Solid-phase microextraction
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Solid-phase extraction (SPE), solid-phase microextraction (SPME) using carbowax/divinylbenzen fiber, and stir bar sorptive extraction (SBSE) followed by solvent back extraction have been used for the extraction of free fatty acids (caproic, caprylic, pelargonic, capric, lauric, myristic, palmitic, stearic, oleic, linoleic, and linolenic acids) from beer. Subsequent gas chromatographic analyses with flame ionization detection were used for the determination of these compounds. Medium-chain fatty acids (caproic-lauric acid) were determined as free acids, and long-chain fatty acids (myristic-linolenic acids) were determined as methyl esters after methylation by BF(3)-methanol 14%. Linearity, recovery, and repeatability of all methods have been determined and compared with the SPE method used as a reference (SPME method was used only for medium-chain fatty acid determination). All three procedures provide similar working parameters characterized by high repeatability (2.3-16.3%) and good linearity (correlation coefficient ranging from 0.9919 to 0.9999). Results of beer analyses obtained by using these three methods were highly correlated. Although all methods provide compatible alternatives, for medium-chain fatty acid analysis SPME may be a more appropriate technique due to its operational simplicity, repeatability, and low cost.
Methods for the separation and determination of terpenes (mono- and sesqui-) and phenylpropanoids such as eugenol and methyleugenol from samples of allspice berries have been developed. Chromatographic analyses of isolated groups of compounds were carried out by means of gas chromatography coupled with mass spectrometry. A comparison of various types of solid-phase microextraction fibers was performed. The highest yields of terpenes were extracted by polydimethylsiloxane and divinylbenzene/Carboxen/polydimethylsiloxane fibers (almost the same for these two fibers), approximately twice as much as by Carbowax/divinylbenzene fiber. The highest amounts of monoterpenes were extracted by divinylbenzene/Carboxen/polydimethylsiloxane fiber, and the highest amounts of sesquiterpenes were extracted by polydimethylsiloxane fiber. Moreover, the effect of water addition on extraction yields as well as time and temperature of extraction were tested. Aroma profiles of extracts obtained by solid-phase microextraction and essential oil obtained by hydrodistillation of allspice berries were compared. The aroma profile of the divinylbenzene/Carboxen/polydimethylsiloxane fiber extract was similar to the aroma profile of essential oil. Particular characteristics of volatile allspice matters were presented. The linear retention indices for each compound were calculated.
- Klíčová slova
- Allspice, Essential oils, Gas chromatography with mass spectrometry, Solid-phase microextraction, Terpenes,
- MeSH
- destilace MeSH
- dimethylpolysiloxany chemie MeSH
- mikroextrakce na pevné fázi metody MeSH
- monoterpeny chemie MeSH
- oleje prchavé MeSH
- Pimenta (rod) chemie MeSH
- plynová chromatografie s hmotnostně spektrometrickou detekcí metody MeSH
- polyethylenglykoly chemie MeSH
- seskviterpeny chemie MeSH
- teplota MeSH
- terpeny analýza chemie MeSH
- vinylové sloučeniny chemie MeSH
- voda chemie MeSH
- Publikační typ
- časopisecké články MeSH
- Názvy látek
- baysilon MeSH Prohlížeč
- carbowax 600 MeSH Prohlížeč
- dimethylpolysiloxany MeSH
- divinyl benzene MeSH Prohlížeč
- monoterpeny MeSH
- oleje prchavé MeSH
- polyethylenglykoly MeSH
- seskviterpeny MeSH
- terpeny MeSH
- vinylové sloučeniny MeSH
- voda MeSH
3D printing is an extensively used manufacturing technique that can pose specific health concerns due to the emission of volatile organic compounds (VOC). Herein, a detailed characterization of 3D printing-related VOC using solid-phase microextraction-gas chromatography/mass spectrometry (SPME-GC/MS) is described for the first time. The VOC were extracted in dynamic mode during the printing from the acrylonitrile-styrene-acrylate filament in an environmental chamber. The effect of extraction time on the extraction efficiency of 16 main VOC was studied for four different commercial SPME arrows. The volatile and semivolatile compounds were the most effectively extracted by carbon wide range-containing and polydimethyl siloxane arrows, respectively. The differences in extraction efficiency between arrows were further correlated to the molecular volume, octanol-water partition coefficient, and vapour pressure of observed VOC. The repeatability of SPME arrows towards the main VOC was assessed from static mode measurements of filament in headspace vials. In addition, we performed a group analysis of 57 VOC classified into 15 categories according to their chemical structure. Divinylbenzene-polydimethyl siloxane arrow turned out to be a good compromise between the total extracted amount and its distribution among tested VOC. Thus, this arrow was used to demonstrate the usefulness of SPME for the qualification of VOC emitted during printing in a real-life environment. A presented methodology can serve as a fast and reliable method for the qualification and semi-quantification of 3D printing-related VOC.
