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SPME StableFlex fiber assortment kit; Kit 1- For Volatile or Semivolatiles. Bulk and Prepack available at Sigmaaldrich.com.

SPME StableFlex™ fiber assortment kit for use with manual holder | Sigma-Aldrich

SPME StableFlex<SUP>™</SUP> fiber assortment kit

The presence of (±)α-pinene, (+)β-pinene, (+)3-carene, and R-(+)limonene terpenes in wastewater of a citrus transformation factory was detected and analyzed, in a previous study, by using Solid Phase Micro-extraction (SPME) followed by GC analyses. Purpose of that research was to compare the genotoxic responses of mixtures of terpenes with the genotoxicity of the individual compounds, and the biological effects of actual wastewater. Genotoxicity was evaluated in the Salmonella reversion assay (Ames test) and in V79 cells by Comet assay. Ames tests indicated that the four single terpenes did not induce an increase of revertants frequency. On the contrary, the mixtures of terpenes caused, in the presence of metabolic activation, a highly significant increase of the revertants in TA100 strain in comparison to the control. The Comet assay showed a significant increase in DNA damage in V79 cells treated for 1h with single or mixed terpenes. Moreover, the actual wastewater was found highly genotoxic in bacterial and mammalian cells. Photocatalytic tests completely photodegraded the pollutants present in aqueous wastewater and the initial high genotoxicity of samples of wastewater collected during the photocatalytic run, was completely lose in 3h of irradiation.

Genotoxicity of citrus wastewater in prokaryotic and eukaryotic cells and efficiency of heterogeneous photocatalysis by TiO(2).

Solid phase micro extraction (SPME) was applied to the determination of selected trihalomethanes (THMs), chloroform, bromodichloromethane, dibromochloromethane, bromoform, in potable and recreational waters. The selected samples were environmentally significant due to mandatory limits imposed by regulatory agencies. Extraction of the analytes was performed using headspace SPME (fused silica fibre with a 100 microm poly(dimethylsiloxane coating) followed by thermal desorption at 220 degrees C and GC-MS analysis. A linear working range of 10-160 microg/l was established with relative standard deviations (%RSD) within the range, 0.9-19%. Limits of detection (LOD) were 1.0-2.8 microg/l. The highest THM concentration was 61.8 microg/l which was well within the proposed European Union directive of 100 microg/l. The total THMs determined in swimming pool waters ranged from 105-134 microg/l, with chloroform accounting for 84-86% of total THM.

Measurement of trihalomethanes in potable and recreational waters using solid phase micro extraction with gas chromatography-mass spectrometry.

Worldwide, tuberculosis (TB) kills nearly 2 million people annually, yet rapid diagnosis still relies on a 100-year-old method of sputum staining for acid-fast bacilli. The advent of solid phase micro-extraction and gas chromatography/mass spectrometry makes it possible to systematically investigate whether volatile metabolites from organisms belonging to the genus Mycobacterium can be used as a rapid and highly selective alternative to the traditional diagnostic methods. We have identified four specific compounds (methyl phenylacetate, methyl p-anisate, methyl nicotinate and o-phenylanisole) from Mycobacterium tuberculosis and Mycobacterium bovis cultures grown in vitro that are distinctive volatile markers. These compounds are detectable before the visual appearance of colonies, potentially useful as the basis of a non-invasive diagnostic test for TB and have characteristic odors.

The scent of Mycobacterium tuberculosis.

