Search results for: Chromatography

Authors: M. O. Ezegbogu, H. B. Osadolor

Abstract:

Lipsticks constitute a significant source of transfer evidence, and can, therefore, provide corroborative or inclusionary evidence in criminal investigation. This study aimed to determine the uniqueness and persistence of different lipstick smears using Thin Layer Chromatography (TLC), and Gas Chromatography with a Flame Ionisation Detector (GC-FID). In this study, we analysed lipstick smears retrieved from tea cups exposed to the environment for up to four weeks. The n-alkane content of each sample was determined using GC-FID, while TLC was used to determine the number of bands, and retention factor of each band per smear. This study shows that TLC gives more consistent results over a 4-week period than GC-FID. It also proposes a maximum exposure time of two weeks for the analysis of lipsticks left in the open using GC-FID. Finally, we conclude that neither TLC nor GC-FID can distinguish lipstick evidence recovered from hypothetical crime scenes.

Keywords: Forensic science, chromatography, identification, lipstick.

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Authors: Areej Babiker Idris Babiker, Rosdiazli Ibrahim

Abstract:

Gas chromatography (GC) is the most widely used technique in analytical chemistry. However, GC has high initial cost and requires frequent maintenance. This paper examines the feasibility and potential of using a neural network model as an alternative whenever GC is unvailable. It can also be part of system verification on the performance of GC for preventive maintenance activities. It shows the performance of MultiLayer Perceptron (MLP) with Backpropagation structure. Results demonstrate that neural network model when trained using this structure provides an adequate result and is suitable for this purpose. cm.

Keywords: Analyzer, Levenberg-Marquardt, Gas chromatography, Neural network

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Authors: Elham Moniri, Homayon Ahmad Panahi, Ahmad Izadi, Mohamad Mehdi Parvin, Atyeh Rahimi

Abstract:

In this investigation Salicylic acid, Sulfosalicylic acid and Acetyl salicylic acid were chosen as a sample for thin layer chromatography (TLC) on silica gel plates. Bicarbonate buffer at different pH containing different amounts of boric acid was applied as mobile phase. Specific interaction of these substances with boric acid has effect on Rf in thin layer chromatography. Regular and similar trend was observed in variations of Rf for mentioned compounds in TLC by altering of percentages of boric acid in mobile phase in pH range of 8-10. Also effect of organic solvent, mixture of water/ organic solvent and organic solvent containing boric acid as mobile phase was studied.

Keywords: Thin layer chromatography (TLC), Aspirin, Salicylic acid, Sulfosalycylic acid, Boric acid.

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Authors: Ishan Arora, Anurag S. Rathore

Abstract:

The primary objective of this work was to study the effect of resin chemistry, pH and molarity of binding and elution buffer on aggregate removal using Cation Exchange Chromatography and find the optimum conditions which can give efficient aggregate removal with minimum loss of yield. Four different resins were used for carrying out the experiments: Fractogel EMD SO3 -(S), Fractogel EMD COO-(M), Capto SP ImpRes and S Ceramic HyperD. Runs were carried out on the AKTA Avant system. Design of Experiments (DOE) was used for analysis using the JMP software. The dependence of the yield obtained using different resins on the operating conditions was studied. Success has been achieved in obtaining yield greater than 90% using Capto SP ImpRes and Fractogel EMD COO-(M) resins. It has also been found that a change in the operating conditions generally has different effects on the yields obtained using different resins.

Keywords: Aggregates, cation exchange chromatography, design of experiments, monoclonal antibodies.

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Authors: Abdul Rahim Yacob, Mohamad Raizul Zinalibdin

Abstract:

A simple method for the simultaneous determination of hippuric acid and benzoic acid in urine using reversed-phase high performance liquid chromatography was described. Chromatography was performed on a Nova-Pak C18 (3.9 x 150 mm) column with a mobile phase of mixed solution methanol: water: acetic acid (20:80:0.2) and UV detection at 254 nm. The calibration curve was linear within concentration range at 0.125 to 6.0 mg/ml of hippuric acid and benzoic acid. The recovery, accuracy and coefficient variance of hippuric acid were 104.54%, 0.2% and 0.2% respectively and for benzoic acid were 98.48%, 1.25% and 0.60% respectively. The detection limit of this method was 0.01ng/l for hippuric acid and 0.06ng/l for benzoic acid. This method has been applied to the analysis of urine samples from the suspected of toluene abuser or glue sniffer among secondary school students at Johor Bahru.

