In this study, caged calcium alginate-caged multiwalled carbon nanotubes dispersive microsolid phase extraction was described for the first time for the extraction of polycyclic aromatic hydrocarbons (PAHs) from water samples prior to gas chromatographic analysis. Fluorene, phenanthrene and fluoranthene were selected as model compounds. The caged calcium alginate-caged multiwalled carbon nanotubes was characterized by Fourier transform infrared spectroscopy, scanning electron microscopy and thermal gravimetry analyses. The effective parameters namely desorption solvent, solvent volume, extraction time, desorption time, the mass of adsorbent and sample volume were optimized. Under the optimum extraction conditions, the developed method showed good linearity in the range of 0.5-50 ng mL-1 (R2 ≥ 0.996), low limits of detection and quantification (0.42-0.22 ng mL-1) (0.73-1.38 ng mL-1) respectively, good relative recoveries (71.2-104.2%) and reproducibility (RSD 1.8-12.4%, n = 3) for the studied PAHs in water sample. With high enrichment factor (1,000), short extraction time (<30 min), low amounts of adsorbent (100 mg) and low amounts of solvent (0.1 mol) have proven that the microsolid phase extraction method based on calcium alginate-caged multiwalled carbon nanotubes are environmentally friendly and convenient extraction method to use as an alternative adsorbent in the simultaneous preconcentration of PAHs from environmental water samples.
This study was conducted to quantitatively determine the fatty acid contents of 20 species of marine fish and four species of shellfish from Straits of Malacca. Most samples contained fairly high amounts of polyunsaturated fatty acids (PUFAs), especially alpha-linolenic acid (ALA, C18:3 n3), eicosapentaenoic acid (EPA, C20:5 n3), and docosahexaenoic acid (DHA, C22:6 n3). Longtail shad, yellowstripe scad, and moonfish contained significantly higher (P < 0.05) amounts of eicosapentaenoic acid (EPA), docosahexaenoic acid (DHA), and alpha-linolenic acid (ALA), respectively. Meanwhile, fringescale sardinella, malabar red snapper, black pomfret, Japanese threadfin bream, giant seaperch, and sixbar grouper showed considerably high content (537.2-944.1 mg/100 g wet sample) of desirable omega-3 fatty acids. The polyunsaturated-fatty-acids/saturated-fatty-acids (P/S) ratios for most samples were higher than that of Menhaden oil (P/S = 0.58), a recommended PUFA supplement which may help to lower blood pressure. Yellowstripe scad (highest DHA, ω - 3/ω - 6 = 6.4, P/S = 1.7), moonfish (highest ALA, ω - 3/ω - 6 = 1.9, P/S = 1.0), and longtail shad (highest EPA, ω - 3/ω - 6 = 0.8, P/S = 0.4) were the samples with an outstandingly desirable overall composition of fatty acids. Overall, the marine fish and shellfish from the area contained good composition of fatty acids which offer health benefits and may be used for nutraceutical purposes in the future.
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.
Phenolic chemicals with their very low taste and odour thresholds, high persistence and toxicity, are of growing concern as water pollutants. The compounds are known to exist in raw water as well as in treated water. The level of phenolic priority pollutants in water within the catchment area of the Linggi River Treatment Plant in Negeri Sembilan, Malaysia, which includes the Linggi river basin, was monitored. The 4-aminoantipyrin colourimetric method was used to determine total phenols whereas capillary column gas chromatography was used to determine the individual compounds. The results show that at most sampling stations, particularly those within the Seremban municipality, the level of phenols was found to exceed the recommended Malaysian standard of 2.0 μg/L(-1) for raw water. This is seen as the direct impact of industrial and urbanization of the area and clearly indicates the unhealthy state of the Linggi river. The results also indicate the need to improve the water quality if the river is going to be used as a source of raw water.
The sample preparation step has been identified as the bottleneck of analytical methodology in chemical analysis. Therefore, there is need for the development of cost-effective, easy to operate, and environmentally friendly miniaturized sample preparation technique. The microextraction techniques combine extraction, isolation, concentration, and introduction of analytes into analytical instrument, to a single and uninterrupted step, and improve sample throughput. The use of liquid-phase microextraction techniques for the analysis of pesticide residues in fruits and vegetables are discussed with the focus on the methodologies employed by different researchers and their analytical performances. Analytes are extracted using water-immiscible solvents and are desorbed into gas chromatography, liquid chromatography, or capillary electrophoresis for identification and quantitation.
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.
