Solid phase extraction (SPE) and dispersive solid-phase extraction (d-SPE) were compared and evaluated for the determination of λ-cyhalothrin and cypermethrin in palm oil matrices by gas chromatography with an electron capture detector (GC-ECD). Several SPE sorbents such as graphitised carbon black (GCB), primary secondary amine (PSA), C(18), silica, and florisil were tested in order to minimise fat residues. The results show that mixed sorbents using GCB and PSA obtained cleaner extracts than a single GCB and PSA sorbents. The average recoveries obtained for each pesticide ranged between 81% and 114% at five fortification levels with the relative standard deviation of less than 7% in all cases. The limits of detection for these pesticides were ranged between 0.025 and 0.05 μg/g. The proposed method was applied successfully for the residue determination of both λ-cyhalothrin and cypermethrin in crude palm oil samples obtained from local mills throughout Malaysia.
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.
A simple and sensitive analytical method has been developed employing gas chromatography coupled with electron capture detector (GC-ECD), and validated for screening and quantification of 15 pesticide residues at trace levels in cabbage, broccoli, cauliflower, lettuce, celery, spinach, and mustard. The method consists of two steps, first, to determine the significance of each factor by Pareto chart followed by optimization of these significant factors using central composite design (CCD). Minitab statistical software was used for these multivariate experiments for the generation of 2(4-1) design and CCD matrices. The method evaluation was done by external standard calibration with linearity range between 0.5 and 3mg/kg, with correlation coefficient 0.99, limit of detection (LOD) ranges between 0.02 and 4.5ng/g, and limit of quantification (LOQ) ranges between 0.2 and 45ng/g. The average recovery was between 60% and 128%, with RSD 0.2-19.8%. The method was applied on real vegetable samples from Cameron Highlands.
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.
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.
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.
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.
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.
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.
High intake of trans fatty acids (TFA) may cause adverse changes in blood lipids as shown in many epidemiological studies. The major sources of TFA in human diet come from bakery products such as cookies, cakes, muffins, breads and pastries. In this study, total fat of baked products was determined using Soxhlet method while TFA content was determined on gas chromatograph using a highly polar capillary column and flame ionization detector. Exposure to TFA from the baked product was estimated based on Food Consumption Statistics of Malaysia 2003. High level of TFA was observed in muffins (3.21-7.34 g per 100 g food) followed by pastries (2.90-6.03 g per 100 g food) and cakes (2.26-8.36 g per 100 g food) regardless of products having brand name or not. Among the TFA isomers, trans 18:1 6t was the most abundant followed by trans 18:1 9t, trans 16:1 9t, trans 18:2 and small quantities of trans 18:1 11t. Exposure to TFA based on the Malaysian Food Consumption Statistics 2003 of the baked products was ranging from 0.14-0.18 g/day. Even with the low estimated exposure, actual intake of baked products must be monitored closely as other high fat food as these products is one of main contributor to TFA in the diet following their high frequency of daily intake.
A study was carried out to distinguish mono- (MAG) and di-acylglycerol (DAG) from plant lipids such as sunflower, rapeseed and soybean oil, from those derived from animal fats such as lard, goat fat and beef fat using fatty acid and thermal profile data. MAG and DAG of both plant and animal lipids were synthesized according to a chemical glycerolysis method catalyzed by sodium hydroxide. MAG and DAG of individual lipid were isolated and purified using the standard column chromatography method and subjected to fatty acid analysis by gas chromatography (GC) and thermal analysis by differential scanning calorimetry (DSC). The application of principal component analysis (PCA) to the data collected from the individual instrumental technique showed that it was possible to distinctly classify MAG and DAG of plant lipids from those derived from animal fats.
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.
The fatty acid composition and trans fatty acid (TFA) contents of biscuits products were determined by gas chromatography, using a highly polar 100m capillary column (HP-88) and flame ionization detection. Total TFA ranged from 0.00 – 0.52 g/100 g total fatty acids and 0.12 – 0.68 g/100 g total fatty acids for local packed and unpacked biscuits, respectively. In imported biscuits, total TFA was higher ranging from 0.03 – 3.09 g/100 g of total fatty acids. Trans 16:1 was the most abundant, with values ranging from 0.01% to 38% followed by trans 18:1 Δ11 (0.01% - 13.11%), trans 18:1 Δ9 (0.01% - 4.68%), trans 18:2 (0.23% - 2.77%) and small quantities of trans 18:1 Δ6. CLA, the natural TFA constituted from 0.1% to
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.
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 fatty acid composition and trans fatty acids (TFA) contents of samples of five Malaysian cream crackers biscuit brands were determined by gas-liquid chromatography, using a 60 m Supelco SP2340 fused silica capillary column and flame ionization detection. The identities of the fatty acids were established by comparing their retention times with authentic standards from Supelco. The results were expressed as relative percentages. The total saturated fatty acids (SFA) in the samples ranged from 48.90% to 54.87% of total fatty acids. As for the polyunsaturated fatty acids (PUFA), the total PUFA in the samples ranged from 9.97% to 11.73% of total fatty acids. Total trans fatty acids (TFA) ranged from 0.17% to 0.77% of total fatty acids. The monotrans 18:2 tc or 18:2 ct isomer content ranged from 0.07% to 0.10% of total fatty acids and the ditrans 18:2 isomer (9t, 12t) was not detected. The results indicate that all the fat sources of the 5 sample crackers biscuit brands were palm oil based.