Keywords: Glue sniffer, High Performance LiquidChromatography, Hippuric Acid, Toluene, Urine.

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Authors: S.H. Khoon, G.I. Issabayeva, L.W. Lee

Abstract:

Air quality in Setapak district of Kuala Lumpur was studied by analysing the rainwater chemical composition using ion chromatography method. Twelve sampling sites were selected and 120 rainwater samples were collected in the period of 10 weeks. The results of this study were compared to the earlier published data and the evaluation showed that the NO3 - ion concentration increased from 0.41 to 3.32 ppm, while SO4 2- ion concentration increased from 0.39 to 3.26 ppm over the past two decades that is mostly due to rapid urban development of the city. However, it was found that the chemical composition for both residential and industrial areas does not have significant difference. Most of the rainwater samples showed alkaline pH (pH > 5.6). The possible factors for such alkaline pH in rainwater samples are assumed to be the marine sources, biomass burning and alkaline character of soil particles.

Keywords: acid deposition; atmospheric pollution; deposition fluxes; trajectories

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Authors: D. Mohd Nazrul Hisham, J. Mohd Lip, R. Suri, H. Mohamed Shafit, Z.Kharis, K. Shazlin, A. Normah, M.F. Nurul Nabilah

Abstract:

Presence of phytosterol compound in Durian seed (Durio zibethinus) or known as King of fruits has been discovered from screening work using reagent test. Further analysis work has been carried out using mass spectrometer in order to support the priliminary finding. Isolation and purification of the major phytosterol has been carried out using an open column chromatography. The separation was monitored using thin layer chromatography (TLC). Major isolated compounds and purified phytosterol were identified using mass spectrometer and nuclear magnetic resonance (NMR). This novel finding could promote utilization of durian seeds as a functional ingredient in food products through production of standardized extract based on phytosterol content.

Keywords: Agrowaste, durian, seed, phytosterol

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Authors: N. Hachemi, A. Nouani, A. Benchabane

Abstract:

The influence of cultivation factors such as content of ammonium sulfate, glucose and water in the culture medium and particle size of dry orange waste, on their bioconversion for pectinase production was studied using complete factorial design. A polygalacturonase (PG) was isolated using ion exchange chromatography under gradient elution 0-0,5 m/l NaCl (column equilibrate with acetate buffer pH 4,5), subsequently by sephadex G75 column chromatography was applied and the molecular weight was obtained about 51,28 KDa. Purified PG enzyme exhibits a pH and temperature optima of activity at 5 and 35°C respectively. Treatment of apple juice by purified enzyme extract yielded a clear juice, which was competitive with juice yielded by pure Sigma Aldrich Aspergillus niger enzyme.

Keywords: Bioconversion, orange wastes, optimization, pectinase.

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Authors: Harshani Uggallage, Kapila D. Dissanayaka

Abstract:

A Sulforhodamine-B assay-guided fractionation on Nigella sativa seeds was conducted to determine the presence of cytotoxic compounds against human hepatoma (HepG2) cells. Initially, a freeze-dried sample of Nigella sativa seeds was sequentially extracted into solvents of increasing polarities. Crude extracts from the sequential extraction of Nigella sativa seeds in chloroform and ethyl acetate showed the highest cytotoxicity. The combined mixture of these two extracts was subjected to bioassay guided fractionation using a modified Kupchan method of partitioning, followed by Sephadex® LH-20 chromatography. This chromatographic separation process resulted in a column fraction with a convincing IC50 (half-maximal inhibitory concentration) value of 13.07 µg/ml, which is considerable for developing therapeutic drug leads against human hepatoma. Reversed phase High-Performance Liquid Chromatography (HPLC) was finally conducted for the same column fraction and the result indicates the presence of one or several main cytotoxic compounds against human HepG2 cells.

Keywords: Cytotoxic compounds, half-maximal inhibitory concentration, high-performance liquid chromatography, human HepG2 cells, Nigella sativa seeds, Sulforhodamine-B assay-guided fractionation.

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Authors: C. I. L. Justino, L. I. B. Silva, K. Duarte, A. C. Freitas, T. A. P. Rocha-Santos, A. C. Duarte

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This work proposes an optical fiber system (OF) for sensing various volatile organic compounds (VOCs) in human breath for the diagnosis of some metabolic disorders as a non-invasive methodology. The analyzed VOCs are alkanes (i.e., ethane, pentane, heptane, octane, and decane), and aromatic compounds (i.e., benzene, toluene, and styrene). The OF displays high analytical performance since it provides near real-time responses, rapid analysis, and low instrumentation costs, as well as it exhibits useful linear range and detection limits; the developed OF sensor is also comparable to a reference methodology (gas chromatography-mass spectrometry) for the eight tested VOCs.

