Determination of short chain chlorinated paraffins in water by stir bar sorptive extraction–thermal desorption–gas chromatography–triple quadrupole tandem mass spectrometry

Microextraction techniques have been proven to provide similar or better results in terms of sensitivity and reproducibility in comparison to liquid-liquid extraction (LLE) and solid-phase extraction (SPE). Furthermore, the high time efficiency and decreased workload leads to a higher sample throughput. In this review the state of the art of some of these techniques, namely solidphase microextraction (SPME), stir-bar sorptive extraction (SBSE), solid-phase dynamic extraction (SPDE), in-tube extraction-dynamic headspace (ITEX-DHS) and PAL SPME Arrow is shown. Furthermore, their benefits and drawbacks are discussed, together with their applicability to the analysis of water samples. To that end, the latest publications of microextraction techniques for a selection of regulated compound classes (chlorophenols (CPs), polycyclic aromatic hydrocarbons (PAHs), polychlorinated biphenyls (PCBs), pesticides, shortchained chlorinated paraffins (SCCPs) and volatile organic compounds (VOCs)) are compared.Finally, a guideline for choosing the best microextraction technique for different analytical needs is described.

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“…SCCPs, with 10 to 13 carbon atoms, are of special interest since they are the most toxic of the compound class [35].…”

Section: Short Chain Chlorinated Paraffinsmentioning

confidence: 99%

Solventless microextraction techniques for water analysis

Lorenzo-Parodi

Kaziur

Stojanović

et al. 2019

TrAC Trends in Analytical Chemistry

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“…It can be recognized that TE procedures are influenced by various factors and as a consequence, suitable conditions necessary for the global analyte transfer from the sorbent to the chromatographic column need to be selected or optimized 9–12 . The univariate approach or recommendations by the thermal desorption equipment’s manufacturers (for some extraction parameters) have been utilized to select optimal conditions for TE procedures in most studies that have been developed to monitor SVOCs in different environmental media 5–8,13–19 . However, the univariate approach involves many analyses, especially when the experimental factors to optimize are many, and obviously, it consumes a lot of time and other resources.…”

Section: Introductionmentioning

confidence: 99%

“…Based on the above limitation, we occasioned this study to fill the gap and pave the way for further studies of the same kind to involve other airborne semi-volatile organic compounds. Additionally, we thought that addressing some of the limitations that were encountered in the previously cited studies 5–8,13–19 , could be interesting.…”

Section: Introductionmentioning

confidence: 99%

Multivariate Optimization of Tenax TA-Thermal Extraction for Determining Gaseous Phase Organophosphate Esters in Air Samples

Matsiko

Wang

et al. 2019

Sci Rep

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Suitable conditions for thermal extraction of semi-volatile organic compounds have largely been arrived at by univariate optimization or based on the recommendations provided by the manufacturers of the extraction equipment. Herein, we demonstrated the multivariate optimization of Tenax TA–thermal extraction for determining organophosphate esters in the gas phase fraction of air samples. Screening and refining experiments were performed using the eighth fraction factorial and Box-Behnken designs, respectively, and satisfactory models were obtained. Subsequently, the process was optimized by Derringer’s desirability function and the global desirability was 0.7299. Following optimization, the analytes were desorbed at 290 °C for 10 minutes at a helium flow of 95 mL min −1 , with the transfer line set at 290 °C. The analytes were then cryofocused at 20 °C and then cryodesorbed into the chromatographic column at 295 °C for 6 minutes. Method validation exhibited high linearity coefficients (>0.99), good precision (CV < 14%) and low detection limits (0.1–0.5 ng m −3 ). The method was tested by pumping 0.024 m 3 of real indoor environment air through Tenax TA sorbent tubes. Furthermore, with multivariate optimization, analysis time and other resources were significantly reduced, and information about experimental factor interaction effects was investigated, as compared to the univariate optimization and other traditional methods.

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“…However, the GC coupled to mass spectrometry with electron capture negative ionization (GC-ECNI-MS) is today the more frequently used approach (Tomy et al 1997;Reth and Oehme 2004;Gandolfi et al 2015). Nowadays, the GC coupled to triple quadrupole mass spectrometry in mode Mass/Mass (GC-QqQ-MS/MS) is beginning to be used for analysis of CCPs in environmental samples using fragments of low m/z Tölgyessy et al 2017). The further fragmentations carried out by tandem mass spectrometry GC-QqQ-MS/MS open a world of possibilities to achieve good selectivity and sensitivity, in relation to low-resolution devices.…”

Section: Introductionmentioning

confidence: 99%

Development of a method for the determination of SCCPs (short-chain chlorinated paraffins) in bivalve mollusk using Soxtec device followed by gas chromatography-triple quadrupole tandem mass spectrometry

et al. 2018

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Background: Organochlorinated compounds are major environmental concern due to their persistence, long-range transportability and bio-accumulation. Chlorinated paraffin (CP) mixtures, especially short-chain CPs (SCCPs), are found in environmental samples at very high levels. However, information about their levels is still insufficient, mainly in marine biota. Methods: This study aimed to optimize and validate a method for the determination of SCCPs (short-chain chlorinated paraffins) in bivalve mollusk using a Soxtec extractor and Gas Chromatography coupled with Mass Spectrometry in tandem GC-QqQ-MS/MS (EI). A Plackett-Burman (2^7*3/16) type III resolution factorial design was used to optimize the extraction and purification procedures, sample amount, extractant volume, boiling and rinsing times as extraction variables and alumina, acid silica gel amounts and elution volume as purification variables. Results: The most influent factors were sample amount, rinsing time, extractant volume and acid silica gel amount. Further experiments were performed in order to attain the optimal values of these factors (4 g sample amount, 50 mL n-hexane-dichloromethane as extractant volume, 2 and 1.5 h boiling and rinsing times, 8 g alumina, 4 g acid silica gel (15%) and 50 mL n-hexane-dichloromethane as elution solvent). Validation of the optimized method presented recoveries higher than 90% with RSD below 10%, showing good accuracy and precision. The whole method limits of detection and quantification were 46.13 mg Kg -1 and 153.75 mg Kg

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Determination of short chain chlorinated paraffins in water by stir bar sorptive extraction–thermal desorption–gas chromatography–triple quadrupole tandem mass spectrometry

Cited by 13 publications

References 13 publications

Solventless microextraction techniques for water analysis

Solventless microextraction techniques for water analysis

Multivariate Optimization of Tenax TA-Thermal Extraction for Determining Gaseous Phase Organophosphate Esters in Air Samples

Development of a method for the determination of SCCPs (short-chain chlorinated paraffins) in bivalve mollusk using Soxtec device followed by gas chromatography-triple quadrupole tandem mass spectrometry

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