SPME Research Papers - Academia.edu (original) (raw)

One of the factors that affect the yield of button mushrooms (Agaricus bisporus) is the quality of mushroom compost. To provide an optimal growth medium for mushrooms, it is important to understand the typical components of mushroom... more

One of the factors that affect the yield of button mushrooms (Agaricus bisporus) is the quality of mushroom compost. To provide an optimal growth medium for mushrooms, it is important to understand the typical components of mushroom compost. The aims of this study were to isolate and identify volatile organic compounds (VOCs) and investigate patterns of change in selected VOCs during the different phases of the mushroom compost production process.

The aim of this paper was to characterize the complete volatile profile of Conciato Romano cheese, a traditional Italian product aged in a mixture of olive oil, wine, and spices, and its modification during ripening, by using SPME... more

The aim of this paper was to characterize the complete volatile profile of Conciato Romano cheese, a traditional Italian product aged in a mixture of olive oil, wine, and spices, and its modification during ripening, by using SPME sampling and GC/MS analysis of volatiles and considering the rind and body parts separately. Seventy-six volatile compounds were identified, belonging to chemical classes of acids (8), aldehydes (3), alcohols (14), esters (36), ketones (9), hydrocarbons (1), and terpenes (5). Acids and esters represented the most important chemical classes and are originated from lipolysis and hydrolysis of triglycerides. Aging caused dramatic changes in volatile compounds, particularly on the cheese rind, where the amount of esters, acids, alcohols, and ketones was found particularly abundant at 8 months of aging. Interesting differences were found in volatile headspace composition depending on the external or inner parts. The higher complexity in volatile profile of aged cheese was attributed both to the aging process and tanning mixture. Sensory analysis resulted in higher perception of “sweet” and “stickiness” and significantly lower olfactory persistence in fresh product, while higher values for “salty,” “spicy,” and “persistent” were found in aged ones.

The present review aims to describe the recent and most impactful applications in pollutant analysis using solid-phase microextraction (SPME) technology in environmental, food, and bio-clinical analysis. The covered papers were published... more

The present review aims to describe the recent and most impactful applications in pollutant analysis using solid-phase microextraction (SPME) technology in environmental, food, and bio-clinical analysis. The covered papers were published in the last 5 years (2014-2019) thus providing the reader with information about the current state-of-the-art and the future potential directions of the research in pollutant monitoring using SPME. To this end, we revised the studies focused on the investigation of persistent organic pollutants (POPs), pesticides, and emerging pollutants (EPs) including personal care products (PPCPs), in different environmental, food, and bio-clinical matrices. We especially emphasized the role that SPME is having in contaminant surveys following the path that goes from the environment to humans passing through the food web. Besides, this review covers the last technological developments encompassing the use of novel extraction coatings (e.g., metal-organic frameworks, covalent organic frameworks, PDMS-overcoated fiber), geometries (e.g., Arrow-SPME, multiple monolithic fiber-SPME), approaches (e.g., vacuum and cold fiber SPME), and on-site devices. The applications of SPME hyphenated with ambient mass spectrometry have also been described.

The volatile compounds in four selected African star apple fruit (Chrysophyllum albidum) varieties were isolated and identified using the headspace solid-phase microextraction (HS-SPME) coupled with gas chromatography-mass spectrometry... more

The volatile compounds in four selected African star apple fruit (Chrysophyllum albidum) varieties were isolated and identified using the headspace solid-phase microextraction (HS-SPME) coupled with gas chromatography-mass spectrometry (GC-MS). A total of 59 compounds were identified. Application of the aroma extract dilution analysis (AEDA) to the aroma distillates from the fruits revealed 45 odour-active compounds in the flavour dilution (FD) factor range of 4-128. Among them, the highest odour activities (FD factors) were determined for methylhexanoate, acetophenone and ethyl dodecanoate. Moreover, aroma lipophilicity appears to reflect molecular conformation. Further analysis of the similarities and differences between the fruit varieties in terms of the key odourants by the application of PLS-DA and PLS-regression coefficient showed strong positive correlation between the very sweet/sweet varieties and 10 key odourants. The odourants included ethyl acetate, acetyl methyl carbinol, methylhexanoate, sabinene, p-cymene, methylbenzoate, ethylbenzoate, geraniol, cis-α-bergomotene, acetophenone, and ethyl dodecanoate.