Keywords: Breath analysis, gas chromatography-mass spectrometry, optical fiber sensor, volatile organic compounds

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Authors: Renata L. C. Leão, João E. Nascimento, Natalia C. E. S. Nascimento, Elaine S. Vasconcelos, Mércia L. Oliveira

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The quality control procedures of a radiopharmaceutical include the assessment of its chemical purity. The method suggested by international pharmacopeias consists of a thin layer chromatographic run. In this paper, the method proposed by the United States Pharmacopeia (USP) is compared to a direct method to determine the final concentration of aminopolyether in Fludeoxyglucose (¹⁸F-FDG) preparations. The approach (no chromatographic run) was achieved by placing the thin-layer chromatography (TLC) plate directly on an iodine vapor chamber. Both methods were validated and they showed adequate results to determine the concentration of aminopolyether in ¹⁸F-FDG preparations. However, the direct method is more sensitive, faster and simpler when compared to the reference method (with chromatographic run), and it may be chosen for use in routine quality control of ¹⁸F-FDG.

Keywords: Chemical purity, Kryptofix 222, thin layer chromatography, validation.

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Authors: K. Jarmkom, P. Eakwaropas, W. Khobjai, S. Techaeoi

Abstract:

Ancient Thai perfumed powder was used as a fragrance for clothing, food, and the body. Plant-based natural Thai perfume products are known as Pang-Rum. The objective of this study was to evaluate the stability of essential oils after six months of incubation. The chemical compositions were determined by gas chromatography-mass spectrometry (GC-MS), in terms of the qualitative composition of the isolated essential oil. The isolation of the essential oil of natural products by incubate sample for 5 min at 40 ºC is described. The volatile components were identified by percentage of total peak areas comparing their retention times of GC chromatograph with NIST mass spectral library. The results show no significant difference in the seven chromatograms of perfumed powder (Pang-Rum) both with binder and without binder. Further identification was done by GC-MS. Some components of Pang-Rum with/without binder were changed by temperature and time.

Keywords: GC-MS analysis, essential oils, stability, Pang-Rum.

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Authors: Rui Qiu, Giles Hardy, Dong Qu, Robert Trengove, Manjree Agarwal, YongLin Ren

Abstract:

Phytophthora cinnamomi (P. c) is a plant pathogenic oomycete that is capable of damaging plants in commercial production systems and natural ecosystems worldwide. The most common methods for the detection and diagnosis of P. c infection are expensive, elaborate and time consuming. This study was carried out to examine whether species specific and life cycle specific volatile organic compounds (VOCs) can be absorbed by solid-phase microextraction fibers and detected by gas chromatography that are produced by P. c and another oomycete Pythium dissotocum. A headspace solid-phase microextraction (HS-SPME) together with gas chromatography (GC) method was developed and optimized for the identification of the VOCs released by P. c. The optimized parameters included type of fiber, exposure time, desorption temperature and desorption time. Optimization was achieved with the analytes of P. c+V8A and V8A alone. To perform the HS-SPME, six types of fiber were assayed and compared: 7μm Polydimethylsiloxane (PDMS), 100μm Polydimethylsiloxane (PDMS), 50/30μm Divinylbenzene/CarboxenTM/Polydimethylsiloxane DVB/CAR/PDMS), 65μm Polydimethylsiloxane/Divinylbenzene (PDMS/DVB), 85μm Polyacrylate (PA) fibre and 85μm CarboxenTM/ Polydimethylsiloxane (Carboxen™/PDMS). In a comparison of the efficacy of the fibers, the bipolar fiber DVB/CAR/PDMS had a higher extraction efficiency than the other fibers. An exposure time of 16h with DVB/CAR/PDMS fiber in the sample headspace was enough to reach the maximum extraction efficiency. A desorption time of 3min in the GC injector with the desorption temperature of 250°C was enough for the fiber to desorb the compounds of interest. The chromatograms and morphology study confirmed that the VOCs from P. c+V8A had distinct differences from V8A alone, as did different life cycle stages of P. c and different taxa such as Pythium dissotocum. The study proved that P. c has species and life cycle specific VOCs, which in turn demonstrated the feasibility of this method as means of

Keywords: Gas chromatography, headspace solid-phase microextraction, optimization, volatile compounds.