Four species of bacteria, Acinetobacter lwoffii, Aeromonas hydrophila, Pseudomonas aeruginosa and Pseudomonas putida, were isolated from soil contaminated with hydrocarbons and selected for the determination of growth requirements and the ability to degrade petroleum hydrocarbon. The bacteria were grown in mineral salt medium (MSM) supplemented with two types of crude oil, either Sumandak or South Angsi at 1% (v/v) concentration. The optimum pH for growth of A. hydrophila and P. aeruginosa was 6.5 when grown with Sumandak and South Angsi oil. For A. lwoffii and P. putida the optimum pH for growth with Sumandak and South Angsi oil was 6.5 or 7.0, respectively. The growth of P. aeruginosa was the highest in MSM when supplemented with 1% South Angsi oil and 0.5% tryptone at pH 6.5 while, in Sumandak oil the growth was the highest when yeast extract was added. Gas chromatography analysis showed that the South Angsi crude oil components of C12 to C25 were more extensively degraded by A. lwoffii after 24 h of incubation compared to the other bacteria over the same period.
INTRODUCTION: There is a lack of information on the trans fatty acid (TFA) content in Malaysian foods. The objective of this study is to determine the TFA content of bakery products, snacks, dairy products, fast foods, cooking oils and semisolid fats, and breakfast cereals and Malaysian fast foods. This study also estimated the quantity of each isomer in the foods assayed.
METHODS: The trans fatty acid content of each food sample was assessed in duplicate by separating the fatty acid methyl esters (FAME) in a gas chromatography system equipped with HP-88 column (USA: split ratio 10: 1) for cis/trans separation. Five major TFA isomers, palmitoelaidic acid (16: 1t9), petroselaidic acid (18:1t6), elaidic acid (18:1t9), vaccenic acid (18: 1t11) and linoelaidic acid (18:2t9, 12), were measured using gas chromatography (GC) and the data were expressed in unit values of g/100 g lipid or g/100 g food.
RESULTS: The total TFA contents in the studied foods were < 0.001 g-8.77 g/100 g lipid or < 0.001 g-5.79 g/100 g foods. This value falls within the standard and international recommendation level for TFA. The measured range of specific TFA isomers were as follows: palmitoelaidic acid (< 0.001 g-0.26 g/100 g lipid), petroselaidic acid (< 0.001 g - 3.09 g/100 g lipid), elaidic acid (< 0.001 g-0.87 g/100 g lipid), vaccenic acid (< 0.001 g-0.41 g/100 g lipid) and linoelaidic acid (< 0.001 g-6.60 g/100 g lipid).
CONCLUSION: These data indicate that most of the tested foods have low TFA contents (< 1 g/100 g lipid).
Effect of 2.0 % ginger oil (GO) and 1.5 % ginger extract (GE) in combination with 10.0 % gum arabic (GA) was evaluated for the postharvest control of anthracnose and maintaining quality of Eksotika II papaya fruit during storage at 12 ± 1 °C and 80-85 % RH. Antifungal compounds present in GO and GE were analyzed using gas chromatography and GO was found to contain α-pinene, 1, 8-cineole and borneol, while only borneol was present in GE due to different extraction methods applied. The highest antifungal activity was shown in 2.0 % GO combined with 10 % GA, which significantly (P
The aim of the present study was to evaluate the effect of chicken nuggets addition on the degradation of canola oil during frying compared to the changes occurring when the same frying medium was simply heated at frying temperature as control. Heating or frying test was carried out at 185±5oC using electric fryer for 8 h/day for 3 consecutive days and the oil sample was collected every 4 h. The changes in fatty acids composition and physicochemical properties of the oil samples during frying and controlled heating experiments were monitored. In this study, refractive index, free fatty acid content, peroxide value, p-anisidine value, polar compounds and viscosity of the oils all increased, whereas iodine value and C18:2/C16:0 ratio decreased as heating or frying progressed. The percentage of linoleic acid tended to decrease, whereas the percentages of palmitic acid increased. Gas chromatography analysis revealed that adding chicken nuggets to heated canola oil led to higher decrease in the ratio of C18.2/C16:0 compared to what was measured when the fat alone was heated at frying temperature. The presence of chicken nuggets accelerates the formation of polymerization products and polar compounds in canola oil during frying.
