scholarly journals Quantitative and enantioselective analysis of monoterpenes from plant chambers and in ambient air using SPME

2010 ◽  
Vol 3 (4) ◽  
pp. 3345-3381
Author(s):  
N. Yassaa ◽  
T. Custer ◽  
W. Song ◽  
F. Pech ◽  
J. Kesselmeier ◽  
...  
Keyword(s):  
Competitive Adsorption ◽  
Solid Phase ◽  
Ambient Air ◽  
Enantiomeric Separation ◽  
Gas Chromatography Mass Spectrometry ◽  
Polydimethyl Siloxane ◽  
Peak Resolution ◽  
Fibre Coating ◽  
Chamber Studies ◽  
Spme Fibre

Abstract. A solid-phase microextraction (HS-SPME) and gas chromatography/mass spectrometry (GC/MS) system has been developed for quantifying enantiomeric and nonenantiomeric monoterpenes in plant chamber studies and ambient air. Performance of this system was checked using a capillary diffusion system to produce monoterpene standards. The adsorption efficiency, competitive adsorption and chromatographic peak resolution of monoterpene enantiomer pairs were compared for three SPME fibre coatings: 75 μm Carboxen-PDMS (CAR-PDMS), 50/30 μm, divinylbenzene-carboxen-polydimethylsiloxane (DVB-CAR-PDMS) and 65 μm divinylbenzene-polydimethyl-siloxane (DVB-PDMS). Key parameters such as the linearity and reproducibility of the SPME system have been investigated in this work. The best compromise between the enantiomeric separation of monoterpenes and competitive adsorption of the isoprenoids on the solid SPME fibre coating was found for DVB-PDMS fibres. The optimum conditions using DVB-PDMS fibres were applied to measure the exchange rates of monoterpenes in the emission of Quercus ilex using a laboratory whole plant enclosure under light and dark conditions, as well as in ambient air. With 592 and 223 ng m−2 s−1, respectively, β-myrcene and limonene were the predominant monoterpenes in the emission of Q. ilex. These values were closely comparable to those obtained using a zNose and cartridge GC-FID systems.

scholarly journals Quantitative and enantioselective analysis of monoterpenes from plant chambers and in ambient air using SPME

2010 ◽  
Vol 3 (6) ◽  
pp. 1615-1627 ◽  
Author(s):  
N. Yassaa ◽  
T. Custer ◽  
W. Song ◽  
F. Pech ◽  
J. Kesselmeier ◽  
...  
Keyword(s):  
Competitive Adsorption ◽  
Solid Phase ◽  
Ambient Air ◽  
Enantiomeric Separation ◽  
Gas Chromatography Mass Spectrometry ◽  
Peak Resolution ◽  
Whole Plant ◽  
Fibre Coating ◽  
Chamber Studies ◽  
Spme Fibre

Abstract. A headspace solid-phase microextraction (HS-SPME) and gas chromatography/mass spectrometry (GC/MS) system has been developed for quantifying enantiomeric and nonenantiomeric monoterpenes in plant chamber studies and ambient air. Performance of this system was checked using a capillary diffusion system to produce monoterpene standards. The adsorption efficiency, competitive adsorption and chromatographic peak resolution of monoterpene enantiomer pairs were compared for three SPME fibre coatings: 75 μm Carboxen-PDMS (CAR-PDMS), 50/30 μm divinylbenzene-carboxen-polydimethylsiloxane (DVB-CAR-PDMS) and 65 μm divinylbenzene-polydimethylsiloxane (DVB-PDMS). Key parameters such as the linearity and reproducibility of the SPME system have been investigated in this work. The best compromise between the enantiomeric separation of monoterpenes and competitive adsorption of the isoprenoids on the solid SPME fibre coating was found for DVB-PDMS fibres. The optimum conditions using DVB-PDMS fibres were applied to measure the exchange rates of monoterpenes in the emission of Quercus ilex using a laboratory whole plant enclosure under light and dark conditions, as well as in ambient air. With 592 and 223 ng m−2 s−1 respectively, β-myrcene and limonene were the predominant monoterpenes in the emission of Q. ilex. These values were closely comparable to those obtained using a zNose and cartridge GC-FID systems.

scholarly journals Determination of multi-class herbicides in soil by liquid-solid extraction coupled with headspace solid phase microextraction method

