Search results for: headspace solid-phase microextraction

Authors: M. Trinidad Pérez-Palacios, Catarina Petisca, Olívia Pinho, Isabel M.P.L.V.O. Ferreira

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This work evaluated the effect of temperature on headspace solid-phase microextraction of volatile and furanic compounds in coated fish sticks. The major goal was the analysis of the samples as consumed, to reproduce volatile compounds people feel when consuming those products. Extraction at 37 ºC (the human body temperature) throughout the HS-SPME analysis of volatile and furanic compounds in coated fish was compared with higher extraction temperatures, which are frequently used for this kind of determinations. The profile of volatile compounds found in deepfried (F) and non-fried (NF) coated fish at 37 and 50 ºC was different from that obtained at 80 ºC. Concerning furan and its derivatives, an extra formation of these compounds was observed at higher extraction temperatures. The analysis of volatile and furanic compounds in fish coated sticks simulating the cooking and eating conditions can be reliably carried out setting the headspace absorption temperature at 37 ºC.

Keywords: Analysis of samples as consumed, fish coated sticks, furans, headspace extraction temperature, volatiles.

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

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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: K. Mohammed, M. Agarwal, J. Mewman, Y. Ren

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An optimum technic has been developed for extracting volatile organic compounds which contribute to the aroma of lime fruit (Citrus aurantifolia). The volatile organic compounds of healthy and infested lime fruit with California red scale Aonidiella aurantii were characterized using headspace solid phase microextraction (HS-SPME) combined with gas chromatography (GC) coupled flame ionization detection (FID) and gas chromatography with mass spectrometry (GC-MS) as a very simple, efficient and nondestructive extraction method. A three-phase 50/30 μm PDV/DVB/CAR fibre was used for the extraction process. The optimal sealing and fibre exposure time for volatiles reaching equilibrium from whole lime fruit in the headspace of the chamber was 16 and 4 hours respectively. 5 min was selected as desorption time of the three-phase fibre. Herbivorous activity induces indirect plant defenses, as the emission of herbivorous-induced plant volatiles (HIPVs), which could be used by natural enemies for host location. GC-MS analysis showed qualitative differences among volatiles emitted by infested and healthy lime fruit. The GC-MS analysis allowed the initial identification of 18 compounds, with similarities higher than 85%, in accordance with the NIST mass spectral library. One of these were increased by A. aurantii infestation, D-limonene, and three were decreased, Undecane, α-Farnesene and 7-epi-α-selinene. From an applied point of view, the application of the above-mentioned VOCs may help boost the efficiency of biocontrol programs and natural enemies’ production techniques.

Keywords: Lime fruit, Citrus aurantifolia, California red scale, Aonidiella aurantii, VOCs, HS-SPME/GC-FID-MS.

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

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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: Suttipong Phosuksirikul, Rawichar Chaipojjana, Arunsri Leejeerajumnean

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The aim of research was to define the relations between volatile compounds, some parameters (pH, titratable acidity (TA), total soluble solid (TSS), lactic acid bacteria count) and consumer preference of commercial fermented milks. These relations tend to be used for controlling and developing new fermented milk product. Three leading commercial brands of fermented milks in Thailand were evaluated by consumers (n=71) using hedonic scale for four attributes (sweetness, sourness, flavour, and overall liking), volatile compounds using headspace-solid phase microextraction (HS-SPME) GC-MS, pH, TA, TSS and LAB count. Then the relations were analyzed by principal component analysis (PCA). The PCA data showed that all of four attributes liking scores were related to each other. They were also related to TA, TSS and volatile compounds. The related volatile compounds were mainly on fermented produced compounds including acetic acid, furanmethanol, furfural, octanoic acid and the volatiles known as artificial fruit flavour (beta pinene, limonene, vanillin, and ethyl vanillin). These compounds were provided the information about flavour addition in commercial fermented milk in Thailand.

Keywords: Fermented milk, volatile compounds, preference, PCA.