In early attempts to isolate palm oil-utilising bacteria from palm oil mill effluent (POME), diluted liquid samples of POME were spread on agar containing POME as primary nutrient. 45 purified colonies were screened for intracellular lipids by staining with Sudan Black B. Of these, 10 isolates were positively stained. The latter were grown in a nitrogen-limiting medium with palm olein (a triglyceride) or saponified palm olein (salts of fatty acids) as carbon source. None of the isolates grew in the palm olein medium but all grew well in the saponified palm olein medium. Of the latter however, only one isolate was positively stained with Nile Blue A, indicating the presence of PHA. This method did not successfully generate bacterial isolates which could metabolise palm olein to produce PHA. An enrichment technique was therefore developed whereby a selective medium was designed. The latter comprised minerals and palm olein (1% w/v) as sole carbon source to which POME (2.5% v/v) was added as the source of bacteria. The culture was incubated with shaking at 30 degrees C for 4 weeks. Out of seven isolates obtained from the selective medium, two isolates, FLP1 and FLP2, could utilise palm olein for growth and production of the homopolyester, poly(3-hydroxybutyrate). FLP1 is gram-negative and is identified (BIOLOG) to have 80% similarity to Burkholderia cepacia. When grown with propionate or valerate, FLP1 produced a copolyester, poly(3-hydroxybutyrate-co-3-hydroxyvalerate).
This study aims to determine the concentration of sterols used as biomarkers in the surface microlayer (SML) in estuarine areas of the Selangor River, Malaysia. Samples were collected during different seasons through the use of a rotation drum. The analysis of sterols was performed using gas chromatography equipped with a flame ionisation detector (GC-FID). The results showed that the concentrations of total sterols in the SML ranged from 107.06 to 505.55 ng L(-1). The total sterol concentration was found to be higher in the wet season. Cholesterol was found to be the most abundant sterols component in the SML. The diagnostic ratios of sterols show the influence of natural sources and waste on the contribution of sterols in the SML. Further analysis, using principal component analysis (PCA), showed distinct inputs of sterols derived from human activity (40.58%), terrigenous and plant inputs (22.59%) as well as phytoplankton and marine inputs (17.35%).
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.
The present work aims to address the gas-phase biotransformation of geraniol into citronellol using growing cells of Saccharomyces cerevisiae (baker's yeast) in a continuous-closed-gas-loop bioreactor (CCGLB). This study revealed that the gaseous geraniol had a severe effect on the production of biomass during the growing cell biotransformation resulting in the decrease in the specific growth rate from 0.07 to 0.05 h⁻¹. The rate of reaction of the growing cell biotransformation was strongly affected by agitation and substrate flow rates. The highest citronellol concentration of 1.18 g/L and initial rate of reaction of 7.06 × 10⁻⁴ g/min g(cell) were obtained at 500 rpm and 8 L/min, respectively.
Kojic acid monooleate is a fatty acid derivative of kojic acid which can be widely used as a skin whitening agent in a cosmetic applications. In avoiding any possible harmful effects from chemically synthesized product, the enzymatic synthesis appears to be the best way to satisfy the consumer demand nowadays. The ability of immobilized lipase from Rhizomucor meihei (lipozyme RMIM) to catalyze the direct esterification of kojic acid and oleic acid was investigated. Response Surface Methodology (RSM) and 5-level-4-factor central composite rotatable were employed to evaluate the effects of synthesis parameters such as enzyme amount (0.1-0.4 g), temperature (30-60 degrees C), substrate molar ratio (1-4 mmol, kojic acid:oleic acid) and reaction time (24-48 h) on percentage molar conversion to kojic acid monooleate. Analysis of the product using TLC, GC and FTIR showed the presence of kojic acid monooleate. The optimal conditions for the enzymatic reaction were obtained after analysis with backward elimination using 0.17 g of enzyme and 4 mmol of substrate at 52.50 degrees C for 42 h. Under these conditions the esterification percentage was 37.21%. The results demonstrated that response surface methodology can be applied effectively to optimize the lipase-catalysed synthesis of kojic acid monooleate. The optimum conditions can be used to scale up the process.
