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.
LOD and LOQ are two important performance characteristics in method validation. This work compares three methods based on the International Conference on Harmonization and EURACHEM guidelines, namely, signal-to-noise, blank determination, and linear regression, to estimate the LOD and LOQ for volatile organic compounds (VOCs) by experimental methodology using GC. Five VOCs, toluene, ethylbenzene, isopropylbenzene, n-propylbenzene, and styrene, were chosen for the experimental study. The results indicated that the estimated LODs and LOQs were not equivalent and could vary by a factor of 5 to 6 for the different methods. It is, therefore, essential to have a clearly described procedure for estimating the LOD and LOQ during method validation to allow interlaboratory comparisons.
Four methods were developed for the analysis of fluroxypyr in soil samples from oil palm plantations. The first method involved the extraction of the herbicide with 0.05 M NaOH in methanol followed by purification using acid base partition. The concentrated material was subjected to derivatization and then cleaning process using a florisil column and finally analyzed by gas chromatography (GC) equipped with electron capture detector (ECD). By this method, the recovery of fluroxypyr from the spiked soil ranged from 70 to 104% with the minimum detection limit at 5 microg/kg. The second method involved solid liquid extraction of fluroxypyr using a horizontal shaker followed by quantification using high performance liquid chromatography (HPLC) equipped with UV detector. The recovery of fluroxypyr using this method, ranged from 80 to 120% when the soil was spiked with fluroxypyr at 0.1-0.2 microg/g soil. In the third method, the recovery of fluroxypyr was determined by solid liquid extraction using an ultrasonic bath. The recovery of fluroxypyr at spiking levels of 4-50 microg/L ranged from 88 to 98% with relative standard deviations of 3.0-5.8% with a minimum detection limit of 4 microg/kg. In the fourth method, fluroxypyr was extracted using the solid liquid extraction method followed by the cleaning up step with OASIS HLB (polyvinyl dibenzene). The recovery of fluroxypyr was between 91 and 95% with relative standard deviations of 4.2-6.2%, respectively. The limit of detection in method 4 was further improved to 1 pg/kg. When the weight of soil used was increased 4 fold, the recovery of fluroxypyr at spiking level of 1-50 microg/kg ranged from 82-107% with relative standard deviations of 0.5-4.7%.
Among the various biomaterials available for tissue engineering and therapeutic applications, microbial polyhydroxyalkanoates (PHAs) offer the most diverse range of thermal and mechanical properties. Of particular interest are the PHAs that contain 4-hydroxybutyrate such as poly(3-hydroxybutyrate-co-4-hydroxybutyrate) [P(3HB-co-4HB) and poly(4-hydroxybutyrate) [P(4HB)]. These polyesters can only be synthesized by a few types of bacteria, among which Comamonas acidovorans has the most efficient metabolic pathways to channel 4HB monomers. The resulting polyesters are bioabsorbable and are being developed as a new biomaterial for medical applications. By controlling the molar ratio of the monomers, it is possible to produce materials that are as tough and elastic as rubber.
A comparison of dissipation of chlorothalonil, chlorpyrifos, and profenofos in a Malaysian agricultural soil between the field experiment and simulation by the PERSIST model was studied. A plot of sweet pea (Pisum sativum) from a farm in the Cameron Highlands was selected for the field experiment. The plot was treated with chlorothalonil, chlorpyrifos, and profenofos. Core soil collection was conducted according to the sampling schedule. Residues of the three pesticides were analyzed in the laboratory. Simulations of the three pesticides' persistency were also conducted using a computer-run software PERSIST. Generally, predicted data obtained using PERSIST were found to be high for the three pesticides except for one field measurement of chlorpyrifos. The predicted data for profenofos, which is the most mobile of the three pesticides tested, was not well matched with the observed data compared to chlorothalonil and chlorpyrifos.
Fatty acid profile from crude extracts of local sea cucumber Stichopus chloronotus was determined using gas chromatography (GC) technique. The extracts were prepared separately in methanol, ethanol, phosphate buffer saline (PBS), and distilled water as part of our study to look at the affinity of these solvents in extracting the lipid from sea cucumber. The PBS and distilled water extractions indicate water-soluble components, while the organic fractions are extracted in methanol and ethanol as organic solvents. Furthermore, water extraction is the conventional method practiced in Malaysia. In our analysis the C14:0 (myristic), C16:0 (palmitic), C18:0 (stearic), C18:2 (linoleic), C20:0 (arachidic), and C20:5 (eicosapentaenoic, EPA) were significantly different (p < 0.01) in the four solvent extractions. However, the PBS extraction contained a much higher percentage of EPA (25.69%) compared to 18.89% in ethanol, 7.84% in distilled water, and only 5.83% in methanol, and variances were significantly different (p < 0.01 ). On the other hand, C22:6 (docosahexaenoic acid or DHA) is much higher in water extraction (57.55%), in comparison to the others where only 3.63% in PBS and 1.20% in methanol, and this difference is significant at p < 0.01. No DHA was detected in ethanol extractions. Subsequently, C18:1 (oleic acid) was only detected in PBS (21.98%) and water extraction (7.50%). It is interesting that palmitic acid, C16:() was higher in methanol (20.82%) and ethanol (2.18%), while 12.55% was detected in PBS and only 2.20% in water extraction: and again this was significantly different at p < 0.01. Although our results have shown that all four solvents were different in terms of their ability to extract fatty acids, the major component for tissue repair was well preserved. Probably this is one of the important precocious steps when working with a delicate sea cucumber, in both experimental and/or at the preparative stages. Freshness of the sea cucumber samples is important when undertaking this type of experiment. Finally, we believe that the local sea cucumber S. chloronotus contains all the fatty acids required to play a potential active role in tissue repair.