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Authors: K. Benhabib, X. Pierens, V-D Nguyen, G. Mimanne

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The main hypothesis of the dynamics of solid phase microextraction (SPME) is that steady-state mass transfer is respected throughout the SPME extraction process. It considers steady-state diffusion is established in the two phases and fast exchange of the analyte at the solid phase film/water interface. An improved model is proposed in this paper to handle with the situation when the analyte (atrazine) is in contact with colloid suspensions (carboxylate latex in aqueous solution). A mathematical solution is obtained by substituting the diffusion coefficient by the mean of diffusion coefficient between analyte and carboxylate latex, and also thickness layer by the mean thickness in aqueous solution. This solution provides an equation relating the extracted amount of the analyte to the extraction a little more complicated than previous models. It also gives a better description of experimental observations. Moreover, the rate constant of analyte obtained is in satisfactory agreement with that obtained from the initial curve fitting.

Keywords: Pesticide, SPME methods, polyacrylate, steady state.

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Authors: Fariba Tadayon, Elmira Hassanlou, Hasan Bagheri, Mostafa Jafarian

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Heavy metals are released into water, plants, soil, and food by natural and human activities. Lead has toxic roles in the human body and may cause serious problems even in low concentrations, since it may have several adverse effects on human. Therefore, determination of lead in different samples is an important procedure in the studies of environmental pollution. In this work, an ultrasonic assisted-ionic liquid based-liquid-liquid microextraction (UA-IL-DLLME) procedure for the determination of lead in zucchini, pomegranate, and lettuce has been established and developed by using flame atomic absorption spectrometer (FAAS). For UA-IL-DLLME procedure, 10 mL of the sample solution containing Pb2+ was adjusted to pH=5 in a glass test tube with a conical bottom; then, 120 μL of 1-Hexyl-3-methylimidazolium hexafluoro phosphate (CMIM)(PF6) was rapidly injected into the sample solution with a microsyringe. After that, the resulting cloudy mixture was treated by ultrasonic for 5 min, then the separation of two phases was obtained by centrifugation for 5 min at 3000 rpm and IL-phase diluted with 1 cc ethanol, and the analytes were determined by FAAS. The effect of different experimental parameters in the extraction step including: ionic liquid volume, sonication time and pH was studied and optimized simultaneously by using Response Surface Methodology (RSM) employing a central composite design (CCD). The optimal conditions were determined to be an ionic liquid volume of 120 μL, sonication time of 5 min, and pH=5. The linear ranges of the calibration curve for the determination by FAAS of lead were 0.1-4 ppm with R2=0.992. Under optimized conditions, the limit of detection (LOD) for lead was 0.062 μg.mL-1, the enrichment factor (EF) was 93, and the relative standard deviation (RSD) for lead was calculated as 2.29%. The levels of lead for pomegranate, zucchini, and lettuce were calculated as 2.88 μg.g-1, 1.54 μg.g-1, 2.18 μg.g-1, respectively. Therefore, this method has been successfully applied for the analysis of the content of lead in different food samples by FAAS.

Keywords: Dispersive liquid-liquid microextraction, Central composite design, Food samples, Flame atomic absorption spectrometry.

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Authors: A. Mandić, M. Sakač, A. Mišan, B. Šojić, L. Petrović, I. Lončarević, B. Pajin, I. Sedej

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Aldehydes as secondary lipid oxidation products are highly specific to the oxidative degradation of particular polyunsaturated fatty acids present in foods. Gas chromatographic analysis of those volatile compounds has been widely used for monitoring of the deterioration of food products. Developed static headspace gas chromatography method using flame ionization detector (SHS GC FID) was applied to monitor the aldehydes present in processed foods such as bakery, meat and confectionary products.

