Application of headspace solid-phase microextraction followed by gas chromatography–mass spectrometry to determine short-chain alkane monocarboxylic acids in aqueous samples

Banel, Anna; Wasielewska, Marta; Zygmunt, Bogdan

doi:10.1007/s00216-010-4415-z

Cited by 14 publications

(16 citation statements)

References 18 publications

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“…This procedure is known to lead to higher values for these parameters [71]. Nonetheless, the LOD and LOQ obtained are closer or even lower than those found in the literature when other approaches are followed [72][73][74], and for several times higher than the odor threshold of each VFA [75], confirming that the proposed methodology has an adequate sensitivity to the intended analysis. The accuracy results, which were obtained from a recovery study at three concentrations, also confirm the method's accuracy, with values ranging from 100.26% for butyric acid up to 108.42% for isovaleric acid.…”

Section: Validation Of the Optimal Extraction Conditionssupporting

confidence: 69%

Definitive Screening Designs and latent variable modelling for the optimization of solid phase microextraction (SPME): Case study - Quantification of volatile fatty acids in wines

Pereira

Reis

Leça

et al. 2018

Chemometrics and Intelligent Laboratory Systems

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In the present study, we apply the recently proposed Definitive Screening Designs (DSD) to optimize HS-SPME extraction in order to analyze volatile fatty acids (VFA) present in wine samples. This is the first attempt to apply this new class of designs to one of the most well-known and widely applied extraction techniques. The latent structure of the responses is also explored for defining the optimal extraction conditions. DSD is a new screening design with the potential to significantly reduce the number of experiments required to estimate the model parameters and to establish the optimum operation conditions. Therefore, there is an obvious interest in assessing the benefits of DSD in practice. In this work, this design framework is applied to the simultaneous optimization of seven extraction parameters (responses). Both qualitative and quantitative extraction parameters are considered, in order to test the flexibility of DSD designs: a two-level qualitative variable, the fiber coating, and six quantitative variables, namely the pre-incubation time, the extraction time and temperature, the headspace/sample volume, the effect of agitation during extraction and the influence of the ethanol content (sample dilution). Optimization of analytes' chromatographic responses was carried out both individually (response by response) and altogether, by modelling the responses in the latent variable space (i.e., explicitly considering their underlying correlation structure). In the end, a consensus analysis of all perspectives was considered in the definition of the overall optimal extraction conditions for the quantification of VFA in fortified wines. The solution found was to use a DVB/Car/PDMS fiber, 10 mL of samples in 20 mL vial, 40 min of extraction at 40 C. The analysis also revealed that the factors incubation time, agitation and sample dilution do not play a significant role in explaining the variability of extraction parameters. Therefore, they were set to the most convenient levels. The methodology followed was thoroughly validated and the following figures of merit were obtained: good linearity (R 2 > 0.999, for all compounds), high sensitivity (LOD and LOQ are close or below the values found in literature), recoveries of approximately 100% and suitable precision (repeatability and reproducibility lower than 7.21% and 8.61%, respectively). Finally, the optimized methodology was tested in practice. Several wine samples were analyzed and the odor activity value calculated to facilitate the identification of their importance as odor active compounds in different aged fortified wines. This work demonstrates the benefits of using DSD and latent variable modelling for the optimization of analytical techniques, contributing to the implementation of rigorous, systematic and more efficient optimization protocols.

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Section: Validation Of the Optimal Extraction Conditionssupporting

confidence: 69%

Definitive Screening Designs and latent variable modelling for the optimization of solid phase microextraction (SPME): Case study - Quantification of volatile fatty acids in wines

Pereira

Reis

Leça

et al. 2018

Chemometrics and Intelligent Laboratory Systems

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“…The extraction of volatile compounds from the free space of the samples was performed using PDMS/CAR/DVB fiber (polydimethylsiloxane/carboxen/divinylbenzene). The extraction time for the fiber was 40 min; the extraction temperature was 105 °C …”