2016 ◽  
Vol 81 (8) ◽  
pp. 923-934 ◽  
Author(s):  
Rada Djurovic-Pejcev ◽  
Tijana Djordjevic ◽  
Vojislava Bursic
Keyword(s):  
Solid Phase Microextraction ◽  
Solid Phase ◽  
Soil Samples ◽  
Gas Chromatography Mass Spectrometry ◽  
Optimum Number ◽  
Polydimethyl Siloxane ◽  
Headspace Solid Phase Microextraction ◽  
Relative Standard ◽  
Detection And Quantification

A method is described for simultaneous determination of five herbicides (metribuzin, acetochlor, clomazone, oxyfluorfen and dimethenamid) belonging to different pesticides groups in soil samples. Developed headspace solid phase microextraction method (HS-SPME) in combination with liquid-solid sample preparation (LS) was optimized and applied in the analysis of some agricultural samples. Optimization of microextraction conditions, such as temperature, extraction time and sodium chloride (NaCl) content was perfor-med using 100 ?m polydimethyl-siloxane (PDMS) fiber. The extraction effi-ciencies of methanol, methanol:acetone=1:1 and methanol:acetone:hexane= =2:2:1 and the optimum number of extraction steps during the sample prepa-ration, were tested, as well. Gas chromatography-mass spectrometry (GC-MS) was used for detection and quantification, obtaining relative standard deviation (RSD) below 13%, and recovery values higher than 83% for multiple analyses of soil samples fortified at 30 ?g kg-1 of each herbicide. Limits of detection (LOD) were less than 1.2 ?g kg-1 for all the studied herbicides.

scholarly journals An Optimized SPME-GC-MS Method for Volatile Metabolite Profiling of Different Alfalfa (Medicago sativa L.) Tissues

Molecules ◽  
2021 ◽  
Vol 26 (21) ◽  
pp. 6473
Author(s):  
Dong-Sik Yang ◽  
Zhentian Lei ◽  
Mohamed Bedair ◽  
Lloyd W. Sumner
Keyword(s):  
Solid Phase ◽  
Glandular Trichomes ◽  
Ambient Air ◽  
Extraction Time ◽  
Gas Chromatography Mass Spectrometry ◽  
Extraction Temperature ◽  
Buffer Solution ◽  
Biochemical Basis ◽  
Volatile Metabolites ◽  
Stems And Leaves

Solid-phase microextraction (SPME) was coupled to gas chromatography mass spectrometry (GC-MS) and a method optimized to quantitatively and qualitatively measure a large array of volatile metabolites in alfalfa glandular trichomes isolated from stems, trichome-free stems, and leaves as part of a non-targeted metabolomics approach. Major SPME extraction parameters optimized included SPME fiber composition, extraction temperature, and extraction time. The optimized SPME method provided the most chemically diverse coverage of alfalfa volatile and semi-volatile metabolites using a DVB/CAR/PDMS fiber, extraction temperature of 60 °C, and an extraction time of 20 min. Alfalfa SPME-GC-MS profiles were processed using automated peak deconvolution and identification (AMDIS) and quantitative data extraction software (MET-IDEA). A total of 87 trichome, 59 stem, and 99 leaf volatile metabolites were detected after background subtraction which removed contaminants present in ambient air and associated with the fibers and NaOH/EDTA buffer solution containing CaCl2. Thirty-seven volatile metabolites were detected in all samples, while 15 volatile metabolites were uniquely detected only in glandular trichomes, 9 only in stems, and 33 specifically in leaves as tissue specific volatile metabolites. Hierarchical cluster analysis (HCA) and principal component analysis (PCA) of glandular trichomes, stems, and leaves showed that the volatile metabolic profiles obtained from the optimized SPME-GC-MS method clearly differentiated the three tissues (glandular trichomes, stems, and leaves), and the biochemical basis for this differentiation is discussed. Although optimized using plant tissues, the method can be applied to other types of samples including fruits and other foods.