- Klíčová slova
- 3D printing, Gas chromatography/mass spectrometry, Solid-phase microextraction, Volatile organic compounds,
- MeSH
- 3D tisk MeSH
- akrylonitril * MeSH
- mikroextrakce na pevné fázi metody MeSH
- siloxany MeSH
- styren MeSH
- těkavé organické sloučeniny * analýza MeSH
- Publikační typ
- časopisecké články MeSH
- Názvy látek
- akrylonitril * MeSH
- baysilon MeSH Prohlížeč
- siloxany MeSH
- styren MeSH
- těkavé organické sloučeniny * MeSH
A method employing the direct immersion solid-phase microextraction followed by GC-MS analysis is presented for the determination of essential oils components in herbal tea infusions, i.e. their direct content in the liquid phase. The extraction performances were compared using five different microextraction fibres. Significant parameters affecting sorption process such as sample amount, sorption and desorption time and temperature, stirring speed, pH adjustment and effect of ionic strength were optimised and discussed. By optimising the key parameters, a detection limits (LOD = S/N × 3) for ten target marker compounds were obtained in the range from 5.3 to 48.2 ng/mL with recoveries ranged between 93.03 and 100.50%. Intra-day and inter-day repeatability at three concentration levels were found to be 1.1-15.3 and 7.2-15.5% RSD, respectively. Finally, the optimised procedure enabling a rapid and simple analysis of essential oils was applied for the direct determination of these compounds in ten herbal tea infusions.
The presented study investigates the use of passive sampling, i.e. solid phase microextraction with polydimethylsiloxane fibers (PDMS-SPME), to assess the bioavailability of fiver neutral organic chemicals (phenanthrene, pyrene, lindane, p,p'-DDT, and PCB 153) spiked to natural and artificial soils after different aging times. Contaminant bioavailability was assessed by comparing PDMS concentrations with results from a 10 day bioaccumulation test with earthworms (Eisenia fetida). The hypotheses tested were (i) organic carbon (OC) normalization, which is commonly used to account for sorption and bioavailability of hydrophobic organic chemicals in soil risk assessment, has limitations due to differences in sorptive properties of OC and aging processes (i.e. sequestration and biodegradation) and (ii) PDMS-SPME provides a more reliable measure of soil contaminant bioavailability than OC normalized soil concentrations. The above stated hypotheses were confirmed since the results showed that: (i) the PDMS/soil organic carbon partition ratio (R) accounting for the role that OC plays in partitioning significantly differed between soils and aging times and (ii) the correlation with earthworm concentrations was better using porewater concentrations derived from PDMS concentrations than when organic normalized soil concentrations were used. Capsule: Sorption of organic compounds measured by SPME method and their bioavailability to earthworms cannot be reliably predicted using OC content.