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Authors: Homayon Ahmad Panahi, Hossein Sid Kalal, Atyeh Rahimi

Abstract:

A high performance thin layer chromatography system (HPTLC) for the separation of vitamin B2 and B12 has been developed. The separation was successfully using a solvent system of methanol, water, ammonia 7.3.1 (V/V) as mobile phase on HPTLC plates impregnated with boric acid. The effect of other mobile phases on the separation of vitamins was also examined. The method is based on different behavior of investigated compounds in impregnated TLC plates with different amount of boric acid. The Rf values of vitamin B2 and B12 are considered on non impregnated and impregnated silica gel HPTLC plate with boric acid. The effect of boric acid in the mobile phase and on HPTLC plates on the RF values of the vitamins has also been studied.

Keywords: High performance thin layer chromatography, HPTLC, Vitamin B2, Vitamin B12, Separation.

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Authors: Labiba I. Hussein, Maher Z. Elsabee, Eid A. Ismail, Hala F. Naguib, Hilda A. Aziz, Moataz A. Elsawy

Abstract:

Jojoba oil-wax is extracted from the seeds of the jojoba (Simmondsia chinensis Link Schneider), a perennial shrub that grows in semi desert areas in Egypt and in some parts of the world. The main uses of jojoba oil-wax are in the cosmetics and pharmaceutical industry, but new uses could arise related to the search of new energetic crops. This paper summarizes a process to convert the jojoba oil-wax to biodiesel by transesterification with ethanol and a series of aliphatic alcohols using a more economic and energy saving method in a domestic microwave. The effect of time and power of the microwave on the extent of the transesterification using ethanol and other aliphatic alcohols has been studied. The separation of the alkyl esters from the fatty alcohols rich fraction has been done in a single crystallization step at low temperature (−18°C) from low boiling point petroleum ether. Gas chromatography has been used to follow up the transesterification process. All products have been characterized by spectral analysis.

Keywords: Jojoba oil, transesterification, microwave, gas chromatography jojoba esters, Jojoba alcohol.

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Authors: Xiang Li, Kui Chen, Bin Wu, Min Zhou

Abstract:

Sclareolide is made from sclareol by oxidiative synthesis and subsequent crystallization, while the crystallization mother liquor still contains 15%~30%wt of sclareolide to be reclaimed. With the reaction material of sclareol is provided as plant extract, many sorts of complex impurities exist in the mother liquor. Due to the difficulty in recycling sclareolide after solvent recovery, it is common practice for the factories to discard the mother liquor, which not only results in loss of sclareolide, but also contributes extra environmental burden. In this paper, a process based on adsorption and elution has been presented for recycling of sclareolide from mother liquor. After pretreatment of the crystallization mother liquor by HZ-845 resin to remove parts of impurities, sclareolide is adsorbed by HZ-816 resin. The HZ-816 resin loaded with sclareolide is then eluted by elution solvent. Finally, the eluent containing sclareolide is concentrated and fed into the crystallization step in the process. By adoption of the recycle from mother liquor, total yield of sclareolide increases from 86% to 90% with a stable purity of the final sclareolide products maintained.

Keywords: Sclareolide, resin, adsorption, chromatography.

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Authors: D. S. Fardhyanti, A. Damayanti

Abstract:

Coal tar is a liquid by-product of coal pyrolysis processes. This liquid oil mixture contains various kinds of useful compounds such as benzoic aromatic compounds and phenolic compounds. These compounds are widely used as raw material for insecticides, dyes, medicines, perfumes, coloring matters, and many others. The coal tar was collected by pyrolysis process of coal obtained from PT Kaltim Prima Coal and Arutmin-Kalimantan. The experiments typically occurred at the atmospheric pressure in a laboratory furnace at temperatures ranging from 300 to 550oC with a heating rate of 10oC/min and a holding time of 1 hour at the pyrolysis temperature. The Gas Chromatography-Mass Spectroscopy (GC-MS) was used to analyze the coal tar components. The obtained coal tar has the viscosity of 3.12 cp, the density of 2.78 g/cm3, the calorific value of 11,048.44 cal/g, and the molecular weight of 222.67. The analysis result showed that the coal tar contained more than 78 chemical compounds such as benzene, cresol, phenol, xylene, naphtalene, etc. The total phenolic compounds contained in coal tar are 33.25% (PT KPC) and 17.58% (Arutmin-Kalimantan). The total naphtalene compounds contained in coal tar is 14.15% (PT KPC) and 17.13% (Arutmin-Kalimantan).