Characterization of Agarwood Incense using Gas Chromatography - Mass Spectrometry (GC-MS) coupled with Solid Phase Micro Extraction (SPME) and Gas Chromatography - Flame Ionization Detector (GC-FID)

2015 ◽  
Vol 12 (2) ◽  
pp. 67
Author(s):  
Nurlaila Ismail ◽  
Mastura Lbrahim ◽  
Seema Zareen ◽  
Mohd Hezri Fazalul Rahiman ◽  
Saiful Nizam Tajuddin ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Solid Phase ◽  
Flame Ionization Detector ◽  
Gas Chromatography Mass Spectrometry ◽  
Solid Phase Micro Extraction ◽  
Ionization Detector ◽  
Polydimethyl Siloxane ◽  
Flame Ionization ◽  
Chromatography Mass Spectrometry

This paper presents the application of Solid Phase Micro Extraction (SPME) coupled with Gas Chromatography-Mass Spectrometry (GC-MS) and Gas Chromatography-Flame Ionization Detector (GC-FID) to charaterize agarwood incense. The work involved three types of SPME fibres at 30 minutes sampling time. The fibres are 50/30 µm divinylbenzene-carboxen­polydimethysiloxane (DVB-CAR-PDMS), 65 µm polydi methylsiloxane­divinylbenzene (PDMS-DVB) and 85 µm carboxen-polydimethyl siloxane (CAR-PDMS). The results showed that among many compounds extracted by GC-MS coupled with SPME, six compounds were found significantly presence in high quality aganvood incense due to their high percentage area (%). They are beta-maaliene, alpha-elemol, beta-selinene, 10-epi-gamma-eudesmol, agarospirol and caryophellene oxide. The finding offers a new approach for establishing the volatile profile of agarwood incense components which is beneficial for agarwood grading and discrimination.

Application of Solid-Phase Micro-Extraction Technology to Drug Screening and Identification

2001 ◽  
Vol 38 (5) ◽  
pp. 541-547 ◽  
Author(s):  
Mohammad H Mosaddegh ◽  
Thomas Richardson ◽  
R W Stoddart ◽  
John McClure
Keyword(s):  
Solid Phase ◽  
Local Anaesthetics ◽  
Gas Chromatography Mass Spectrometry ◽  
Solid Phase Micro Extraction ◽  
Extraction Technology ◽  
Fibre Coating ◽  
Coefficients Of Variation ◽  
Screening And Identification ◽  
One Step ◽  
Temperature Time

Benzodiazepines, tricyclic antidepressants and local anaesthetics are frequently involved in poisoning episodes and fatalities. A specific, sensitive and rapid procedure for identifying and quantifying such drugs in postmortem matrices has been developed using solid-phase micro-extraction (SPME) and gas chromatography-mass spectrometry. Very clean extracts were obtained in one step using SPME. The most commonly used fibre coatings were tested to select the best coating for SPME of the drugs. The appropriate fibre coating for most drugs was polyacrylate, followed by Carbowax-divinylbenzene. A Hewlett-Packard 5890 gas chromatograph in combination with a Trio 2000 mass spectrometer was used to analyse the samples. Temperature, time, pH and addition of sodium chloride were optimized to obtain consistent extraction. The between-day and within-day coefficients of variation were less than 16% and less than 6%, respectively.

Fast determination of methyl chloride and methyl bromide emissions from dried plant matter and soil samples using HS-SPME and GC-MS: method and first results

2009 ◽  
Vol 6 (4) ◽  
pp. 311 ◽  
Author(s):  
Noureddine Yassaa ◽  
Asher Wishkerman ◽  
Frank Keppler ◽  
Jonathan Williams
Keyword(s):  
Methyl Bromide ◽  
Solid Phase Microextraction ◽  
Solid Phase ◽  
Methyl Chloride ◽  
Field Studies ◽  
Soil Samples ◽  
Gas Chromatography Mass Spectrometry ◽  
Spme Fibre ◽  
Non Destructive