- Klíčová slova
- Aging, Artificial soil, Bioaccumulation, Solid phase micro-extraction (SPME), Total organic carbon content (TOC),
- MeSH
- látky znečišťující půdu chemie metabolismus MeSH
- mikroextrakce na pevné fázi * MeSH
- monitorování životního prostředí MeSH
- Oligochaeta chemie metabolismus MeSH
- organické látky analýza metabolismus MeSH
- zvířata MeSH
- Check Tag
- zvířata MeSH
- Publikační typ
- časopisecké články MeSH
- práce podpořená grantem MeSH
- Názvy látek
- látky znečišťující půdu MeSH
- organické látky MeSH
This paper deals with comparison of efficiency of extraction techniques (solid-phase extraction, SPE and solid-phase microextraction, SPME) used for extraction of nitrate esters (ethyleneglycoldinitrate, EGDN and nitroglycerin, NG), representing the first step of the method of quantitative determination of trace concentrations of nitrate esters in water samples. EGDN and NG are subsequently determined by means of high-performance liquid chromatography with ultraviolet detection (HPLC-UV). Optimization of SPE and SPME conditions was carried out using model water samples. Seven SPE cartridges were tested and the conditions were optimized (type of sorbent, type and volume of solvent to be used as eluent). For both nitrate esters the limit of detection (LOD) and the limit of quantification (LOQ) obtained using SPE/HPLC-UV were 0.23 microg mL(-1) and 0.70 microg mL(-1), respectively. Optimization of SPME conditions: type of SPME fibre (four fibres were tested), type and time of sorption/desorption, temperature of sorption. PDMS/DVB (polydimethylsiloxane/divinylbenzene) fibre coating proved to be suitable for extraction of EGDN and NG. For this fibre the LOD and the LOQ for both nitrate esters were 0.16 microg mL(-1) and 0.50 microg mL(-1), respectively. Optimized methods SPE/HPLC-UV and SPME/HPLC-UV were then used for quantitative determination of nitrate esters content in real water samples from the production of EGDN and NG.
- MeSH
- adsorpce MeSH
- časové faktory MeSH
- dusičnany analýza izolace a purifikace MeSH
- estery analýza izolace a purifikace MeSH
- kalibrace MeSH
- mikroextrakce na pevné fázi metody MeSH
- nitroglycerin analýza izolace a purifikace MeSH
- reprodukovatelnost výsledků MeSH
- rozpouštědla MeSH
- teplota MeSH
- voda chemie MeSH
- vysokoúčinná kapalinová chromatografie MeSH
- Publikační typ
- časopisecké články MeSH
- práce podpořená grantem MeSH
- srovnávací studie MeSH
- Názvy látek
- dusičnany MeSH
- estery MeSH
- nitroglycerin MeSH
- rozpouštědla MeSH
- voda MeSH
For the first time, headspace solid-phase microextraction coupled with GC-MS analysis was used to study volatile compounds emitted by the tick Ixodes ricinus (L.). Variables such as the type of SPME fibre, equilibration time and extraction time have been evaluated with the mixture of four selected standards, a so-called artificial tick (acetophenone, racemic 4-heptanolide, methyl 2-methoxybenzoate and methyl 3-chloro-4-methoxybenzoate). Optimized conditions were obtained by the use of polydimethylsiloxan 100 microm fibre at 30 min equilibration and 15 min extraction time. The method proved to have a good linearity (r2 >0.98) at a concentration range from 0.5 ng (1 ng for methyl 3-chloro-4-methoxybenzoate) to 25 ng. LODs for a compound ranged between 0.19 and 1 ng, RSD (%) ranged from 13.76 to 25.08. The determination of 1.99 ng of methyl 3-chloro-4-methoxybenzoate emitted by five engorged females proved the usefulness of the developed method to identify and quantify the volatile compounds emitted by I. ricinus ticks.
