Anopheles maculatus Theobald sensu lato is a species complex now consisting of eight sibling species; An. maculatus is still represented by two cytologically distinct forms; i.e., the widely distributed sensu strictu or B, and E from southern Thailand and adjacent areas in northern Malaysia. Cuticular lipid profiles in conjunction with principal component analysis was used to separate An. maculatus form E from sensu stricto form B in a preliminary survey of the An. maculatus complex at five locations spanning peninsular Malaysia. The relative rank orders, from the areas of the five gas chromatographic peaks used to determine lipid differences for specimens from peninsular Malaysia, matched well with those from cytogenetically identified colony specimens of An. maculatus forms B and E. The two-dimensional principal component pattern of specimens identified as form E was highly clumped, which indicated that very similar cuticular lipids were present within this putative malaria vector. Both forms coexisted in peninsular Malaysia, but form E may be dominant except in the south.
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.
Aquaculture activity has increased the population of crab, hence increasing the generation of related wastes, particularly the shell. In addition, the number of molting process in crabs compounds further the amount of waste shell generated. As such, in the present work, the application of the waste crab shell as a source of CaO in transesterification of palm olein to biodiesel (methyl ester) was investigated. Preliminary XRD results revealed that thermally activated crab shell contains mainly CaO. Parametric study has been investigated and optimal conditions were found to be methanol/oil mass ratio, 0.5:1; catalyst amount, 4 wt. %; and reaction temperature, 338 K. As compared to laboratory CaO, the catalyst from waste crab shell performs well, thus creating another low-cost catalyst source for producing biodiesel as well as adding value to the waste crab shell. Reusability of crab shell CaO has also been studied and the outcome confirmed that the catalyst is capable to be reutilized up to 11 times, without any major deterioration.
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.
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.
The leaf and bark oils of Cinnamomum verum J.S. Presl. were examined for their antifungal activity against 6 dermatophytes (Trichophyton rubrum, T. mentagrophytes, T. tonsurans, Microsporum canis, M. gypseum and M. audouini), one filamentous fungi (Aspergillus fumigatus) and 5 strains of yeasts (Candida albicans, Ca. glabrata, Ca. tropicalis, Ca. parapsilosis and Crytococcus neoformans) by using the broth microdilution method. The antifungal activities of 4 standard compounds (cinnamaldehyde, eugenol, linalool and a-terpineol) which were major constituents in the oils were also investigated in an effort to correlate the effectiveness of the oils with those of the components of the oils. The combined antifungal effect of the oils against M. canis, M. gypseum and Cr. neoformans was investigated by the checkerboard assay. Isobolograms were constructed and Fractional Inhibitory Concentrations Index (FICI) were calculated to determine the combination effects between the oils. The chemical composition of the oils was analyzed by gas chromatography (GC) and gas chromatography- mass spectrometry (GC-MS). The oils showed strong activity against all the tested fungi with Minimum Inhibition Concentration (MIC) values ranging from 0.04 to 0.31 mg/ml. Cinnamaldehyde which was the most abundant component of the bark oil of C. verum showed the strongest activity against all the fungi studied. Based on the results of the assay on standard samples, it may be that the high levels of cinnamaldehyde and eugenol in the oils and in combination with the minor components could be responsible for the high antifungal activity of the oils. The antifungal effect of the leaf and bark oils of C. verum in combination against the tested fungi was not synergistic. However, the effect was additive against M. gypseum and antagonistic against Cr. neoformans and M. canis.
This paper discusses a rapid GC-FID technique for the simultaneous quantitative analysis of FFA, MAG, DAG, TAG, sterols, and squalene in vegetable oils, with special reference to palm oil. The FFA content determined had a lower SE compared with a conventional titrimetric method. Squalene and individual sterols, consisting of beta-sitosterol, stigmasterol, campesterol, and cholesterol, were accurately quantified without any losses. This was achieved through elimination of tedious conventional sample pretreatments, such as saponification and preparative TLC. With this technique, the separation of individual MAG, consisting of 16:0, 18:0, and 18:1 FA, and the DAG species, consisting of the 1,2(2,3)- and 1,3-positions, was sufficient to enable their quantification. This technique enabled the TAG to be determined according to their carbon numbers in the range of C44 to C56. Comparisons were made with conventional methods, and the results were in good agreement with those reported in the literature.
The application of supercritical fluid chromatography (SFC) coupled with a UV variable-wavelength detector to isolate the minor components (carotenes, vitamin E, sterols, and squalene) in crude palm oil (CPO) and the residual oil from palm-pressed fiber is reported. SFC is a good technique for the isolation and analysis of these compounds from the sources mentioned. The carotenes, vitamin E, sterols, and squalene were isolated in less than 20 min. The individual vitamin E isomers present in palm oil were also isolated into their respective components, alpha-tocopherol, alpha-tocotrienol, gamma-tocopherol, gamma-tocotrienol, and delta-tocotrienol. Calibration of all the minor components of palm as well as the individual components of palm vitamin E was carried out and was found to be comparable to those analyzed by other established analytical methods.
Methyl esters from the triglyceride fraction of the neutral lipids of natural rubber latex were found by gas liquid chromatography to contain about 90% of a furanoid acid. Spectroscopic analysis identified the acid as 10,13-epoxy-11-methyloctadeca-10,12-dienoic acid.