Environmental context. Headspace solid-phase microextraction (HS-SPME) and analysis by gas chromatography–mass spectrometry (GC/MS) system has been employed for quantifying the emissions of methyl chloride (CH3Cl) and methyl bromide (CH3Br) from plants and soils. Compared with more commonly used techniques, HS-SPME coupled to GC/MS is simple, fast, sensitive, economical and non-destructive, with potential for laboratory-based and field studies. Abstract. Headspace solid-phase microextraction (HS-SPME) and gas chromatography–mass spectrometry (GC/MS) system have been employed for quantifying the emissions of methyl chloride (CH3Cl) and methyl bromide (CH3Br) from plants and soils. Seven SPME fibre coatings including 75 μm Carboxen-polydimethylsiloxane (CAR-PDMS), 85 μm Carboxen-PDMS (CAR-PDMS), 50/30 μm divinylbenzene-CAR-PDMS (DVB-CAR-PDMS), 65 μm DVB-PDMS, 65 μm carbowax-DVB (CW-DVB), 30 μm PDMS (PDMS) and 100 μm PDMS, were tested by comparing their sampling efficiencies towards CH3Cl and CH3Br. Key parameters such as extraction time, desorption temperature and time were all optimised in this work. The optimum conditions were found with CAR-PDMS 75 μm as an SPME fibre coating, a 1-min sampling time, a 50°C incubation temperature and a 2-min desorption time and a 250°C desorption temperature. These conditions were used for the determination of CH3Cl and CH3Br emission rates from different plant species as well as soil samples. Compared with more commonly used techniques, HS-SPME coupled to GC/MS is simple, fast, sensitive, economical and non-destructive, with potential for laboratory-based and field studies.

Leachability of Solidified Petroleum Sludge

2014 ◽  
Vol 917 ◽  
pp. 123-133 ◽  
Author(s):  
Asna Mohd Zain ◽  
Shaaban Md Ghazaly ◽  
Mahmud Hilmi
Keyword(s):  
Organic Compounds ◽  
Acidic Medium ◽  
Solid Phase ◽  
Effective Diffusion ◽  
Carbon Chain ◽  
Solid Sample ◽  
Gas Chromatography Mass Spectrometry ◽  
Ethyl Benzene ◽  
Polydimethyl Siloxane ◽  
Petroleum Sludge

Petroleum sludge was solidified in ordinary Portland cement, and the leachability test was performed based on American Nuclear Society 16.1 to produce leachate. The organic in solidified sludge was extracted by micro solid extraction to determine the organic in the sample. Organic in the leachate sample was detected by solid phase micro extraction by head space polydimethyl siloxane fiber using gas chromatography mass spectrometry. The targeted organic compounds in solid sample and leachate were quantified by the benzene, toluene, ethyl benzene, xylene, naphthalene and phenanthrene standards. The organic compounds in solidified sludge consist of aliphatic and ester acid with long carbon chain of Carbon 15 to Carbon 64. The aliphatic group in the leachate was found at the reduced rate of about tenfold of the solid sample. Derivative leachate products mainly composed of cyclic siloxane compounds. The metals leachability in the acidic medium depends on the metal hydroxide solubility value. High lead mobility in the acidic medium was due to its high solubility induced the highest effective diffusion coefficient of 1.59 x 10-07cm2/s.

Characterization of Agarwood Incense using Gas Chromatography - Mass Spectrometry (GC-MS) coupled with Solid Phase Micro Extraction (SPME) and Gas Chromatography - Flame Ionization Detector (GC-FID)

2015 ◽  
Vol 12 (2) ◽  
pp. 67
Author(s):  
Nurlaila Ismail ◽  
Mastura Lbrahim ◽  
Seema Zareen ◽  
Mohd Hezri Fazalul Rahiman ◽  
Saiful Nizam Tajuddin ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Solid Phase ◽  
Flame Ionization Detector ◽  
Gas Chromatography Mass Spectrometry ◽  
Solid Phase Micro Extraction ◽  
Ionization Detector ◽  
Polydimethyl Siloxane ◽  
Flame Ionization ◽  
Chromatography Mass Spectrometry

This paper presents the application of Solid Phase Micro Extraction (SPME) coupled with Gas Chromatography-Mass Spectrometry (GC-MS) and Gas Chromatography-Flame Ionization Detector (GC-FID) to charaterize agarwood incense. The work involved three types of SPME fibres at 30 minutes sampling time. The fibres are 50/30 µm divinylbenzene-carboxen­polydimethysiloxane (DVB-CAR-PDMS), 65 µm polydimethylsiloxane­divinylbenzene (PDMS-DVB) and 85 µm carboxen-polydimethyl siloxane (CAR-PD MS). The results showed that among many compounds extracted by GC-MS coupled with SPME, six compounds were found significantly presence in high quality aganvood incense due to their high percentage area(%). They are b-maaliene, a-elemol, b-selinene, 10-epi-y-eudesmol, agarospirol and caryophellene oxide. The finding offers a new approach for establishing the volatile profile of agarwood incense components which is beneficial for agarwood grading and discrimination. 

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