M, Nizami M
    Data Brief, 2019 Apr;23:103845.
    PMID: 31372470 DOI: 10.1016/j.dib.2019.103845
    The data presented in this article were generated through the gas chromatography (GC) with a flame ionization detector (FID). The flaxseed oil was converted into fatty acid methyl ester (FAME) then used in the GC with FID and observe the retention time of different fatty acid present in the flaxseed oil. The observed retention time was compared with the standard fatty acid to confirm the specific fatty acid presence in the flaxseed oil. The part of the data is used in the article "Optimization of the process variable for biodiesel production by transesterification of flaxseed oil and produced biodiesel characterizations" Renewable Energy journal (Ahmad et al., 2019).
    Matched MeSH terms: Chromatography, Gas
  14. Effect of Chitosan Nanoparticle-Loaded Thymus serpyllum on Hydrogen Peroxide-Induced Bone Marrow Stromal Cell Damage
    Baig S, Azizan AHS, Raghavendran HRB, Natarajan E, Naveen S, Murali MR, et al.
    Stem Cells Int, 2019;2019:5142518.
    PMID: 30956670 DOI: 10.1155/2019/5142518
    We have determined the protective effects of Thymus serpyllum (TS) extract and nanoparticle-loaded TS on hydrogen peroxide-induced cell death of mesenchymal stromal cells (MSCs) in vitro. Gas chromatography-mass spectroscopy confirmed the spectrum of active components in the extract. Out of the three different extracts, the hexane extract showed significant free radical scavenging activity. Treatment of MSCs with H2O2 (hydrogen peroxide) significantly increased intracellular cell death; however, pretreatment with TS extract and nanoparticle-loaded TS (200 μg/ml) suppressed H2O2-induced elevation of Cyt-c and MMP13 and increased the survival rates of MSCs. H2O2-induced (0.1 mM) changes in cytokines were attenuated in the extract and nanoparticles by pretreatment and cotreatment at two time points (p < 0.05). H2O2 increased cell apoptosis. In contrast, treatment with nanoparticle-loaded TS suppressed the percentage of apoptosis considerably (p < 0.05). Therefore, TS may be considered as a potential candidate for enhancing the effectiveness of MSC transplantation in cell therapy.
    Matched MeSH terms: Chromatography, Gas
  15. Fulltext Two-Step Purification of Glycerol as a Value Added by Product From the Biodiesel Production Process
    Abdul Raman AA, Tan HW, Buthiyappan A
    Front Chem, 2019;7:774.
    PMID: 31799239 DOI: 10.3389/fchem.2019.00774
    For every ton of biodiesel produced, about 100 kg of glycerol is also generated as a by-product. The traditional method of removing glycerol is mainly by gravity separation or centrifugation. This method generates crude glycerol, which may still contain impurities such as methanol, oil, soap, salt, and other organic materials at ppm levels. The effective usage of crude glycerol is important to improve the economic sustainability of the biodiesel industry while reducing the environmental impacts caused by the generated waste. The application and value of crude glycerol can be enhanced if these impurities are removed or minimized. Thus, it is important to develop a method which can increase the economic and applicable value of crude glycerol. Therefore, in the present study, the dual step purification method comprised of acidification and ion exchange techniques has been used to purify the crude glycerol and convert it into higher-value products. The acidification process started with the pH adjustment of the crude glycerol, using phosphoric acid to convert soap into fatty acid and salts. Then, the pretreated glycerol was further purified by ion exchange with a strong cation H+ resin. Gas chromatography (GC) was used to analyze both crude and purified glycerol and expressed as the weight percentage of glycerol content. A maximum glycerol purity of 98.2% was obtained after the dual step purification method at the optimized conditions of 60% of solvent, the flow rate of 15 mL/min and 40 g of resin. Further, the glycerol content measured being within the accepted amount of BS 2621:1979. Therefore, this study has proven that the proposed crude glycerol purification process is effective in improving the glycerol purity and could enhance the applicability of glycerol in producing value-added products which bring new revenue to the biodiesel industry.
