Development of a headspace solid-phase microextraction procedure for the determination of free volatile fatty acids in waste waters

Ábalos, Manuela; Bayona, Josep M.; Pawliszyn, Janusz

doi:10.1016/s0021-9673(99)01263-7

Cited by 103 publications

(58 citation statements)

References 27 publications

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“…Total dissolved organic carbon concentrations were determined by catalytic high-temperature combustion using a Shimadzu TOC-V CPH carbon analyzer (Shimadzu USA, Columbia, MD). Acetate concentrations in water samples were determined by solid-phase microextraction/gas chromatography using a method adapted from the method of Á balos et al (1). Briefly, volatile fatty acids in an acidified pore water sample were adsorbed to a Carbo-Wax fused-silica fiber and injected into an HP 6890 gas chromatograph equipped with a 30-m NUKOL capillary column and a flame ionization detector; quantification was achieved by comparison with volumetric standards of sodium acetate.…”

Section: Methodsmentioning

confidence: 99%

Salinity Constraints on Subsurface Archaeal Diversity and Methanogenesis in Sedimentary Rock Rich in Organic Matter

Waldron

Petsch

Martini

et al. 2007

Appl Environ Microbiol

116

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The diversity of microorganisms active within sedimentary rocks provides important controls on the geochemistry of many subsurface environments. In particular, biodegradation of organic matter in sedimentary rocks contributes to the biogeochemical cycling of carbon and other elements and strongly impacts the recovery and quality of fossil fuel resources. In this study, archaeal diversity was investigated along a salinity gradient spanning 8 to 3,490 mM Cl ؊ in a subsurface shale rich in CH 4 derived from biodegradation of sedimentary hydrocarbons. Shale pore waters collected from wells in the main CH 4 -producing zone lacked electron acceptors such as O 2 , NO 3 ؊ , Fe 3؉ , or SO 4 2؊ . Acetate was detected only in high-salinity waters, suggesting that acetoclastic methanogenesis is inhibited at Cl ؊ concentrations above ϳ1,000 mM. Most-probable-number series revealed differences in methanogen substrate utilization (acetate, trimethylamine, or H 2 /CO 2 ) associated with chlorinity. The greatest methane production in enrichment cultures was observed for incubations with salinity at or close to the native pore water salinity of the inoculum. Restriction fragment length polymorphism analyses of archaeal 16S rRNA genes from seven wells indicated that there were links between archaeal communities and pore water salinity. Archaeal clone libraries constructed from sequences from 16S rRNA genes isolated from two wells revealed phylotypes similar to a halophilic methylotrophic Methanohalophilus species and a hydrogenotrophic Methanoplanus species at high salinity and a single phylotype closely related to Methanocorpusculum bavaricum at low salinity. These results show that several distinct communities of methanogens persist in this subsurface, CH 4 -producing environment and that each community is adapted to particular conditions of salinity and preferential substrate use and each community induces distinct geochemical signatures in shale formation waters.

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Section: Methodsmentioning

confidence: 99%

Salinity Constraints on Subsurface Archaeal Diversity and Methanogenesis in Sedimentary Rock Rich in Organic Matter

Waldron

Petsch

Martini

et al. 2007

Appl Environ Microbiol

116

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“…Since the first SPME fibres became commercially available, it has been more and more used and the fields of application have been continuously growing, including a wide range of food analysis, namely the volatile composition of wines [18][19][20][21][22], beers [23,24], whiskys [25][26][27] and several kinds of fruits [28][29][30][31], clinical chemistry [32], environmental chemistry [33,34] and pharmaceutical analysis [35,36], with nowadays about 3000 research papers published.…”

Section: Introductionmentioning

confidence: 99%

Development of a dynamic headspace solid-phase microextraction procedure coupled to GC–qMSD for evaluation the chemical profile in alcoholic beverages