Keywords: Coal tar, pyrolysis, gas chromatography-mass spectroscopy.

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Authors: Kyung-Tae Kwon, Md. Salim Uddin, Go-Woon Jung, Jeong-Eun Sim, Byung-Soo Chun

Abstract:

Supercritical carbon dioxide (SC-CO2) was used as a solvent to extract oil from wheat bran. Extractions were carried out in a semi-batch process at temperatures ranging from 40 to 60ºC and pressures ranging from 10 to 30 MPa, with a carbon dioxide (CO2) flow rate of 26.81 g/min. The oil obtained from wheat bran at different extraction conditions was quantitatively measured to investigate the solubility of oil in SC-CO2. The solubility of wheat bran oil was found to be enhanced in high temperature and pressure. The composition of fatty acids in wheat bran oil was measured by gas chromatography (GC). Linoleic, palmitic, oleic and γ-linolenic acid were the major fatty acids of wheat bran oil. Tocopherol contents in oil were analyzed by high performance liquid chromatography (HPLC). The highest amount of phenolics and tocopherols (α and β) were found at temperature of 60ºC and pressure of 30 MPa.

Keywords: Supercritical carbon dioxide, Tocopherols, Totalphenolic content, Wheat bran oil

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Authors: M. Bounechada, F. Benia, M. Aiouaz, S. Bouharati, N. Djirar, H. Benamrani

Abstract:

The cuticular hydrocarbons of Pamphagus elephas (Orthoptera: Pamphagidae) has been analysed by gas chromatography and by combined gas chromatograph-mass spectrometry. The following hydrocarbon classes have been identified in insect cuticular hydrocarbons are: n-alkanes and methylalkanes comprising Monomethyl-, dimethyl-and trimethylalkanes. Sexual dimorphism is observed in long chain alkanes (C24-C36) present on male and female. The cuticulars hydrocarbons of P.elephas ranged from 24 to 36 carbons and incluted n-alkanes, Dimethylalkanes and Trimethylalkanes. nalkanes represented by (C24-C36,72,7% on male and 79,2% on female), internally branched Monomethylalkanes identified were (C25, C30-C32,C35-C37;11% on male and 9,4% on female), Dimethylalkanes detected are (C31-C32, C36; 2,2% on male and 2,06% on female) and Trimethylalkanes detected are (C32, C36; 3,1% on male and 4, 97 on female). Larvae male and female (stage 7) showed the same quality of n-alkanes observed in adults. However a difference quantity is noted.

Keywords: Cuticular hydrocarbons, Gas chromatography, Mass spectrometry, Pamphagus elephas, , Sexual dimorphism

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Authors: N. B. Dhayanithi, T. T. Ajith Kumar, T. Balasubramanian

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Present study summarizes the control of Vibrio alginolyticus infection in hatchery reared Clownfish, Amphiprion sebae with the extract of the mangrove plant, Avicennia marina. Fishes with visible symptoms of hemorrhagic spots were chosen and the genomic DNA of the causative bacterium was isolated and sequenced based on 16S rDNA gene. The in vitro assay revealed that a fraction of A. marina leaf extract elucidated with ethyl acetate: methanol (6:4) showed a high activity (28 mm) at 125 μg/ml concentrations. About 4 % of the fraction fed along with live V. alginolyticus was significantly decreased the cumulative mortality (P<0.05) in the experimental groups than the control group. The responsible fraction was investigated by gas chromatography - mass spectroscopy and found the presence of active compounds. This is the first research in India to control vibriosis infection in marine ornamental fish with mangrove leaf extract.

Keywords: Amphiprion seabe, Avicennia marina, Gas Chromatography - Mass Spectroscopy, Vibrio alginolyticus

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Authors: S. Lakestani, B. Karakas, S. Acar Vaizoglu, B. Guciz Dogan, C. Guler, B. Sekerel, A. Taner, G. Gullu

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Abstract–Indoor air (VOCs) samples were collected simultaneously from variety of indoors (e.g. living rooms, baby-s rooms) and outdoor environments which were voluntarily selected from the houses in which pregnant residents live throughout Ankara. This is the first comprehensive study done in Turkey starting from prenatal period and continued till the babies had one year old. VOCs levels were measured over 76 homes. Air samples were collected in Tenax TA sorbent filled tubes with active sampling method and analyzed with Thermal Desorber and Gas Chromatography/Mass spectrometry (TD-GC/MS). At the first sampling period in the baby-s rooms maximum concentration of toluene was measured about 240.77μg.m-3 and in the living rooms maximum concentration of naphthalene was 180.24μg.m-3. At the second sampling period in the baby-s rooms maximum concentration of toluene was measured about 144.97μg.m-3 and in the living rooms maximum concentration of naphthalene was 247.89μg.m-3. Concentration of TVOCs in the first period was generally higher than the second period.