A powerful technique was developed for the identification and quantification of 9 volatile compounds of beer, using headspace solid phase micro-extraction (HS/SPME) and gas chromatograph coupled to a mass spectrometer and a flame ionization detector (GC/MS/FID). Optimized parameters included type of fiber, desorption time, and exposure time. Optimization was achieved with standard solutions of the target compounds. All samples were analyzed in triplicate. An exposure time of 45 min with PDMS fiber in the sample headspace was enough to reach equilibrium of the phases. A desorption time of 15 min in the gas chromatograph injector was enough for the fiber to desorb the target compounds. It was found that less polar compounds were more readily absorbed by the fiber (for example, isoamyl acetate) than more polar compounds (for example, acetaldehyde), under the extraction conditions, due to the nature of the fiber. Extraction conditions are important criteria to perform a good quantification of volatile compounds. Concentrations found in sampled beer, for the compounds of interest, ranged between 0.32 and 41.7 ppm. Results show that the reproducibility of the technique depends on the compounds. Esters have higher values (RSD mean value 5.05%) than higher alcohols (RSD mean value 2.5%) and aldehydes (RSD 3.7%). The simplicity of the validated methodology enables its use as a regular quality control procedure for beer flavor analysis. This study describes a technique successfully used to identify and quantify volatiles of interest in beer that can be used for quality control purposes under normal brewery production conditions. The technique uses a gas chromatograph coupled to a mass spectrometer with a flame ionization detector.

Beer volatile analysis: optimization of HS/SPME coupled to GC/MS/FID.

2-Methoxy-3-isobutylpyrazine (MIBP) contributes a bell pepper aroma to many grape cultivars and has a reported aroma threshold of ∼2 ng L(-1) in water. The purpose of this study was twofold: (1) develop a procedure using headspace solid phase micro-extraction combined with GC-MS in the selected ion monitoring mode (HS-SPME-GC-MS-SIM) for analysis of MIBP in grape berries, and (2) determine the location of MIBP biosynthesis in grapevines by approach grafting clusters of Vitis vinifera L. cvs Cabernet Sauvignon and Muscat blanc onto each other. The soluble solids and pH of the grape juice/homogenate matrix from different grape berry developmental stages influenced the method precision; therefore, quantification via the method of standard addition was used. Using our developed method, the limit of detection (LOD) and limit of quantitation (LOQ) of MIBP were 0.1 ng L(-1) and 2 ng L(-1), respectively, measured in a model juice and non-MIBP containing Chardonnay juice. Spiked recoveries averaged between 91% and 112% in Cabernet Sauvignon and Pinot noir homogenates and the overall relative standard deviation was less than 10%. The method was used to analyze MIBP in 29 grape cultivars and in fruit from clusters grafted to Cabernet Sauvignon or Muscat vines. Quantifiable levels were found only in Cabernet franc, Cabernet Sauvignon, Merlot, Sauvignon blanc and Semillon, providing information on the genetic connection for the occurrence of MIBP in grapes. No MIBP was detected in the berries of Muscat blanc clusters grafted onto Cabernet Sauvignon vines when sampled at fruit maturity. MIBP was detected in all berries of Cabernet Sauvignon regardless the graft configuration. The data indicate that MIBP or its precursors originate in the berry and its formation depends upon grape genotype.

2-Methoxy-3-isobutylpyrazine in grape berries and its dependence on genotype.

The influence of vine training and sunlight exposure on the 3-alkyl-2-methoxypyrazines contents in musts and wines was studied by means of two previously reported methods based on headspace solid-phase micro-extraction. Experimental samples were monitored throughout grape ripening and wine making. 3-Isobutyl-2-methoxypyrazine, 3-sec-butyl-2-methoxypyrazine and 3-isopropyl-2-methoxypyrazine were identified. The 3-isobutyl-2-methoxypyrazine content decreased throughout grape ripening in all of the sample types studied. After 1 day of maceration with the skins, there was an increase, but after racking, no further increase was observed. No significant differences between samples were found during grape ripening. Wines from goblet-trained vines, however, contained significantly less 3-isobutyl-2-methoxypyrazine. Clusters protected from sunlight since the beginning of the veraison resulted in wines with a significantly lower content of this compound than the control samples.

Influence of vine training and sunlight exposure on the 3-alkyl-2-methoxypyrazines content in musts and wines from the Vitis vinifera variety cabernet sauvignon.