Phoenix dactylifera L (Date palm) is one of the oldest known fruit crops in the world, and
the consumption of date fruits is no longer restricted to the Middle Eastern countries. Date
palm kernels are waste products of date fruit industry which are normally being discarded.
Based on their dietary fiber content; date palm kernels (DPK) have been proposed to be used
as fiber-based food supplement, caffeine free coffee alternative and animal feed ingredient.
Hence, utilization of such waste is highly desirable for the date industry. To accommodate these
benefits, and subsequent to some uses associated with DPK, this study sought to investigate the
biochemical and nutritional values of the Barhi date palm kernels (BDPK) grown in Iraq. The
results show that BDPK is an excellent source of dietary fiber (66.24 g/100g). Glutamic acid
was found to be the predominant amino acid, (0.674 g/100g), followed by Arginine and aspartic
acid (0.437 g/100g and 0.320 g/100g, respectively). Potassium was the most occurring mineral
in BDPK (2.39 g/kg), and the main sugars were sucrose and fructose (0.548 g/100g and 0.249
g/100g, respectively). Gas-liquid chromatography revealed that the main unsaturated fatty acid
(USFA) was oleic acid (40.927 mg/100g), while the main saturated fatty acid (SFA) were lauric
acid (20.270 mg/100g) and myristic acid (12.288 mg/100g). Furthermore, the BDPK depicted
considerable concentrations of vitamins, in which vitamin B5 (40.4 mg/100g) showed the
highest value. The results obtained indicate a strong potential for BDPK to be used in human
nutrition, cosmetics, and pharmaceutical applications and may provide an important economic
advantage through increasing the utilization of BDKP while also additive value will be added
to the residue.
A simple analytical method for the determination of propionic acid and propionates in bakery products using a simple sample preparation procedure is described. The method involves the conversion of propionates to the non-ionized molecular form by adding glacial acetic acid, which is at the same time efficiently extracted into dichloromethane. After vortexing for 1 min, the extract was directly injected into a capillary gas chromatographic column with flame ionization detector. The method was applied for the determination of propionates in 112 commercial bakery samples. The levels of propionic acid plus propionates in bread, cake/ rolls, burger/hot dog buns and pita breads ranged from 197-1273, 98-1846, 546-1932 and 479-1680 µg mL -1 , respectively. No propionate was detected in any of the 36 biscuit samples analyzed.
Three strains of Spirulina platensis isolated from different locations showed capability of synthesizing poly(3-hydroxybutyrate) [P(3HB)] under nitrogen-starved conditions with a maximum accumulation of up to 10 wt.% of the cell dry weight (CDW) under mixotrophic culture conditions. Intracellular degradation (mobilization) of P(3HB) granules by S. platensis was initiated by the restoration of nitrogen source. This mobilization process was affected by both illumination and culture pH. The mobilization of P(3HB) was better under illumination (80% degradation) than in dark conditions (40% degradation) over a period of 4 days. Alkaline conditions (pH 10-11) were optimal for both biosynthesis and mobilization of P(3HB) at which 90% of the accumulated P(3HB) was mobilized. Transmission electron microscopy (TEM) revealed that the mobilization of P(3HB) involved changes in granule quantity and morphology. The P(3HB) granules became irregular in shape and the boundary region was less defined. In contrast to bacteria, in S. platensis the intracellular mobilization of P(3HB) seems to be faster than the biosynthesis process. This is because in cyanobacteria chlorosis delays the P(3HB) accumulation process.
A simple and rapid gas chromatography (GC) method with flame ionization detector was developed for detection of isopropyl para-toluenesulphonate (IPTS) in palm-based isopropyl palmitate (IPP) and isopropyl myristate (IPM). The method involved spiking the IPP/IPM samples with IPTS and directly injecting the spiked samples into GC without undergoing clean-up steps. The calibration curves for IPTS showed good linearity with coefficient correlation of 0.9999 for six-point calibration from 0.5 to 50 μg mL(-1) and 0.9996 for six-point calibration from 0.5 to 200 μg mL(-1) . IPTS recoveries from IPP were 98.6-103.5% with relative standard deviation (RSD) of 0.40-2.80%, whereas recoveries from IPM were 97.0-107.2% with RSD of 0.42-4.21%. The identity of IPTS recovered from the isopropyl esters was confirmed by a GC-mass spectrometer detector. The method was successfully applied to the analyses of IPTS in commercial samples. It was found that there were IPTS in the range of 34.8-1303.0 μg g(-1) in the palm-based esters for some of the samples analysed.