Five selected aldehydes were determined in samples without any sample preparation, except grinding for bakery and meat products. SHS–GC analysis allows the separation of propanal, pentanal, hexanal, heptanal and octanal, within 15min. Aldehydes were quantified in fresh and stored samples, and the obtained range of aldehydes in crackers was 1.62±0.05 – 9.95±0.05mg/kg, in sausages 6.62±0.46 – 39.16±0.39mg/kg; and in cocoa spread cream 0.48±0.01 – 1.13±0.02mg/kg. Referring to the obtained results, the following can be concluded, proposed method is suitable for different types of samples, content of aldehydes varies depending on the type of a sample, and differs in fresh and stored samples of the same type.

Keywords: Lipid oxidation, aldehydes, crackers, sausage, cocoa cream spread.

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Authors: Rita Riekstina-Dolge, Zanda Kruma, Daina Karklina

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Aroma forming volatiles are important components of fermented beverages. The aim of current research is to evaluate the volatile compounds and phenolic compounds of commercial ciders. Volatile aroma compounds and TPC of seven commercial ciders were determined. Extraction of aroma compounds was performed using solid phase microextraction (DVB/Car/PDMS fibre). Analysis of volatile aroma compounds was made using a Perkin Elmer Clarus 500 GC/MS. Total phenol content (TPC) was determined according to the Folin-Ciocalteu spectrophotometric method and results were expressed as gallic acid equivalents. The highest volatile compounds were in apple ciders with pear flavor. The highest TPC and lower content of volatile compounds were detected in French ciders.

Keywords: cider, TPC, volatile compounds

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Authors: Eva Ungure, Sandra Muizniece-Brasava, Lija Dukalska, Vita Levkane

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The objective of the research was to evaluate the quality of milk pomade sweet – sherbet packed in different packaging materials (Multibarrier 60, met.BOPET/PE, Aluthen), by several packaging technologies – active and modified atmosphere (MAP) (consisting of 100% CO2), and control – in air ambiance. Experiments were carried out at the Faculty of Food Technology of Latvia University of Agriculture. Samples were stored at the room temperature +21±1 °C. The physiochemical properties – weight losses, moisture, hardening, colour and changes in headspace atmosphere concentration (CO2 and O2) of packs were analysed before packaging and after 2, 4, 6, 8, 10 and 12 storage weeks.

Keywords: packaging, shelf life, sherbet with crunchy peanut chip's

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Authors: Sandra Muizniece-Brasava, Lija Dukalska, Irisa Murniece, Ilona Dabina-Bicka, Emils Kozlinskis, Svetlana Sarvi, Ralfs Santars, Anna Silvjane

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The research object was wheat bread. Experiments were carried out at the Faculty of Food Technology of the Latvia University of Agriculture. An active packaging in combination with modified atmosphere (MAP, CO2 60% and N2 40%) was examined and compared with traditional packaging in air ambiance. Polymer Multibarrier 60, PP and OPP bags were used. Influence of iron based oxygen absorber in sachets of 100 cc obtained from Mitsubishi Gas Chemical Europe Ageless® was tested on the quality during the shelf of wheat bread. Samples of 40±4 g were packaged in polymer pouches (110 mm x 120 mm), hermetically sealed by MULTIVAC C300 vacuum chamber machine, and stored in room temperature +21.0±0.5 °C. The physiochemical properties – weight losses, moisture content, hardness, pH, colour, changes of atmosphere content (CO2 and O2) in headspace of packs, and microbial conditions were analysed before packaging and in the 7th, 14th, 21st and 28th days of storage.

Keywords: Active packaging, wheat bread, shelf life.

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Authors: Ping Du, Masaki Sagehashi, Akihiko Terada, Masaaki Hosomi

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Prediction of benzene transport in soil and volatilization from soil to the atmosphere is important for the preservation of human health and management of contaminated soils. The adequacy of a simple numerical model, assuming two-phase diffusion and equilibrium of liquid/solid adsorption, was investigated by experimental data of benzene concentration in a flux chamber (with headspace) where Andosol and sand were filled. Adsorption experiment for liquid phase was performed to determine an adsorption coefficient. Furthermore, adequacy of vapor phase adsorption was also studied through two runs of experiment using sand with different water content. The results show that the model adequately predicted benzene transport and volatilization from Andosol and sand with water content of 14.0%. In addition, the experiment additionally revealed that vapor phase adsorption should be considered in diffusion model for sand with very low water content.