Headspace-solid phase microextraction coupled with gas chromatography-mass spectrometry analysis were used to provide the volatile profile of roasted chickpea as a means of unravelling and elucidating roasted chickpea as a prerequisite in... more

Headspace-solid phase microextraction coupled with gas chromatography-mass spectrometry analysis were used to provide the volatile profile of roasted chickpea as a means of unravelling and elucidating roasted chickpea as a prerequisite in developing chickpea snack item for the health and functional food sectors. The results of the HS- SPME and optimization analysis using response surface methodology showed that DVB/CAR/PDMS was the most effective fibre and further results revealed the extraction temperature to be the dominant factor. A total of 61 volatile compounds were identified in the roasted chickpea. The best response within the range studied was established at 60o C extraction temperature, 30 min of equilibrium time and 15 min of extraction time. The volatile compounds iden- tified comprised of aldehydes (25%), hydrocarbons (25%), terpenoids (20%), esters (8%), ketones (8%), alcohols (8%) and heterocyclic (8%). The results further indicated that the final model was significantly (P < 0.05) fitted for the response variable (total flavour peak area) studied with a relatively high R 2 (0.9658).

This research was carried out to determine the effects of pre-rigor injection of beef semimembranosus muscle with nine proteases from plant and microbial sources, on the volatile profile of cooked beef after 1 day and 21 days post-mortem... more

This research was carried out to determine the effects of pre-rigor injection of beef semimembranosus muscle with nine proteases from plant and microbial sources, on the volatile profile of cooked beef after 1 day and 21 days post-mortem (PM) storage using Solid-phase microextraction gas chromatography mass spectrometry analysis. A total of 23 aldehydes, 5 ketones, 3 furans, 8 nitrogen and sulphur compounds, 4 alkanes, 7 alcohols and 6 terpenes were detected. Eleven volatile compounds characteristic of ginger flavour were detected in zingibain-treated meat. Benzaldehyde significantly increased (p<0.05) only in kiwifruit juice (KJ), fungal 31 protease and Asparagus protease (ASP) treated samples from 1 day to 21 days PM storage. A significant increase (p<0.05) in 3-methylbutanal was observed in KJ, bacterial and fungal protease treated samples at 21 days PM storage. Treatments with bromelain, papain, ASP, actinidin, and KJ (except KJ 21 days) proteases resulted in flavour profi...

Multiple, highly sensitive chemical techniques were used to analyze ancient pottery vessels from an excavated cemetery in Colima, west-central Mexico, dated to the Capacha phase (ca. 1500-1000 B.C). A double-chambered jar type, together... more

Multiple, highly sensitive chemical techniques were used to analyze ancient pottery vessels from an excavated cemetery in Colima, west-central Mexico, dated to the Capacha phase (ca. 1500-1000 B.C). A double-chambered jar type, together with bowl and miniature cup types, are hypothesized to have been used as a pre-Hispanic distillation still. The results from the ancient vessels were compared to those from modern replica jars of the same types in which agave had been successfully distilled to a high-alcoholic beverage. Chemical biomarkers of agave in the modern replicas were absent from the ancient vessels, as were compounds of other native natural products of the region (e.g., maize, hog plum, prickly pear, etc.). Archaeological and archaeobotanical considerations, while suggestive, also provided no definitive evidence for a pre-Hispanic distillation hypothesis. Our study is placed within a broader ancient context of how this important technology for medicines, aromatics, metal purification, and alcoholic beverages, developed in east Asia and the Middle East, later to be adopted in Europe and brought to the New World. While an independent invention of a distillation apparatus in Mexico is yet to be proved, our goal is to stimulate further research and discussion, possibly leading to more compelling evidence.