Physical properties of whey protein isolate (WPI) coating solution incorporating ascorbic palmitate (AP) and alpha-tocopherol (tocopherol) were characterized, and the antioxidant activity of dried WPI coatings against lipid oxidation in roasted peanuts were investigated. The AP and tocopherol were mixed into a 10% (w/w) WPI solution containing 6.7% glycerol. Process 1 (P1) blended an AP and tocopherol mixture directly into the WPI solution using a high-speed homogenizer. Process 2 (P2) used ethanol as a solvent for dissolving AP and tocopherol into the WPI solution. The viscosity and turbidity of the WPI coating solution showed the Newtonian fluid behavior, and 0.25% of critical concentration of AP in WPI solution rheology. After peanuts were coated with WPI solutions, color changes of peanuts were measured during 16 wk of storage at 25 degrees C, and the oxidation of peanuts was determined by hexanal analysis using solid-phase micro-extraction samplers and GC-MS. Regardless of the presence of antioxidants in the coating layer, the formation of hexanal from the oxidation of peanut lipids was reduced by WPI coatings, which indicates WPI coatings protected the peanuts from oxygen permeation and oxidation. However, the incorporation of antioxidants in the WPI coating layer did not show a significant difference in hexanal production from that of WPI coating treatment without incorporation of antioxidants.

Coating of peanuts with edible whey protein film containing alpha-tocopherol and ascorbyl palmitate.

To identify the volatile organic compounds (VOCs) in lung cancer tissue and lung cancer cell lines. The lung cancer tissue samples from 18 patients were cultured and 4 lung cell lines (A549, NCI-H446, SK-MES-1, BEAS-2B) were also included in the study. Air samples in the headspace of culture flasks were analyzed for VOCs with solid-phase micro-extraction and gas chromatography-mass spectroscopy technique (SPME-GC/MS). Two kinds of VOCs 2-pentadecanone and nonadecane were detected in lung cancer cell lines A549, NCI-H446 and SK-MES-1. The concentration of 2-pentadecanone were (1.382 + or -0.171) X 10(-5)mg/L, (1.681 + or - 0.190) X 10(-4)mg/L and (2.835 + or - 0.401) X 10(-6)mg/L, respectively; the concentrations of nonadecane were (8.382 + or - 0.606 ) X 10(-6)mg/L, (1.845 + or - 0.130) X 10(-5)mg/L and (6.220 + or - 0.362) X 10(-6)mg/L), respectively. The eicosane was detected in A549 and NCI-H446 with the concentration of (8.313 + or - 1.130) X 10(-6)mg/L and (1.020 + or - 0.141) X 10(-5)mg/L), respectively. All the 3 VOCs were not detected in cell line BEAS-2B. The concentrations of 12 VOCs including decane, 2- pentadecanone, nonadecane and eicosane were high in 18 lung cancer tissue samples; the concentrations of 2-pentadecanone were 5.421 X 10(-6)mg/L-3.621 X 10(-5)mg/L,those of nonadecane were 5.805 X 10(-6)mg/L-1.830 X 10(-5)mg/L, those of eicosane were 2.730 X 10(-6)mg/L-2.343 X 10(-5)mg/L. There were no differences of VOCs levels among patients with different cancer differentiation (P>0.05). The concentration of eicosane in the non-squamous carcinoma was higher than that in squamous carcinoma, the same results were confirmed in the lung cancer cell lines. This study has identified VOCs produced by lung cancer tissue, which may support to use breath test as a complementary noninvasive diagnostic method for lung cancer.

[Determination of volatile organic compounds in lung cancer cell lines and lung cancer tissue].