Keywords: Indoor Air, Volatile Organic Compounds (VOCs), Gas Chromatography

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Authors: Najari Moghadam Sh., Qomi M., Raofie F., Khadiv J.

Abstract:

In this study, a liquid phase microextraction by hollow fiber (HF-LPME) combined with high performance liquid chromatography-UV detector was applied to preconcentrate and determine trace levels of Cyproheptadine in human urine and plasma samples. Cyproheptadine was extracted from 10 mL alkaline aqueous solution (pH: 9.81) into an organic solvent (n-octnol) which was immobilized in the wall pores of a hollow fiber. Then was back-extracted into an acidified aqueous solution (pH: 2.59) located inside the lumen of the hollow fiber. This method is simple, efficient and cost-effective. It is based on pH gradient and differences between two aqueous phases. In order to optimize the HF-LPME some affecting parameters including the pH of donor and acceptor phases, the type of organic solvent, ionic strength, stirring rate, extraction time and temperature were studied and optimized. Under optimal conditions enrichment factor, limit of detection (LOD) and relative standard deviation (RSD(%), n=3) were up to 112, 15 μg.L⁻¹ and 2.7, respectively.

Keywords: Biological samples, Cyproheptadine, hollow fiber, liquid phase microextraction.

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Authors: D. S. Fardhyanti, A. Damayanti

Abstract:

The utilization of biomass as a source of new and renewable energy is being carried out. One of the technologies to convert biomass as an energy source is pyrolysis which is converting biomass into more valuable products, such as bio-oil. Bio-oil is a liquid which is produced by steam condensation process from the pyrolysis of coconut shells. The composition of a coconut shell e.g. hemicellulose, cellulose and lignin will be oxidized to phenolic compounds as the main component of the bio-oil. The phenolic compounds in bio-oil are corrosive; they cause various difficulties in the combustion system because of a high viscosity, low calorific value, corrosiveness, and instability. Phenolic compounds are very valuable components which phenol has used as the main component for the manufacture of antiseptic, disinfectant (known as Lysol) and deodorizer. The experiments typically occurred at the atmospheric pressure in a pyrolysis reactor at temperatures ranging from 300 ^oC to 350 ^oC with a heating rate of 10 ^oC/min and a holding time of 1 hour at the pyrolysis temperature. The Gas Chromatography-Mass Spectroscopy (GC-MS) was used to analyze the bio-oil components. The obtained bio-oil has the viscosity of 1.46 cP, the density of 1.50 g/cm³, the calorific value of 16.9 MJ/kg, and the molecular weight of 1996.64. By GC-MS, the analysis of bio-oil showed that it contained phenol (40.01%), ethyl ester (37.60%), 2-methoxy-phenol (7.02%), furfural (5.45%), formic acid (4.02%), 1-hydroxy-2-butanone (3.89%), and 3-methyl-1,2-cyclopentanedione (2.01%).

Keywords: Bio-oil, pyrolysis, coconut shell, phenol, gas chromatography-mass spectroscopy.

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Authors: Donna M. Morrison, Lambert Chester, Coretta A. N. Samuels, David R. Ledoux

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A survey was conducted in the five rice-growing regions in Guyana to determine the presence of aflatoxins in multiple fractions of rice in June/October 2015 growing season. The fractions were paddy, steamed paddy, cargo rice, white rice and parboiled rice. Samples were analyzed by High Performance Liquid Chromatography. A subset of the samples was further analyzed by enzyme-linked immunosorbent assay (ELISA) for concurrence. All analyses were conducted at the University of Missouri, USA. Of the 186 samples tested, 16 had aflatoxin concentrations greater than 20 ppb the recommended limit for aflatoxins in food according to the United States Food and Drug Administration. An additional three samples had aflatoxin B₁ concentrations greater than the European Union Commission maximum levels for aflatoxin B₁ in rice at 5 µg/kg and total aflatoxins (B₁, B₂, G₁ and G₂) at 10 µg/kg. The survey indicates that there is no widespread aflatoxin problem in rice in Guyana. The incidence of aflatoxins appears to be localized.