Dioxins are a most toxic compound ever studied by human until today. Their significant health effects involved all ranges of age, including infants due to exposure to contaminated breast milk. The objective of the study was to appraise the status of dioxin contamination in breast milk among postnatal mothers live in urban and suburban areas in Klang Valley. It was conducted as a cross sectional study involving 101 postnatal mothers who came for their infant second hepatitis B vaccination. The samples were analysed using High Resolution Gas Chromatography (HRGC) following the USEPA Method 8290. About 70.3% of the samples were found detected with dioxin congeners. More suburban mothers have positive breast milk dioxins compared to urban mothers, 100.0% and 67.0% respectively. Significant associated factors include high fat daily intake (p=0.013), high milk daily intake (p= 0.044), high meat daily intake (p=0.001), body mass index more than 30 kg/m2 (p=0.005), and body fat % of more than 26% (p=0.046). In conclusion, amount daily intake of fat diet, meat, milk, body mass index and body fat are significant associated factors for the present of dioxins in breast milk among postnatal mothers in Klang Valley. More suburban mothers contain dioxins in their breast milk, which poses higher risk of health problems among their infants. A comprehensive study need to be conducted and regular followup need to be established in monitoring the future severity of maternal breast milk contamination to ensure the health of the next generations.
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).
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%).
Extended use of GC-FID and GC-MS in oil spill fingerprinting and matching is significantly important for oil classification from the oil spill sources collected from various areas of Peninsular Malaysia and Sabah (East Malaysia). Oil spill fingerprinting from GC-FID and GC-MS coupled with chemometric techniques (discriminant analysis and principal component analysis) is used as a diagnostic tool to classify the types of oil polluting the water. Clustering and discrimination of oil spill compounds in the water from the actual site of oil spill events are divided into four groups viz. diesel, Heavy Fuel Oil (HFO), Mixture Oil containing Light Fuel Oil (MOLFO) and Waste Oil (WO) according to the similarity of their intrinsic chemical properties. Principal component analysis (PCA) demonstrates that diesel, HFO, MOLFO and WO are types of oil or oil products from complex oil mixtures with a total variance of 85.34% and are identified with various anthropogenic activities related to either intentional releasing of oil or accidental discharge of oil into the environment. Our results show that the use of chemometric techniques is significant in providing independent validation for classifying the types of spilled oil in the investigation of oil spill pollution in Malaysia. This, in consequence would result in cost and time saving in identification of the oil spill sources.
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.
Sensorial analysis of pineapple breads (conventionally baked, Cpb; fully baked frozen, Fpb and partially baked, Ppb) showed no significant differences in terms of aroma and taste. On the contrary, the scores for the overall quality between the partially baked and conventionally baked breads showed significant (p < 0.05) differences. At the same time, headspace analysis using a solid-phase microextraction (SPME) method identified 59 volatile compounds. The results of the aroma extracts dilution analysis (AEDA) revealed 19 most odour-active compounds with FD factors in the range of 32-128 as the key odourants of the pineapple breads. Further analysis of the similarities and differences between the pineapple breads in terms of the key odourants were carried out by the application of PLS-DA and PLS-regression coefficients. Results showed that Ppb exhibited strong positive correlations with most of the volatile- and non-volatile compounds, while the Cpb showed significant positive correlations with hexanal and 4-hydroxy-2,5-dimethyl-3(2H)-furanone, and the Fpb had strong positive correlations with lactic acid, benzoic acid, benzaldehyde and ethyl propanoate.
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.
Vitamin E is recognized as an essential vitamin since its discovery in 1922. Most vegetable oils contain a mixture of tocopherols and tocotrienols in the vitamin E composition. Structurally, tocopherols and tocotrienols share a similar chromanol ring and a side chain at the C-2 position. Owing to the three chiral centers in tocopherols, they can appear as eight different stereoisomers. Plant sources of tocopherol are naturally occurring in the form of RRR while synthetic tocopherols are usually in the form of all-racemic mixture. Similarly, with only one chiral center, natural tocotrienols occur as the R-isoform. In this review, we aim to discuss a few chromatographic methods that had been used to separate the stereoisomers of tocopherols and tocotrienols. These methods include high performance liquid chromatography, gas chromatography and combination of both. The review will focus on method development including selection of chiral columns, detection method and choice of elution solvent in the context of separation efficiency, resolution and chiral purity. The applications for separation of enantiomers in vitamin E will also be discussed especially in terms of the distinctive biological potency among the stereoisoforms.
The essential oils obtained by hydrodistillation of the rhizomes of Alpinia aquatica Rosc. syn. Alpinia melanocarpa and Alpinia malaccensis Roscoe were analysed by capillary gas chromatography and gas chromatography-mass spectrometry. Eighteen compounds, representing 98.4% of the essential oil were identified in A. aquatica rhizome oil, with β-sesquiphellandrene in 36.5% being the major constituent, while 20 compounds representing 99.7% of the rhizome oil of A. malaccensis were identified, among which methyl (E)-cinnamate (78.2%) was the major constituent.
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.
Redox polymerization of acrylonitrile (AN) with ethyl acrylate (EA) and fumaronitrile (FN), as comonomer and termonomer respectively, were carried out using sodium bisulfite (SBS) and potassium persulphate (KPS) as initiators at 40°C. The actual composition of monomers in copolymers and terpolymers has been characterized by gas chromatography (GC). The effects of EA and FN on the glass transition temperature (Tg) and stabilization temperature have been studied by Differential Scanning Calorimetry (DSC). The degradation behaviour and char yield were obtained by thermogravimetric analysis. Meanwhile, incorporation of 10 mol% of EA in homoPAN system was found to greatly reduce Tg to 66°C as compared to that of the homoPAN (Tg=105°C). The initial cyclization temperature (Ti) was found to be higher (264°C) in comparison to that of homoPAN (246°C). In addition, the incorporation of EA was also shown to reduce the char yield of copolymer to 40%. When FN was incorporated as termonomer, the char yield of poly(AN/EA/ FN) 90/4/6 increased up to 44% after the heat treatment with the lowest Ti (241°C).