Keywords: Benzene; Transport Model, Adsorption, Soil Contaminant.

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Authors: Sandra Muizniece-Brasava, Lija Dukalska, Solvita Kampuse, Irisa Murniece, Martins Sabovics, IlonaDabina-Bicka, Emils Kozlinskis, Svetlana Sarvi

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The research object was apple-black currant marmalade candies. Experiments were carried out at the Faculty of Food Technology of the Latvia University of Agriculture. An active packaging in combination with modified atmosphere (MAP, CO2 100%) was examined and compared with traditional packaging in air ambiance. Polymer Multibarrier 60 and paper bags were used. Influence of iron based oxygen absorber in sachets of 500 cc obtained from Mitsubishi Gas Chemical Europe Ageless® was tested on the quality during the shelf of marmalade. Samples of 80±5 g were packaged in polymer pouches (110 mm x 110 mm), hermetically sealed by MULTIVAC C300 vacuum chamber machine, and stored in room temperature +20.0±1.0 °C. The physiochemical properties – weight losses, moisture content, hardness, aw, pH, colour, changes of atmosphere content (CO2 and O2) in headspace of packs, and microbial conditions were analysed before packaging and in the 1st, 3rd , 5th, 8th, 11th and 15th weeks of storage.

Keywords: Active packaging, marmalade candies, shelf life

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Authors: I. Krasnova, L. Dukalska, D. Seglina, K. Juhnevica, E. Sne, D. Karklina

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Experiments were carried out at the Latvia State Institute of Fruit-Growing in 2011. Fresh-cut minimally processed apple and pear mixed salad were packed by passive modified atmosphere (MAP) in PP containers, which were hermetically sealed by breathable conventional BOPP PropafreshTM P2GAF, and Amcor Agrifresh films. Biodegradable NatureFlexTM NVS INNOVIA Films and VC999 BioPack PLA films coated with a barrier of pure silicon oxide (SiOx) were used to compare the fresh-cut produce quality with this packed in conventional packaging films. Samples were cold stored at temperature +4.0±0.5 °C up to 10 days. The quality of salad was evaluated by physicochemical properties – weight losses, moisture, firmness, the effect of packaging modes on the colour, dynamics in headspace atmosphere concentration (CO2 and O2), titratable acidity values, as well as by microbiological contamination (yeasts, moulds and total bacteria count) of salads, analyzing before packaging and after 2, 4, 6, 8, and 10 storage days.

Keywords: Biodegradable packaging, conventional, fresh-cut fruit salad

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Authors: Edison Muzenda, Ayo S. Afolabi

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This paper is a continuation of our interest in the influence of temperature on specific retention volumes and the resulting infinite dilution activity coefficients. This has a direct effect in the design of absorption and stripping columns for the abatement of volatile organic compounds. The interaction of 13 volatile organic compounds (VOCs) with polydimethylsiloxane (PDMS) at varying temperatures was studied by gas liquid chromatography (GLC). Infinite dilution activity coefficients and specific retention volumes obtained in this study were found to be in agreement with those obtained from static headspace and group contribution methods by the authors as well as literature values for similar systems. Temperature variation also allows for transport calculations for different seasons. The results of this work confirm that PDMS is well suited for the scrubbing of VOCs from waste gas streams. Plots of specific retention volumes against temperature gave linear van-t Hoff plots.

Keywords: Specific retention volume, Waste gas streams, specific retention, infinite dilution, abatement, transport.