Rodrigues

Caldeira

Câmara

2008

Analytica Chimica Acta

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t r a c tIn the present study, a simple and sensitive methodology based on dynamic headspace solidphase microextraction (HS-SPME) followed by thermal desorption gas chromatography with quadrupole mass detection (GC-qMSD), was developed and optimized for the determination of volatile (VOCs) and semi-volatile (SVOCs) compounds from different alcoholic beverages:wine, beer and whisky. Key experimental factors influencing the equilibrium of the VOCs and SVOCs between the sample and the SPME fibre, as the type of fibre coating, extraction time and temperature, sample stirring and ionic strength, were optimized. The performance of five commercially available SPME fibres was evaluated and compared, namely polydimethyl- An objective comparison among different alcoholic beverages has been established in terms of qualitative and semi-quantitative differences on volatile and semi-volatile compounds. These compounds belong to several chemical families, including higher alcohols, ethyl esters, fatty acids, higher alcohol acetates, isoamyl esters, carbonyl compounds, furanic compounds, terpenoids, C13-norisoprenoids and volatile phenols. The optimized extraction conditions and GC-qMSD, lead to the successful identification of 44 compounds in white wines, 64 in beers and 104 in whiskys. Some of these compounds were found in all of the examined beverage samples.The main components of the HS-SPME found in white wines were ethyl octanoate (46.9%), ethyl decanoate (30.3%), ethyl 9-decenoate (10.7%), ethyl hexanoate (3.1%), and isoamyl octanoate (2.7%). As for beers, the major compounds were isoamyl alcohol (11.5%), ethyl octanoate (9.1%), isoamyl acetate (8.2%), 2-ethyl-1-hexanol (5.9%), and octanoic acid (5.5%).Ethyl decanoate (58.0%), ethyl octanoate (15.1%), ethyl dodecanoate (13.9%) followed by 3-methyl-1-butanol (1.8%) and isoamyl acetate (1.4%) were found to be the major VOCs in whisky samples.

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“…[27][28][29][30][31][32] Headspace SPME (HS--SPME) has been previously reported for determination of short chain volatile fatty acids, including the C 2 --C 7 carbon chain or their ethyl esters from waste water. 33,34 However, extraction of long chain fatty acids in biological and nutrition analysis is a very challenging goal due to their hydrophobicity, perceived abundance as plasticizers, ubiquity in the environment, great tendency to bioconcentrate, vast distribution in conjugated forms in cellular structure, very high affinity to biological proteins such as albumin, and a high risk of matrix effect encounters. The main goal of this study is to address the above mentioned challenges for unbiased high throughput quantification of "total" and "free" concentration of nonesterified fatty acids in the complex biological media via optimization and validation of a SPME assay followed by HPLC--ESI--MS.…”

mentioning

confidence: 99%

Application of Solid Phase Microextraction for Quantitation of Polyunsaturated Fatty Acids in Biological Fluids

et al. 2014

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Development of a straightforward strategy for simultaneous quantitative analysis of nonesterified fatty acids (NEFA) species in biofluids is a challenging task because of the extreme complexity of fatty acid distribution in biological matrices. In this study, we present a direct immersion solid phase microextraction method coupled to liquid chromatography--mass spectrometry platform (DI--SPME--HPLC--ESI --MS ) for determination of unconjugated fatty acids (FA) in fish and human plasma. The proposed method was fully validated according to bioanalytical method validation guidelines. The LOD and LOQ were in the range of 0.5--2 and 5--12 ng/ml, respectively, with a linear dynamic range of 100 fold for each compound. Absolute and relative matrix effects were comprehensively evaluated and found to be in the acceptable range of 91--116%. The affinity constant (K a ) of individual FAs to protein albumin was determined to be 9.2×10 4 to 4.3×10 5 M -1 . The plasma protein binding (PPB%) was calculated, and found to be in the range of 98.0--99.7% for different polyunsaturated fatty acids (PUFAs). The PUFAs under study were found at a high concentration range in fish plasma, whereas only a few were within quantification range in control human plasma. The method was successfully applied for monitoring PUFA changes during the operation in plasma samples obtained from patients undergoing cardiac surgery with the use of cardiopulmonary bypass (CPB). The most significant contribution induced by surgery was noticed in the concentration level of α--linolenic acid (18:3, ALA), arachidonic acid (20:4, AA), and docosahexanoic acid (22:6, DHA) soon after administration of CPB in all cases.

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Development of a headspace solid-phase microextraction procedure for the determination of free volatile fatty acids in waste waters

Cited by 103 publications

References 27 publications

Salinity Constraints on Subsurface Archaeal Diversity and Methanogenesis in Sedimentary Rock Rich in Organic Matter

Salinity Constraints on Subsurface Archaeal Diversity and Methanogenesis in Sedimentary Rock Rich in Organic Matter

Development of a dynamic headspace solid-phase microextraction procedure coupled to GC–qMSD for evaluation the chemical profile in alcoholic beverages

Application of Solid Phase Microextraction for Quantitation of Polyunsaturated Fatty Acids in Biological Fluids

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