Pseudomonas aeruginosa infections are associated with progressive life threatening decline of lung function in cystic fibrosis sufferers. Growth of Ps. aeruginosa releases a "grape-like" odour that has been identified as the microbial volatile organic compound 2-aminoacetophenone (2-AA). We investigated 2-AA for its specificity to Ps. aeruginosa and its suitability as a potential breath biomarker of colonisation or infection by Solid Phase Micro Extraction and Gas Chromatography-Mass Spectrometry (GC/MS). Cultures of 20 clinical strains of Ps. aeruginosa but not other respiratory pathogens had high concentrations of 2-AA in the head space of in vitro cultures when analysed by GC/MS. 2-AA was stable for 6 hours in deactivated glass sampling bulbs but was not stable in Tedlar® bags. Optimisation of GC/MS allowed detection levels of 2-AA to low pico mol/mol range in breath. The 2-AA was detected in a significantly higher proportion of subjects colonised with Ps. aeruginosa 15/16 (93.7%) than both the healthy controls 5/17 (29%) (p < 0.0002) and CF patients not colonised with Ps. aeruginosa 4/13(30.7%) (p < 0.001). The sensitivity and specificity of the 2-AA breath test compared to isolation of Ps. aeruginosa in sputum and/or BALF was 93.8% (95% CI, 67-99) and 69.2% (95% CI, 38-89) respectively. The peak integration values for 2-AA analysis in the breath samples were significantly higher in Ps. aeruginosa colonised subjects (median 242, range 0-1243) than the healthy controls (median 0, range 0-161; p < 0.001) and CF subjects not colonised with Ps. aeruginosa (median 0, range 0-287; p < 0.003). Our results report 2-AA as a promising breath biomarker for the detection of Ps. aeruginosa infections in the cystic fibrosis lung.

2-Aminoacetophenone as a potential breath biomarker for Pseudomonas aeruginosa in the cystic fibrosis lung.

A novel activated carbon coating fiber used for solid phase micro-extraction (SPME) was prepared using activated carbon powder and silica resin adhesive. The extraction properties of the novel activated carbon coating fiber were investigated. The results indicate that this coating fiber has high concentration ability, with enrichment factors for chloroform, carbon tetrachloride, trichloroethylene and tetrachloroethylene in the range of 13.8 to 18.7. The fiber is stable at temperature as high as 290 degrees C and it can be used for over 140 times at 250 degrees C. The activated carbon coating fiber was then applied to the analysis of the four halocarbon compounds mentioned above. A linear correlation with correlation coefficients between 0.995 2 and 0.999 4 and the detection limits between 0.008 and 0.05 microg/L were observed. The method was also applied to a real water sample analysis and the recoveries of these halocarbon compounds were from 95.5% to 104.6%.

[Preparation of a novel activated carbon coating fiber for solid phase micro-extraction and its application for halocarbon compound analysis in water].

The purpose of this study was to determine whether volatile organic compounds specific to Pseudomonas aeruginosa could be detected in clinical sputum specimens. Patients were recruited from specialist bronchiectasis and cystic fibrosis clinics. The gold standard for diagnosing Ps. aeruginosa infection was a positive sputum culture. About 72 sputum headspace samples taken from patients at risk of or known to have prior Ps. aeruginosa infection were analysed by solid phase micro-extraction mass spectrometry. 2-nonanone was a marker in Ps. aeruginosa in sputum headspace gas with sensitivity of 72% and specificity of 88%. A combination of volatile compounds, a sputum library of 17 compounds with 2-nonanone, increased sensitivity in the detection of Ps. aeruginosa to 91% with specificity of 88%. In contrast to the 48-hour turnaround for classical microbiological culture, these results were available within 1-2 h. These data demonstrate the potential for rapid and accurate diagnosis of Ps. aeruginosa infection from sputum samples. 2-Nonanone is a compound requiring further study in the exhaled breath as it may improve diagnostic of Ps. aeruginosa infection when combined with other reported volatile markers.

Volatile biomarkers of Pseudomonas aeruginosa in cystic fibrosis and noncystic fibrosis bronchiectasis.

The volatile constituents of the essential oil of wild Melissa officinalis L. obtained from the Kurdistan province of Iran were extracted by headspace/solid-phase micro-extraction and were analysed by gas chromatography and gas chromatography/mass spectrometry. Of a total of 14 compounds in the oil, 12 (85.7%) were identified. The main components were as follows: (E)-citral (37.2%), neral (23.9%) and citronellal (20.3%). Some physicochemical properties, such as the logarithm of calculated octanol-water partitioning coefficients (log K (ow))(,) total biodegradation (TB (d) in mol h(-1) and g h(-1)), water solubility (S (w), mg L(-1) at 25°C) and median lethal concentration 50 (LC(50)), were calculated for compounds 1-14 from M. officinalis L.