Muchas decisiones importantes se basan en los resultados de análisis químicos, es el caso de la estimación de rendimientos ó de verificación de especificaciones o límites legales de materiales. Debido a esto cada vez hay mayor presión... more

Muchas decisiones importantes se basan en los resultados de análisis químicos, es el caso de la estimación de rendimientos ó de verificación de especificaciones o límites legales de materiales. Debido a esto cada vez hay mayor presión sobre los químicos para demostrar la calidad de sus resultados y su aptitud para el uso. Uno de los principales parámetros metrológicos que demuestra esta capacidad, es la incertidumbre de la medición. Su estimación no es una tarea fácil debido a los múltiples factores que influyen en su cálculo, para lo cual se requiere un buen conocimiento en metrología y de algunos conceptos estadísticos. En este estudio se evaluó la incertidumbre en el análisis de Hidrocarburos Aromáticos Policíclicos en muestras de agua natural y potable, en un método para el prestador del servicio de agua potable en el Valle de Aburrá (Colombia), que utiliza la técnica de preparación de muestra por microextracción en fase sólida (SPME) automática por inmersión, y su posterior separación y detección por cromatografía de gases con detector selectivo de masas. Este trabajo da respuesta a este requisito, establecido en la norma ISO-IEC 17025 para la acreditación de laboratorios de ensayo.

Understanding the aroma profile of wines made from cold climate grapes is needed to help winemakers produce quality aromatic wines. The current study aimed to add to the very limited knowledge of aroma-imparting compounds in wines made... more

Understanding the aroma profile of wines made from cold climate grapes is needed to help winemakers produce quality aromatic wines. The current study aimed to add to the very limited knowledge of aroma-imparting compounds in wines made from the lesser-known Frontenac and Marquette cultivars. Headspace solid-phase microextraction (SPME) and gas chromatography-mass spectrometry (GC-MS) with simultaneous olfactometry was used to identify and quantify selected, aroma-imparting volatile organic compounds (VOC) in wines made from grapes harvested at two sugar levels (22 • Brix and 24 • Brix). Aroma-imparting compounds were determined by aroma dilution analysis (ADA). Odor activity values (OAV) were also used to aid the selection of aroma-imparting compounds. Principal component analysis and hierarchical clustering analysis indicated that VOCs in wines produced from both sugar levels of Marquette grapes are similar to each other, and more similar to wines produced from Frontenac grapes har...

Speciation analysis by solid phase microextraction (SPME) is explored for the pesticide atrazine in an aqueous dispersion of model latex nanoparticles. It is found that the rate of extraction is governed by coupled diffusion of free and... more

Speciation analysis by solid phase microextraction (SPME) is explored for the pesticide atrazine in an aqueous dispersion of model latex nanoparticles. It is found that the rate of extraction is governed by coupled diffusion of free and particle-bound analyte towards the solid/solution interface. The nanoparticles do not enter the solid phase: the eventual equilibrium analyte concentration in the solid phase is dictated by the parti tion coefficient k wf and the concentration of the free analyte in the sample solution. The rate of release of atrazine from the latex particles is fast on the effective time scale of the microextraction process. All together, the results indicate that SPME has the potential of developing into a powerful technique for dynamic speciation analysis of organic compounds in aqueous media.

Naphthalene is a volatile solid that often has been used as a pesticide to treat artifacts, particularly ethnographic material, and natural history col-lections. Naphthalene residues pose an ongoing health risk in museums and to... more

Naphthalene is a volatile solid that often has been used as a pesticide to treat artifacts, particularly ethnographic material, and natural history col-lections. Naphthalene residues pose an ongoing health risk in museums and to communities that receive contaminated artifacts through cultural repatriation. The Museum of the American Indian disposed of its supply of "moth flakes" in 1985, but noxious residues remain on collections. It has been demonstrated that naphthalene vapors become stronger in humid air, which increases the potential health risk. A method for quantifying naphthalene vapor concentrations using SPME-GC/FID is pre-sented, and the relationship between naphthalene, water vapor, and textile fibers is explored as a step in the development of a treatment to remediate the pesticide residues.