Keywords: Aflatoxins, enzyme-linked immunosorbent assay, high-performance liquid chromatography, rice fractions.

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Authors: Espinoza S. Clara, Gamarra Q. Flor, Marianela F. Ramos Quispe S. Miguel, Flores R. Omar

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Tropaeolum majus L. is a native plant to South and Central America, used since ancient times by our ancestors to combat different diseases. Glucotropaeolonin is one of its main components, which when hydrolyzed, forms benzyl isothiocyanate (BIT) that promotes cellular apoptosis (programmed cell death in cancer cells). Therefore, the present research aims to evaluate the effect of the pressure and temperature of BIT extraction by supercritical CO₂ from Tropaeolum majus L. The extraction was carried out in a supercritical fluid extractor equipment Speed SFE BASIC Brand: Poly science, the leaves of Tropaeolum majus L. were ground for one hour and lyophilized until obtaining a humidity of 6%. The extraction with supercritical CO₂ was carried out with pressures of 200 bar and 300 bar, temperatures of 50°C, 60°C and 70°C, obtained by the conjugation of these six treatments. BIT was identified by thin layer chromatography using 98% BIT as the standard, and as the mobile phase hexane: dichloromethane (4:2). Subsequently, BIT quantification was performed by high performance liquid chromatography (HPLC). The highest yield of oleoresin by supercritical CO₂ extraction was obtained pressure 300 bar and temperature at 60°C; and the higher content of BIT at pressure 200 bar and 70°C for 30 minutes to obtain 113.615 ± 0.03 mg BIT/100 g dry matter was obtained.

Keywords: Tropaeolum majus L., supercritical fluids, benzyl isothiocyanate.

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Authors: Beena Sethi

Abstract:

This work involves the degradation of plastic waste in the presence of three different nanocatalysts. A thin film of LLDPE was formed with all three nanocatalysts separately in the solvent. Thermo Gravimetric Analysis (TGA) and Differential Scanning Calorimetric (DSC) analysis of polymers suggest that the presence of these catalysts lowers the degradation temperature and the change mechanism of degradation. Gas chromatographic analysis was carried out for two films. In gas chromatography (GC) analysis, it was found that degradation of pure polymer produces only 32% C3/C4 hydrocarbons and 67.6% C5/C9 hydrocarbons. In the presence of these catalysts, more than 80% of polymer by weight was converted into either liquid or gaseous hydrocarbons. Change in the mechanism of degradation of polymer was observed therefore more C3/C4 hydrocarbons along with valuable feedstock are produced. Adjustment of dose of nanocatalyst, use of nano-admixtures and recycling of catalyst can make this catalytic feedstock recycling method a good tool to get sustainable environment. The obtained products can be utilized as fuel or can be transformed into other useful products. In accordance with the principles of sustainable development, chemical recycling i.e. tertiary recycling of polymers along with the reuse (zero order recycling) of plastics can be the most appropriate and promising method in this direction. The tertiary recycling is attracting much attention from the viewpoint of the energy resource.

Keywords: Degradation, differential scanning calorimetry, feedstock recycling, gas chromatography, thermogravimetric analysis. DSC.

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Authors: Mohanad El-Harbawi, Nurul Amirah Hanim Bt. Umar, Norizan Ali, Yoshimitsu Uemura

Abstract:

Study of fire and explosion is very important mainly in oil and gas industries due to several accidents which have been reported in the past and present. In this work, we have investigated the flammability of bio oil vapour mixtures. This mixture may contribute to fire during the storage and transportation process. Bio oil sample derived from Palm Kernell shell was analysed using Gas Chromatography Mass Spectrometry (GC-MS) to examine the composition of the sample. Mole fractions of 12 selected components in the liquid phase were obtained from the GC-FID data and used to calculate mole fractions of components in the gas phase via modified Raoult-s law. Lower Flammability Limits (LFLs) and Upper Flammability Limits (UFLs) for individual components were obtained from published literature. However, stoichiometric concentration method was used to calculate the flammability limits of some components which their flammability limit values are not available in the literature. The LFL and UFL values for the mixture were calculated using the Le Chatelier equation. The LFLmix and UFLmix values were used to construct a flammability diagram and subsequently used to determine the flammability of the mixture. The findings of this study can be used to propose suitable inherently safer method to prevent the flammable mixture from occurring and to minimizing the loss of properties, business, and life due to fire accidents in bio oil productions.