Omega-3 fatty acids have been shown to reduce the risk of chronic diseases like cardiovascular disease and cancer as well as promote brain development among infants and children. This study was carried out to compare total protein, fat and omega-3 fatty acids content of raw and pressurized fish of P. pangasius (yellowtail catfish) and H. macrura (long tail shad). The fish was cooked using pressure cooker for six minute to be pressurized. The protein content was determined by using Kjedahl method while total fat was determined using solvent extraction using chloroform and methanol. Fatty acid methyl esters (FAME) were prepared by a direct transesterification method, and quantified by gas chromatography using external standard. Results showed that marine fish H. macrura (long tail shad) had higher content (p < 0.05) of protein (18.30 ± 0.040 g/100 g), fat (10.965 ± 1.610 g/100 g), EPA (11.83 ± 0.02 g/100 g) and DHA (5.96 ± 0.31 g/100 g) compared to freshwater fish P. pangasius (yellowtail catfish). The protein content of pressurized fish was higher compare to raw fish, but there was no difference in total fat and omega-3 fatty acids content between raw and pressurized of freshwater fish P. pangasius and marine fish, H. macrura. In conclusion, marine fish are better source of protein, fat and omega-3 content, while pressurized fish shown to have comparable amount of protein, fat and omega-3 fatty acids content with raw fish. The result obtained assist the consumers to prepare a healthy menu in order to retain the protein and omega-3 fatty acids content of fish through healthy way of cooking.
The present study investigates the detection of lard in cocoa butter through changes in fatty acids composition, triacylglycerols profile, and thermal characteristics. Cocoa butter was mixed with 1% to 30% (v/v) of lard and analyzed using a gas chromatography flame ionization detector, high performance liquid chromatography, and differential scanning calorimetry. The results revealed that the mixing of lard in cocoa butter showed an increased amount of oleic acid in the cocoa butter while there was a decrease in the amount of palmitic acid and stearic acids. The amount of POS, SOS, and POP also decreased with the addition of lard. A heating thermogram from the DSC analysis showed that as the concentration of lard increased from 3% to 30%, two minor peaks at -26 °C and 34.5 °C started to appear and a minor peak at 34.5 °C gradually overlapped with the neighbouring major peak. A cooling thermogram of the above adulterated cocoa butter showed a minor peak shift to a lower temperature of -36 °C to -41.5 °C. Values from this study could be used as a basis for the identification of lard from other fats in the food authentication process.
The aim of this study was to optimize the antioxidant activity of Piper nigrum L. essential oil extracted using the supercritical carbon dioxide (SC-CO₂) technique. Response surface methodology was applied using a three-factor central composite design to evaluate the effects of three independent extraction variables: pressure of 15-30 MPa, temperature of 40-50 °C and dynamic extraction time of 40-80 min. The DPPH radical scavenging method was used to evaluate the antioxidant activity of the extracts. The results showed that the best antioxidant activity was achieved at 30 MPa, 40 °C and 40 min. The extracts were analyzed by GC-FID and GC-MS. The main components extracted using SC-CO₂ extraction in optimum conditions were β-caryophyllene (25.38 ± 0.62%), limonene (15.64 ± 0.15%), sabinene (13.63 ± 0.21%), 3-carene (9.34 ± 0.04%), β-pinene (7.27 ± 0.05%), and α-pinene (4.25 ± 0.06%). The essential oil obtained through this technique was compared with the essential oil obtained using hydro-distillation. For the essential oil obtained by hydro-distillation, the most abundant compounds were β-caryophyllene (18.64 ± 0.84%), limonene (14.95 ± 0.13%), sabinene (13.19 ± 0.17%), 3-carene (8.56 ± 0.11%), β-pinene (9.71 ± 0.12%), and α-pinene (7.96 ± 0.14%). Radical scavenging activity of the extracts obtained by SC-CO₂ and hydro-distillation showed an EC₅₀ of 103.28 and 316.27 µg mL(-1) respectively.
Thermally assisted hydrolysis and methylation-gas chromatography (THM-GC) in the presence of an organic alkali was validated for the compositional analysis of poly(3-hydroxybutyrate-co-3-hydroxyhexanoate) [P(3HB-co-3HHx)] accumulated in whole bacterial cells. Recombinant Cupriavidus necator Re2058/pCB113 was grown in a batch fermentation with different concentration of palm oil and fructose in order to control the molar fraction of 3HHx in P(3HB-co-3HHx) produced in the cells. Trace amounts (30μg) of freeze-dried cells were directly subjected to THM-GC in the presence of tetramethylammonium hydroxide (TMAH) at 400°C. The obtained chromatograms clearly showed nine characteristic peaks, attributed to the THM products from 3HB and 3HHx units in the polymer chains, without any appreciable interference by the bacterial matrix components. Based on these peak intensities, the copolymer compositions were determined rapidly without using any cumbersome and lengthy sample pretreatment as in conventional GC method. Moreover, the compositions thus obtained were strongly correlated with those by NMR and conventional GC involving solvent extraction.
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.