    Matched MeSH terms: Chromatography, Gas
  16. Magnetite-sporopollenin/graphene oxide as new preconcentration adsorbent for removal of polar organophosphorus pesticides in vegetables
    Markus A, Gbadamosi AO, Yusuff AS, Agi A, Oseh J
    Environ Sci Pollut Res Int, 2018 Dec;25(35):35130-35142.
    PMID: 30328041 DOI: 10.1007/s11356-018-3402-3
    In this study, a new magnetic adsorbent based on magnetite-sporopollenin/graphene oxide (Fe3O4-SP/GO) was successfully developed. The adsorbent was applied for magnetic solid phase extraction (MSPE) of three selected polar organophosphorus pesticides (OPPs), namely, dimethoate, phenthoate, and phosphamidon, prior to gas chromatography analysis with electron capture detection (GC-μECD). The Fe3O4-SP/GO adsorbent combines the advantages of superior adsorption capability of the modified sporopollenin (SP) with graphene oxide (GO) and magnetite (Fe3O4) for easy isolation from sample solution. Several MSPE parameters were optimized. Under optimized conditions, excellent linearity (R2 ≥ 0.9994) was achieved using matrix match calibration in the range of 0.1 to 500 ng mL-1. The limit of detection (LOD) method (S/N = 3) was from 0.02 to 0.05 ng mL-1. The developed Fe3O4-SP/GO MSPE method was successfully applied for the determination of these three polar OPPs in cucumber, long beans, bell pepper, and tomato samples. Good recoveries (81.0-120.0%) and good relative standard deviation (RSD) (1.4-7.8%, n = 3) were obtained for the spiked OPPs (1 ng mL-1) from real samples. This study is beneficial for adsorptive removal of toxic pesticide compounds from vegetable samples.
    Matched MeSH terms: Chromatography, Gas
  17. Fulltext Data on organochlorine concentration levels in soil of lowland paddy field, Kelantan, Malaysia
    Osman BE, Khalik WMAWM
    Data Brief, 2018 Oct;20:999-1003.
    PMID: 30225314 DOI: 10.1016/j.dib.2018.08.178
    The main goal of this research work is to measure the concentration levels of organochlorine residue in soil. The potential health risk of this pollutant on human was also determined. 10 samples were taken from a lowland paddy field situated in Kelantan, Malaysia. Physical parameters namely soil pH, organic carbon content, water content and particle size were identified to evaluate the quality of soil from the agriculture site. Soxhlet extraction and florisil clean-up process were applied to isolate 10 targeted organochlorine compounds prior to the final determination using a gas chromatography-electron capture detector. Soil from the lowland has characteristics such as slightly acidic, low organic carbon content, high water content and texture dominated by the sandy type. Concentration levels of six detected organochlorine pesticides were calculated in µg/kg. Hazard quotient value in all samples was less than the acceptable risk level HQ ≤ 1, thus reflecting the status of soil in the subjected area as unlikely to pose any adverse health effects.
    Matched MeSH terms: Chromatography, Gas
  18. Fate, distribution, and bioconcentration of pesticides impact on the organic farms of Cameron Highlands, Malaysia
    Farina Y, Munawar N, Abdullah MP, Yaqoob M, Nabi A
    Environ Monit Assess, 2018 Jun 09;190(7):386.
    PMID: 29884954 DOI: 10.1007/s10661-018-6762-8
    Occurrence and distribution of organochlorine pesticides (OCPs), organophosphate pesticides (OPPs), and pyrethroid pesticides (PYRs) residues in the leafy vegetables were analyzed together with the soil samples using gas chromatography-electron capture detector. Edible tissues of vegetables showed detectable residues of these compounds indicating the influence of the conventional farms and nearby organic farms. In the vegetables, the OCPs concentrations were recorded as nd-133.3 ng/g, OPPs as nd-200 ng/g, and PYRs as nd-33.3 ng/g. In the soil, the OCPs concentrations were recorded as nd-30.6 ng/g, OPPs as nd-26.6 ng/g, and for PYRs as nd-6.7 ng/g. Bioconcentration factor (BCF) was higher for the OPPs (0.3) than the OCPs and PYRs (1.1). The OCPs concentration in the vegetables decreased in the following order: spinach > celery > broccoli > cauliflower > cabbage > lettuce > mustard. For OPPs, the concentration decreased in the following order: cauliflower > spinach > celery > cabbage > broccoli > lettuce > mustard and for PYRs as spinach > celery > lettuce > cabbage > broccoli. Principal component analysis indicates that the sources of these pesticides are not the same, and the pesticide application on the vegetables depends on the type of crop. There is a significant positive correlation between OPPs and the soil (r = 0.65) as compared to OCPs and PYRs (r = 0.1) as the vegetables accumulated OPPs more efficiently than OCPs and PYRs.