Keywords: Gas chromatography, compositions, lower and upper flammability limits (LFL & UFL), flammability diagram.

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Authors: Mauro Giacomini, Stefania Bertone, Federico Caneva Soumetz, Carmelina Ruggiero

Abstract:

Environmental micro-organisms include a large number of taxa and some species that are generally considered nonpathogenic, but can represent a risk in certain conditions, especially for elderly people and immunocompromised individuals. Chemotaxonomic identification techniques are powerful tools for environmental micro-organisms, and cellular fatty acid methyl esters (FAME) content is a powerful fingerprinting identification technique. A system based on an unsupervised artificial neural network (ANN) was set up using the fatty acid profiles of standard bacterial strains, obtained by gas-chromatography, used as learning data. We analysed 45 certified strains belonging to Acinetobacter, Aeromonas, Alcaligenes, Aquaspirillum, Arthrobacter, Bacillus, Brevundimonas, Enterobacter, Flavobacterium, Micrococcus, Pseudomonas, Serratia, Shewanella and Vibrio genera. A set of 79 bacteria isolated from a drinking water line (AMGA, the major water supply system in Genoa) were used as an example for identification compared to standard MIDI method. The resulting ANN output map was found to be a very powerful tool to identify these fresh isolates.

Keywords: Cellular fatty acid methyl esters, environmental bacteria, gas-chromatography, unsupervised ANN.

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Authors: Jingming Wu, Ruikang Hu, Junqi Yue, Zhaoguang Yang, Lifeng Zhang

Abstract:

Fecal sterol has been proposed as a chemical indicator of human fecal pollution even when fecal coliform populations have diminished due to water chlorination or toxic effects of industrial effluents. This paper describes an improved derivatization procedure for simultaneous determination of four fecal sterols including coprostanol, epicholestanol, cholesterol and cholestanol using gas chromatography-mass spectrometry (GC-MS), via optimization study on silylation procedures using N-O-bis (trimethylsilyl)-trifluoroacetamide (BSTFA), and N-(tert-butyldimethylsilyl)-N-methyltrifluoroacetamide (MTBSTFA), which lead to the formation of trimethylsilyl (TMS) and tert-butyldimethylsilyl (TBS) derivatives, respectively. Two derivatization processes of injection-port derivatization and water bath derivatization (60 oC, 1h) were inspected and compared. Furthermore, the methylation procedure at 25 oC for 2h with trimethylsilydiazomethane (TMSD) for fecal sterols analysis was also studied. It was found that most of TMS derivatives demonstrated the highest sensitivities, followed by methylated derivatives. For BSTFA or MTBSTFA derivatization processes, the simple injection-port derivatization process could achieve the same efficiency as that in the tedious water bath derivatization procedure.

Keywords: Fecal Sterols, Methylation, Silylation, BSTFA, MTBSTFA, TMSD, GC-MS.

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Authors: Jingming Wu, Ruikang Hu, Junqi Yue, Zhaoguang Yang, Lifeng Zhang

Abstract:

Fecal sterol has been proposed as a chemical indicator of human fecal pollution even when fecal coliform populations have diminished due to water chlorination or toxic effects of industrial effluents. This paper describes an improved derivatization procedure for simultaneous determination of four fecal sterols including coprostanol, epicholestanol, cholesterol and cholestanol using gas chromatography-mass spectrometry (GC-MS), via optimization study on silylation procedures using N-O-bis (trimethylsilyl)-trifluoroacetamide (BSTFA), and N-(tert-butyldimethylsilyl)-N-methyltrifluoroacetamide (MTBSTFA), which lead to the formation of trimethylsilyl (TMS) and tert-butyldimethylsilyl (TBS) derivatives, respectively. Two derivatization processes of injection-port derivatization and water bath derivatization (60 oC, 1h) were inspected and compared. Furthermore, the methylation procedure at 25 oC for 2h with trimethylsilydiazomethane (TMSD) for fecal sterols analysis was also studied. It was found that most of TMS derivatives demonstrated the highest sensitivities, followed by methylated derivatives. For BSTFA or MTBSTFA derivatization processes, the simple injection-port derivatization process could achieve the same efficiency as that in the tedious water bath derivatization procedure.

Keywords: Fecal Sterols, Methylation, Silylation, BSTFA, MTBSTFA, TMSD, GC-MS.

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