Solid-phase extraction (SPE) of organochlorine pesticide residues from environmental water samples was evaluated using octadecyl (C18)-bonded porous silica. The efficiency of SPE of these pesticide residues from reagent water samples at 1-5 micrograms dm-3 levels was compared with those obtained by solvent extraction with hexane and Freon TF (trichlorotrifluoroethane). Average recoveries exceeding 80% for these organochlorine pesticides were obtained via the SPE method using small cartridges containing 100 mg of 40 microns C18-bonded porous silica. The average recovery by solvent extraction with hexane and Freon TF exceeded 90% in both instances. It was concluded that the recoveries and precision for the SPE of organochlorine pesticides were poorer than those for the solvent extraction method. Organochlorine pesticide residue levels in environmental water samples from two major rivers flowing through predominantly rice-growing areas were monitored by gas chromatography using the solvent extraction method with hexane. Exceptionally high levels of organochlorine pesticide residues such as BHC, DDT, heptachlor, endosulfan and dieldrin were found in these water samples.
1. Fatty acid profiles in the external mucus extract and roe of Channa striatus were determined using gas chromatography (GC). 2. The mucus samples were collected by inducing hypothermic stress (-20 degrees C) for about 1 hr, and the roe were collected from gravid females at night soon after they liberated their eggs in a spawning program. 3. All mucus and roe samples were freeze-dried, except a part of roe which was not. 4. The mucus extract contained unsaturated fatty acid (oleic acid, C18:1 and linoleic acid, C18:2) as a major component, 21.25% and 22.47% of total lipid. 5. For the freeze- and nonfreeze-dried roe, the major components of fatty acid were somewhat similar to the mucus but with higher percentages: 58.56%, 26.08% and 45.76%, 20.94%. Interestingly, the nonfreeze-dried roe contained a large proportion of arachidic acid, C20:0 (22.16%), which was totally absent in the freeze-dried roe samples. 6. This profiling of the fatty acid mucus extract and roe is useful in strengthening the earlier claims that haruan possesses a potential remedy for wound healing (Mat Jais et al., 1994). Therefore, we are discussing the possibility of getting an optimum amount of the essential fatty acid for wound healing from various other parts of the fish without sacrificing the fish.
The use of organochlorine pesticides has caused concern due to their effects on human health and the Malaysian aquatic ecosystem, particularly so in view of their persistent and bioaccumulative properties. Since the extent of organochlorine pesticide pollution in Malaysian waterways is unknown except for isolated instances, a systematic survey has now been carried out. Water samples from various rivers were extracted, cleaned up with Florisil and analysed for the individual organochlorine pesticides by gas chromatography (GC) with an electron capture detector (ECD). DDE, DDT and heptachlor were present in all the river water samples of the west coast of Peninsular Malaysia. Other organochlorine pesticides were also identified from the water samples. However, the levels of all these are still below criteria values for Malaysian aquatic life, indicating that organochlorine pesticide pollution is less of a problem than other organic or inorganic pollutants.
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.