... Over the past few years, method based on headspace solid phase microextraction (HS-SPME) has been used extensively in the analysis of volatile compounds in fruits (Chen et al., 2005, Kourkoutas et al., 2006 and Riu-Aumatell et al.,... more

... Over the past few years, method based on headspace solid phase microextraction (HS-SPME) has been used extensively in the analysis of volatile compounds in fruits (Chen et al., 2005, Kourkoutas et al., 2006 and Riu-Aumatell et al., 2004). ... Joseph, MI, USA) was used. ...

The composition of the essential oil of the endemic Viola etrusca Erben from Monte Labbro (Italy) has been studied for the first time. It was made up almost exclusively of methyl salicylate (96%), together with many other mono- and... more

The composition of the essential oil of the endemic Viola etrusca Erben from Monte Labbro (Italy) has been studied for the first time. It was made up almost exclusively of methyl salicylate (96%), together with many other mono- and sesquiterpenes and non-terpenic alcohols and aldehydes. In addition, the SPME technique has been used to evaluate the volatiles emitted in vivo by different-coloured flowers. Copyright © 2002 John Wiley & Sons, Ltd.

Colony integrity and survival in honeybees is regulated by chemical signals that are actively produced by glands and syner-gically transmitted between the members. A number of these signals regulate the typical age-related division of... more

Colony integrity and survival in honeybees is regulated by chemical signals that are actively produced by glands and syner-gically transmitted between the members. A number of these signals regulate the typical age-related division of labor among the worker bees performing different tasks at different ages. In this study, the analysis of the cuticular profiles in Apis mellifera ligus-tica Spinola, 1806 workers at various tasks (newly emerged, nurse and forager bees) was performed using in vivo solid-phase microextraction gas chromatography-mass spectrometry (SPME-GC-MS). The use of in vivo SPME shed new light on the complexity of the molecular pattern on the epicuticle of honeybees. The identified molecules are mainly hydrocarbons, saturated and unsaturated carboxylic acids, and to a less extent, esters, sterols, aldehydes, and alcohols. Their relative abundance between the three task groups was evaluated using descriptive statistics and multivariate pattern recognition analysis (i.e., principal component analysis, PCA, and linear discriminant analysis, LDA). Eleven molecules namely nonacosane, pentacosane, (Z)-12-penta-cosene, 11-tricosene, 11-methylnonacosane, squalene, 13-methyl-heptacosane, heptacosane, heneicosane, docosane and tricosane, occur with high frequency in newly emerged, nurse, and forager bees. The compounds that contributed the most for the separation of the three task groups in the PCA were pentacosane, (Z)-12-pen-tacosene, 13-methylheptacosane and squalene; while for LDA, nonacosane, 11-methylnonacosane and pentacosane were the molecules that contributed most to the discrimination.

This review highlights developments of Solid Phase MicroExtraction in toxins analysis after 2005. It covers the major mycotoxins such as aflatoxins and ochratoxins where applications have been reported in the literature and some... more

This review highlights developments of Solid Phase MicroExtraction in toxins analysis after 2005. It covers the major mycotoxins such as aflatoxins and ochratoxins where applications have been reported in the literature and some cyanobacteria toxins. Solid Phase MicroExtraction can act as an important sampling and sample preparation tool for the analysis of toxins in various matrices expanding its existing broad spectrum of analytes.

We investigated the new solid-phase microextraction method by high-performance liquid chromatography with electrochemical detection for the analysis of biogenic amines. The Carbowax–Templated Resin 50 mm (purple) fibre coating 21 offers... more

We investigated the new solid-phase microextraction method by high-performance liquid chromatography with electrochemical detection for the analysis of biogenic amines. The Carbowax–Templated Resin 50 mm (purple) fibre coating 21 offers good performances for dopamine and serotonin separation, i.e., good selectivity and high sensibility (0.1 mg l). We also tested this fibre for biogenic amines quantification of rat striatum. The coating seems to be selective towards the amines and has low affinity for the metabolites, allowing a good separation and preventing drawbacks from the biological matrix. These first results obtained using this original separation method offer large perspectives of application to many biological samples. 