    Matched MeSH terms: Chromatography, Gas
  19. Observation and explanation of two-dimensional interconversion of oximes with multiple heart-cutting using comprehensive multidimensional gas chromatography
    Kulsing C, Nolvachai Y, Wong YF, Glouzman MI, Marriott PJ
    J Chromatogr A, 2018 Apr 20;1546:97-105.
    PMID: 29548566 DOI: 10.1016/j.chroma.2018.02.035
    Real-time interconversion processes produce unconventional peak broadening in gas chromatography (GC), and can be used to generate kinetic and thermodynamic data. In this study, an unusual separation situation in comprehensive two dimensional GC where two dimensional interconversion (i.e. a raised plateau in both first and second dimension, 1D and 2D) was observed in analysis of oxime isomers. This resulted in a characteristic and unusual rectangular peak shape in the two dimensional result. A related theoretical approach was introduced to explain the peak shape supported by simulation results which can be varied depending on concentration profiles and kinetics of the process. The simulated results were supported by experimental results obtained by a comprehensive heart-cut multidimensional GC (H/C MDGC) approach which was developed to clearly investigate isomerisation of E/Z oxime molecules in both 1D and 2D separations under different isothermal conditions. The carrier gas flow and oven temperature were selected according to initial results for 1D interconversion on a poly(ethyleneglycol) stationary phase, which was further used in both 1D and 2D separations to result in broad zones of oxime interconversion in both dimensions. The method involved repetitive injections of oxime sample, then sampling contiguous fractions of sample into a long 2D column which is intended to promote considerable interconversion. Comprehensiveness arises from the fact that the whole sample is sampled from the 1D to the 2D column, with the long 2D column replacing the short 2D column used in classical comprehensive two-dimensional gas chromatography, where the latter will not promote sufficient interconversion. Data processing and presentation permits a 'rectangular' distribution corresponding to the separated compounds, characteristic of this experiment.
    Matched MeSH terms: Chromatography, Gas/methods*
  20. Phytochemical analysis and antioxidant activity of the seed of Telfairia occidentalis Hook (Cucurbitaceae)
    Eseyin OA, Daniel A, Paul TS, Attih E, Emmanuel E, Ekarika J, et al.
    Nat Prod Res, 2018 Feb;32(4):444-447.
    PMID: 28361553 DOI: 10.1080/14786419.2017.1308366
    The 2,2-diphenyl-1-picryl hydrazyl (DPPH) radical, nitric oxide, reducing power, hydrogen peroxide scavenging, and total antioxidant activities of the methanol extract, n-hexane, dichloromethane, ethyl acetate, butanol and aqueous fractions of the seed of Telfairia occidentalis were evaluated. Total phenolic content was determined using the Folin-Ciocalteu method. The dichloromethane fraction exhibited the highest DPPH radical scavenging, reducing power and total antioxidant activities. Two pure compounds which were identified by FTIR, H-and 2D NMR and Mass spectroscopy as 9-octadecenoic acid (TOS B) and 10-hydroxyoctadecanoic acid (TOS C) and four oily isolates, TOS A, TOS D, TOS E and TOS F were obtained from the dichloromethane fraction. TOS E had the highest DPPH radical scavening activity comparable to that of ascorbic acid. GC-MS analysis revealed the major compounds in TOS E as 4-(2,2-Dimethyl-6-methylene cyclohexylidene)-2-butanol; 3-(3-hydroxybutyl)-2,4,4-trimethyl-2-cyclohexene-1-one and 1,2-Benzenedicarboxylic acid disooctyl ester. Thus, the seed of T. occidentalis can be consumed for its antioxidant property.
    Matched MeSH terms: Chromatography, Gas
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