Lactic acid concentration was determined in 37 specimens of cerebrospinal fluid by gas liquid chromatography. It was found to be raised (30 mg/dl) in 15 specimens from culture positive cases of bacterial meningitis and one of fungal meningitis. It was < 30 mg/dl in cerebrospinal fluid from four cases of viral meningoencephalitis and 10 contaminated specimens. It was also raised in two specimens from culture negative cases. Determination of cerebrospinal fluid lactic acid concentration by gas liquid chromatography provides a useful, additional test in the diagnosis of bacterial meningitis
Separation of 1,2(2,3)- and 1,3-positional isomers of diacylglycerols (DAG) from vegetable oils by reversed-phase high-performance liquid chromatography (RP-HPLC) is investigated. The method is based on isocratic elution using 100% acetonitrile and UV detection at 205 nm. The following elution order of DAG molecular species is identified: 1,3-dilinolein < 1,2-dilinolein < 1,3-dimyristin < 1-oleoyl-3-linoleoyl-glycerol < 1,2-dimyristoyl-rac-glycerol < 1(2)-oleoyl-2(3)-linoleoyl-glycerol < 1-linolenoyl-3-stearoyl-glycerol < 1(2)-linolenoyl-2(3)-stearoyl-glycerol < 1,3-diolein < 1-palmitoyl-3-oleoyl-glycerol < 1,2-dioleoyl-sn-glycerol < 1(2)-palmitoyl-2(3)-oleoyl-glycerol < 1-linoleoyl-3-stearoyl-glycerol < 1,3-dipalmitin < 1(2)-linoleoyl-2(3)-stearoyl-glycerol < 1-oleoyl-3-stearoyl-glycerol < 1,2-dipalmitoyl-rac-glycerol < 1-palmitoyl-3-stearoyl-sn-glycerol < 1,3-distearin < 1,2-distearoyl-rac-glycerol. Linearity is observed over three orders of magnitude. Limits of detection and quantitation range 0.2-0.7 microg/mL for 1,3-dilinolein to 0.6-1.9 microg/mL for 1,2-dioleoyl-sn-glycerol, respectively. Precision and accuracy of the method are also demonstrated. The method is developed to separate mixtures of DAG molecular species produced from edible oils.
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.
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.
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.
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.
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).
This study investigates the effect of flaxseed oil towards physicochemical and sensory properties of reduced fat ice creams and its stability in ice-creams upon storage. Three formulations, (F1, F2, F3) were developed by substituting milk fat with flaxseed oil at levels of 2.5%, 5.0% and 7.5%, (w/w) respectively. Samples were subjected to sensory evaluation and analyses such as meltdown, titratable acidity, pH, total solids, protein and fatty acids composition. Incorporation of flaxseed oil into ice-cream showed no effects on physicochemical properties of the ice-creams. However, it increased the colour of ice-cream towards yellowness, decreased the sweetness, smoothness and creaminess. Flaxseed oil incorporation also slightly (P < 0.05) decreased the acceptance level of aroma, flavour, texture and overall acceptability of formulated icecreams. The most acceptable level of flaxseed oil substitution is at 2.5 %. Gas chromatography analysis showed that fatty acids slightly decreased upon storage.
A study was carried out to compare the composition and thermal profiles of the fat component of six brands of commercial biscuits (BA, BB, BC, BD, BE & BF) with those of lard and palm oil. Extraction of fat from biscuit samples was done using petroleum ether according to the soxhlet extraction procedure. The isolated fat samples along with lard and palm oil were analyzed using gas liquid chromatography (GLC), reversed-phase high performance liquid chromatography (RP-HPLC), and differential scanning calorimetry (DSC). According to GLC analysis, palm oil, lard and all six biscuit brands had either palmitic or oleic acid as major fatty acids. Sn-2 positional analysis of fatty acids showed that oleic (> 60%) as the most dominant fatty acid of palm oil and biscuit brands BA, BB, BC, and BD while palmitic (> 60%) as the most dominant fatty acid of lard and biscuit brands BE and BF. RP-HPLC analysis showed that the triacylglycerol (TAG) profiles of lard and biscuit brands BE and BF were closely similar while those of brands BA, BB, BC, and BD and palm oil were similar. DSC analysis showed that the cooling and heating profiles of lard and brands BE and BF were similar, while those of palm oil and brands BA, BB, BC, and BD were similar. Hence, this study concluded that biscuit brands BE and BF are not suitable for consumers whose religious restriction prohibit the use of lard as food ingredient.
The application of magnetized graphene (G) layers synthesized on the carbon nanofibers (CNFs) (m-G/CNF) was investigated as novel adsorbent for the magnetic solid-phase extraction (MSPE) of polycyclic aromatic hydrocarbons (PAHs) in water samples followed by gas chromatography-flame ionization detector (GC-FID). Six important parameters, affecting the extraction efficiency of PAHs, including: amount of adsorbent, adsorption and desorption times, type and volume of the eluent solvent and salt content of the sample were evaluated. The optimum extraction conditions were obtained as: 5min for extraction time, 20mg for sorbent amount, dichloromethane as desorption solvent, 1mL for desorption solvent volume, 5min for desorption time and 15% (w/v) for NaCl concentration. Good performance data were obtained at the optimized conditions. The calibration curves were linear over the concentration ranges from 0.012 to 100ngmL(-1) with correlation coefficients (r) between 0.9950 and 0.9967 for all the analytes. The limits of detection (LODs, S/N=3) of the proposed method for the studied PAHs were 0.004-0.03ngmL(-1). The relative standard deviations (RSDs) for five replicates at two concentration levels (0.1 and 50ngmL(-1)) of PAHs were ranged from 3.4 to 5.7%. Appropriate relative recovery values, in the range of 95.5-99.9%, were also obtained for the real water sample analysis.