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Authors: A. Hematian Sourki, F. Tabatabaei Yazdi, M. Ghiafeh Davoodi, S.A. Mortazavi, M. Karimi, S.H. Razavizadegan Jahromi, A. Pourfarzad

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This study investigated the use of modified atmosphere packaging (MAP) and different packaging to extend the shelf life of Barbari flat bread. Three atmospheres including 70%CO2 and 30%N2, 50% CO2 and 50%N2 and a normal air as control were used. The bread samples were packaged in three type pouches. The shelf life was determined by appearance of mold and yeast (M +Y) in Barbari bread samples stored at 25 ± 1°C and 38 ± 2% relative humidity. The results showed that it is possible to prolong the shelf life of Barbari bread from four days to about 21 days by using modified atmosphere packaging with high carbon dioxide concentration and high-barrier laminated and vacuum bags packages. However, the hardness of samples kept in MAP increase significantly by increase of carbon dioxide concentration. The correlation coefficient (r) between headspace CO2 concentration and hardness was 0.997, 0.997 and 0.599 for A, B and C packaging respectively. High negative correlation coefficients were found between the crumb moisture and the hardness values in various packaging. There were significant negative correlation coefficients between sensory parameters and hardness of texture.

Keywords: modified atmosphere packaging, flat bread, Iranian bread, staling, correlation.

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Authors: Solvita Kampuse, Elga Berna, Sandra Muizniece-Brasava, Lija Dukalska, Irisa Murniece, Martins Sabovics, Zanda Kruma, Karina Ruse, Svetlana Sarvi, Kaspars Kampuss

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Experiments with pumpkin-rowanberry marmalade candies were carried out at the Faculty of Food Technology of the Latvia University of Agriculture. The objective of this investigation was to evaluate the quality changes of pumpkin-rowanberry marmalade candies packed in different packaging materials during the storage of 15 weeks, and to find the most suitable packaging material for prolongation of low sugar marmalade candies shelf-life. An active packaging in combination with modified atmosphere (MAP, CO2 100%) was examined and compared with traditional packaging in air ambiance. Polymer Multibarrier 60 and paper bags were used. Influence of iron based oxygen absorber in sachets of 500 cc obtained from Mitsubishi Gas Chemical Europe Ageless® on the marmalade candies’ quality was tested during shelf life. Samples of 80±5 g were packaged in polymer pouches (110 mm x 110 mm), hermetically sealed by MULTIVAC C300 vacuum chamber machine, and stored in a room temperature +21±0.5 °C. The physiochemical properties –moisture content, hardness, aw, pH, changes of atmosphere content (CO2 and O2), ascorbic acid, total carotenoids, total phenols in headspace of packs, and microbial conditions were analysed before packaging and in the 1st, 3rd , 5th, 8th, 11th and 15th weeks of storage.

Keywords: Active packaging, marmalade candies, shelf life

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Authors: Edison Muzenda

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The aim of this study was to compare the solubility of selected volatile organic compounds in water and silicon oil using the simple static headspace method. The experimental design allowed equilibrium achievement within 30 – 60 minutes. Infinite dilution activity coefficients and Henry-s law constants for various organics representing esters, ketones, alkanes, aromatics, cycloalkanes and amines were measured at 303K. The measurements were reproducible with a relative standard deviation and coefficient of variation of 1.3x10-3 and 1.3 respectively. The static determined activity coefficients using shaker flasks were reasonably comparable to those obtained using the gas liquid - chromatographic technique and those predicted using the group contribution methods mainly the UNIFAC. Silicon oil chemically known as polydimethysiloxane was found to be better absorbent for VOCs than water which quickly becomes saturated. For example the infinite dilution mole fraction based activity coefficients of hexane is 0.503 and 277 000 in silicon oil and water respectively. Thus silicon oil gives a superior factor of 550 696. Henry-s law constants and activity coefficients at infinite dilution play a significant role in the design of scrubbers for abatement of volatile organic compounds from contaminated air streams. This paper presents the phase equilibrium of volatile organic compounds in very dilute aqueous and polymeric solutions indicating the movement and fate of chemical in air and solvent. The successful comparison of the results obtained here and those obtained using other methods by the same authors and in literature, means that the results obtained here are reliable.

Keywords: Abatement, absorbent, activity coefficients, equilibrium, Henry's law constant.

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