Chemical composition analysis of the essential oil of Melissa officinalis L. from Kurdistan, Iran by HS/SPME method and calculation of the biophysicochemical coefficients of the components.

The headspace solid-phase micro-extraction technique with on-fibre derivatisation followed by gas chromatography-tandem mass spectrometry has been evaluated for the analysis of 1,3-dichloro-2-propanol in water. An asymmetric factorial design has been performed to study the influence of five experimental factors: extraction time and temperature, derivatisation time and temperature and pH. The best extraction performance is achieved in the headspace mode, with 5 mL stirred water samples (pH 4) containing 1.3 g of NaCl, equilibrated for 30 min at 25 degrees C, using divinylbenzene-carboxen-polydimethylsiloxane as the fibre coating. On-fibre derivatisation has been used for the first time with 50 microL of bis(trimethylsilyl)trifluoroacetamide at 25 degrees C during 15 min, leading to effective yields. The proposed method provides high sensitivity, good linearity and repeatability (relative standard deviation of 5.1% for 10 ng mL(-1) and n = 5). The limits of detection and quantification were 0.4 and 1.4 ng mL(-1), respectively. Analytical recoveries obtained for different water samples were approx. 100%.

Solid-phase micro-extraction procedure for the determination of 1,3-dichloro-2-propanol in water by on-fibre derivatisation with bis(trimethylsilyl)trifluoroacetamide.

The complex molecular assemblages were analysed in the soil gas phase after applying pine forest wastes (PFW) or sugarbeet vinasses (SBV) for soil-borne crop pests' management. For this purpose, solid-phase micro-extraction (SPME) and gas chromatography (GC) were used coupled with mass spectrometry (MS). The organic wastes were applied either to Calcic Entisol or Haplic Arenosol moistened at field capacity and soil was covered with polyethylene sheet for 28-30 days to retain the volatiles. The PFW-treated soil mainly released volatile terpene hydrocarbons (trans-caryophyllene, beta-myrcene and p-cymene), with alpha-humulene and ethylbenzotriazole prevailing in the untreated soil. After SBV application mainly alkyl compounds and alkylbenzenes were released, whereas cyclohexanone, limonene, butanone, acetic acid, camphor and benzaldehyde occurred in the untreated soil. Compound assemblages also depended on the increasing water saturation in terms of soil depth, with sulphur compounds prevailing in deep horizons. Our results showed that SPME can be directly applied to soils to provide valuable information on volatile products from organic amendments.

Solid-phase micro-extraction (SPME) in the early detection of potentially active volatile compounds from organic wastes used for the management of soil-borne pathogens.

The occurrence of methional in fresh orange juice, and possible occurrence of beta-damascenone in heated orange juice, has been previously suggested. Here we report on the occurrence of 2-methyl-3-furanthiol in the headspace, collected by solid-phase micro-extraction, of fresh, pasteurized, and stored orange juice. The contents of 2-methyl-3-furanthiol and methional were quantified, and the relative level of beta-damascenone was estimated, in the headspace of fresh, pasteurized, and stored orange juices using the nasal impact frequency (NIF) and surface of NIF (SNIF) GC-Olfactometry procedure. 2-Methyl-3-furanthiol concentrations were 2 ng/L in fresh and pasteurized Shamuti orange juice, and 270 ng/L in stored juice of the same variety. Methional concentrations were 550, 830, and 11,550 ng/L in fresh, pasteurized, and stored pasteurized juices, respectively. beta-Damascenone content appeared to have increased during pasteurization and storage. Aroma-similarity experiments strongly suggest that 2-methyl-3-furanthiol and methional, at the levels found in stored orange juice (21 days at 35 degrees C), contribute to stored orange juice off-flavor.

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