Naphthalene is a volatile solid that often has been used as a pesticide to treat artifacts, particularly ethnographic material, and natural history collections. Naphthalene residues pose an ongoing health risk in museums and to... more

Naphthalene is a volatile solid that often has been
used as a pesticide to treat artifacts, particularly
ethnographic material, and natural history collections.
Naphthalene residues pose an ongoing
health risk in museums and to communities that
receive contaminated artifacts through cultural
repatriation. The Museum of the American Indian
disposed of its supply of “moth flakes” in 1985, but
noxious residues remain on collections. It has been
demonstrated that naphthalene vapors become
stronger in humid air, which increases the potential
health risk. A method for quantifying naphthalene
vapor concentrations using SPME-GC/FID is presented,
and the relationship between naphthalene,
water vapor, and textile fibers is explored as a step
in the development of a treatment to remediate the
pesticide residues.

Cadaver-detection dogs are a preferred search tool utilised by law enforcement agencies for the purposes of locating victim remains due to their efficiency and minimal disturbance to the crime scene. In Australia, a specific group of... more

Cadaver-detection dogs are a preferred search tool utilised by law enforcement agencies for the purposes of locating victim remains due to their efficiency and minimal disturbance to the crime scene. In Australia, a specific group of these canines are blood-detection dogs, which are trained to detect and locate blood evidence and search potential crime scenes in cases where a cadaver may not be present. Their role sometimes requires searches to be carried out after considerable time has passed since the crime occurred, and this is important for developing effective training protocols. This study aimed to investigate the volatile organic compounds (VOCs) produced from fresh and aged human blood on various surfaces. Solid phase microextraction (SPME) was used to extract VOCs from the headspace of dried blood samples aged and sampled periodically over 12 months from a non-porous (i.e. aluminium) and porous (i.e. cotton) surface. Samples were analysed using comprehensive two-dimensional...

Macquarie University ResearchOnline.

In the present study a new method involving extraction by SPME fibers and storage in an organic solvent is described and tested in an ant species, Dinoponera quadriceps. The results demonstrate that the cuticular hydrocarbons trapped by... more

In the present study a new method involving extraction by SPME fibers and storage in an organic solvent is
described and tested in an ant species, Dinoponera quadriceps. The results demonstrate that the cuticular
hydrocarbons trapped by SPME fibers can be efficiently desorbed from the fibers to hexane and stored for
later analysis. This method can be used as an alternative procedure for the collection of samples in field
studies. This technique is an effective non-lethal method for the extraction of cuticular hydrocarbons
and was developed specifically for the long-term monitoring of individuals, as well as for situations in
which gas chromatography equipment is unavailable at the sampling site.

A novel extraction technique was reported. The solid phase material, nanofiber, was prepared by electrospinning using polystyrene. Twenty different drugs (10 lg/L in water) were extracted using 1 mg of nanofibers within 5 min. The... more

A novel extraction technique was reported. The solid phase material, nanofiber, was prepared by electrospinning using polystyrene. Twenty different drugs (10 lg/L in water) were extracted using 1 mg of nanofibers within 5 min. The analytes can be desorpted from the fibers with 50 lL of the methanol and then monitored by LC coupled to a UV detector. Packed-fiber SPE (PFSPE) provide high recoveries (A50%) for some relatively non-polar drugs (log P A1.5) (n-octanol-to-water partition ratio), and relatively low recoveries (9.9–39.8%) for the drugs within the log P window below 1. Experimental optimization of the technique has been carried out using seven representative drugs, edaravone, cinchonine, quinine, voriconazole, chlordiazepoxide, verapamil, and rutonding. Except for edaravone, the maximum yields of seven drugs (0.2 lg/L) from water samples were approximately 100%, and were 33.7–88.2% from human plasma. The advantageous aspect of the technique encompasses high throughput, high sensitivity, simplicity, low cost, and green chemistry.