- MeSH
- anisoly analýza MeSH
- benzoáty analýza chemie MeSH
- klíště chemie MeSH
- mikroextrakce na pevné fázi metody MeSH
- plynová chromatografie s hmotnostně spektrometrickou detekcí metody MeSH
- sexuální lákadla analýza chemie MeSH
- volatilizace MeSH
- zvířata MeSH
- Check Tag
- mužské pohlaví MeSH
- ženské pohlaví MeSH
- zvířata MeSH
- Publikační typ
- časopisecké články MeSH
- práce podpořená grantem MeSH
- Názvy látek
- 1,3-dimethoxybenzene MeSH Prohlížeč
- anisoly MeSH
- benzoáty MeSH
- sexuální lákadla MeSH
In this study, an optimisation of extraction of sulphur volatile compounds (SVCs) has been performed using Central Composite Design. The conditions of the highest amount of eluated peaks and total peaks area have been treated. Factors such as coating of fiber for SPME (Solid Phase Microextraction), extraction temperature and extraction time have been optimised. The SVCs have shown the optimal extraction using a DVB/CAR/PDMS (divinylbenzene/carboxen/polydimethylsiloxane) fiber at 73 °C during 50 min. Furthermore, a pre-incubation step lasting 20 min at the extraction temperature has been used. In total, 12 samples have been investigated at the mentioned optimal conditions, eight from the Alliaceae and four from the Brassicaceae family. The highest number of SVCs (24) has been identified in the sample of chive. The most frequently identified compound found in 11 of 12 samples has been dimethyl trisulphide.
- Klíčová slova
- Alliaceae, Brassicaceae, Gas chromatography/mass spectrometry, Headspace, Solid-phase microextraction, Sulphur volatile compounds,
- Publikační typ
- časopisecké články MeSH
The linear solvation energy relationship (LSER) model was used to characterize interactions responsible for sorption of volatile organic compounds (VOCs) in air samples on six different solid-phase microextraction (SPME) fibers at 296K and zero relative humidity. The polydimethylsiloxane and polyacrylate fibers sorption data were also modeled at different relative humidities in the range of 10-90% and influence of water vapors on the extraction process is discussed. The LSER equations were obtained by a multiple regression of the distribution coefficients of 14 probe solutes on an appropriate SPME fiber against the solvation parameters of the solutes. The derived LSER equations successfully predicted the VOC distribution coefficients and the selectivity of individual SPME fibers for the various volatile solutes. The LSER approach coupled with SPME is a relatively simple and reliable tool to rapidly characterize the sorption mechanism of VOCs with various stationary phases and may potentially be applied to design and test new chromatographic materials for sampling or separation of VOCs.
- MeSH
- adsorpce MeSH
- mikroextrakce na pevné fázi metody MeSH
- multivariační analýza MeSH
- organické látky analýza izolace a purifikace MeSH
- vlhkost MeSH
- volatilizace MeSH
- vzduch analýza MeSH
- Publikační typ
- časopisecké články MeSH
- Názvy látek
- organické látky MeSH
INTRODUCTION: The analysis of plant and herbal samples is a challenging task for analytical chemists due to the complexity of the matrix combined with the low concentration of analytes. In recent years different liquid-phase microextraction (LPME) techniques coupled with a variety of analytical equipment have been developed for the determination of both organic and inorganic analytes. OBJECTIVE: Over the past few years, the number of research papers in this field has shown a markedly growing tendency. Therefore, the purpose of this review paper is to summarise and critically evaluate research articles focused on the application of LPME techniques for the analysis of plant and herbal samples. RESULTS: Due to the complex nature of the samples, the direct application of LPME techniques to the analysis of plants has not often been done. LPME techniques as well as their modalities have been commonly applied in combination with other pretreatment techniques, including a solid-liquid extraction technique supported by mechanical agitation or auxiliary energies for plant analysis. Applications and the most important parameters are summarised in the tables. CONCLUSION: This review summarises the application of the LPME procedure and shows the major benefits of LPME, such as the low volume of solvents used, high enrichment factor, simplicity of operation and wide selection of applicable detection techniques. We can expect further development of microextraction analytical methods that focus on direct sample analysis with the application of green extraction solvents while fully automating procedures for the analysis of plant materials.
- Klíčová slova
- dispersive liquid-liquid microextraction, herbal, liquid-phase microextraction, plant, single-drop microextraction, solid samples,
- MeSH
- mikroextrakce kapalné fáze * MeSH
- rostliny MeSH
- rozpouštědla MeSH
- Publikační typ
- časopisecké články MeSH
- přehledy MeSH
- Názvy látek
- rozpouštědla MeSH