Section: Methodsmentioning

confidence: 99%

SPME‐GC/MS Analysis of Volatile Compounds Contained in the Insect Larvae of Tenebrio molitor and Leptinotarsa decemlineata before and after Using Insecticides

Wojciechowska

Gołębiowski

2020

Chemistry & Biodiversity

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The larvae of two harmful insect species Tenebrio molitor and Leptinotarsa decemlineata were analyzed. The insects were sprayed with insecticides containing the active substances cyfluthrin and deltamethrin (T. molitor), and thiamethoxam and acetamiprid (L. decemlineata). The sprayed insect larvae were left for 24, 48 and 72 h. Samples were then prepared using SPME fiber to identify the volatile compounds contained in the larvae. The determinations were made by gas chromatography coupled with mass spectrometry (GC/MS). Chemical compounds were found in the analyzed samples: alkanes, aldehydes, ketones, esters, terpenes, fatty acids. In the samples prepared from T. molitor larvae, more than 20 % of aldehydes and 8 -41 % of alkanes were determined. In the samples from L. decemlineata, fatty acids were 8-65 % depending on the length of time after applying the insecticide.

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“…The implementation of solid‐phase microextraction is simple. This technique can be used to determine environmental samples with complex matrices which contain suspended matter (Banel et al, ).…”

Section: Discussionmentioning

confidence: 99%

“…The method is simple and the availability of fibers with various sorbents allows the concentration of various chemical compounds. In addition, various analytical techniques (GC, HPLC, GC–MS) can be used for proper analysis (Banel, Wasilewska, & Zygmunt, ; Chodkowski, ; Witkiewicz, ).…”

Section: Introductionmentioning

confidence: 99%

Application of headspace solid‐phase microextraction followed by gas chromatography coupled with mass spectrometry to determine esters of carboxylic acids and other volatile compounds inDermestes maculatusandDermestes aterlipids

Cerkowniak

Boguś

Włóka

et al. 2017

Biomedical Chromatography

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A constant problem in veterinary medicine, human healthcare, agriculture, forestry and horticulture is the large number of pests, and the lack of effective methods to combat them which cause no harm to the rest of the environment. It is recommended and desired to reduce the use of chemicals and increase the use of agents based on knowledge acquired in the fields of biology, chemistry and agrochemicals. To learn the defense mechanisms of insects we should consider not only the site of their physiological ability to protect against external factors (cuticle), but also the possibility of chemical protection, formed by all compounds on the surface and in the body of insects. In this study, a procedure was developed to determine the esters of carboxylic acids in insect lipids. Headspace solid-phase microextraction was followed by gas chromatography coupled with gas spectrometry. First, the best conditions were selected for the analysis to obtain the best chromatographic separation. An RTx-5 column was used for this purpose. Polydimethylsiloxane/divinylbenzene (PDMS/DVB) and polyacrylate fibers were used to isolate acid esters. PDMS/DVB fiber achieved the best conditions for the extraction; the extraction time was 50 min, the extraction temperature was 105°C and the desorption time was 10 min at 230°C. These solid-phase microextraction conditions were used to analyze volatile compounds extracted from insects belonging to the Dermestidae family.

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Application of headspace solid-phase microextraction followed by gas chromatography–mass spectrometry to determine short-chain alkane monocarboxylic acids in aqueous samples

Cited by 14 publications

References 18 publications

Definitive Screening Designs and latent variable modelling for the optimization of solid phase microextraction (SPME): Case study - Quantification of volatile fatty acids in wines

Definitive Screening Designs and latent variable modelling for the optimization of solid phase microextraction (SPME): Case study - Quantification of volatile fatty acids in wines

SPME‐GC/MS Analysis of Volatile Compounds Contained in the Insect Larvae of Tenebrio molitor and Leptinotarsa decemlineata before and after Using Insecticides

Application of headspace solid‐phase microextraction followed by gas chromatography coupled with mass spectrometry to determine esters of carboxylic acids and other volatile compounds inDermestes maculatusandDermestes aterlipids

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