Solid-phase extraction versus solid-phase microextraction for the determination of chlorinated paraffins in water using gas chromatography–negative chemical ionisation mass spectrometry

Castells, Pere Arqué; Santos, F.J.; Galcerán, M.T.

doi:10.1016/j.chroma.2003.10.069

Cited by 46 publications

(27 citation statements)

References 20 publications

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“…replicates. A c c e p t e d M a n u s c r i p t 33 [19,21] SPE with GC/ECNI-MS [20] DI-SPME with GC/ECNI-MS [20] SBSE with GC/ECD [23] HS-SPME with GC/ECNI-MS (this work) 0.05 (seawater) a n.r. : not reported b : LOD obtained by using DI-SPME coupled to GC/ECD c n.m.: not measured Table 4: Occurrences and concentration levels (ng.L -1 ) of SCCPs in south France aquatic environment.…”

Section: Resultsmentioning

confidence: 99%

“…The developed method was then applied to analyze real water samples: surface water Spain [20,22], UK [48], and Canada [49].…”

Section: Trueness In Surface Waters and Occurrence Of Sccps In South mentioning

confidence: 99%

“…The classical liquid-liquid extraction (LLE) and solid-phase extraction (SPE) are still the most commonly used extraction techniques for preconcentration of CPs from aqueous samples [20,21]. But, LLE requires high purity solvent and tedious clean-up task and SPE often causes high baseline blanks.…”

Section: Introductionmentioning

confidence: 99%

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Parameters optimization using experimental design for headspace solid phase micro-extraction analysis of short-chain chlorinated paraffins in waters under the European water framework directive

Gandolfi

Malleret

Sergent

et al. 2015

Journal of Chromatography A

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Section: Resultsmentioning

confidence: 99%

“…The developed method was then applied to analyze real water samples: surface water Spain [20,22], UK [48], and Canada [49].…”

Section: Trueness In Surface Waters and Occurrence Of Sccps In South mentioning

confidence: 99%

See 1 more Smart Citation

Parameters optimization using experimental design for headspace solid phase micro-extraction analysis of short-chain chlorinated paraffins in waters under the European water framework directive

Gandolfi

Malleret

Sergent

et al. 2015

Journal of Chromatography A

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“…Various extraction techniques from water, such as liquid-liquid extraction, solid phase extraction and solid phase microextraction, have been reported [3]. However, quantification is the main problem to be solved.…”

Section: Introductionmentioning

confidence: 99%

Determination of the Sum of Short Chain Polychlorinated n‐Alkanes with a Chlorine Content of Between 49 and 67% in Water by GC‐ECNI‐MS and Quantification by Multiple Linear Regression

Geiß¹,

Einax²,

Scott³

2010

CLEAN Soil Air Water

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This new approach for the quantification of the sum of short chain polychlorinated alkanes in mixtures (commonly abbreviated as SCCPs, where P stands for paraffin) with average chlorine contents between 49 and 67% and different C-number distributions is the background for ISO CD 12010, allowing standardized analysis according to the European water framework directive in unfiltered surface water, ground water, drinking water and waste water. A quantification method for the sum of short chain polychlorinated n-alkanes by GC-ECNI-MS (gas chromatography coupled with electron capture chemical ionization mass spectrometry), independent of the chlorine content and robust against changes in C-number distribution, was developed. This means that the very different response factors in GC-ECNI-MS, depending on the chlorine content, are no longer a problem for the analysis of SCCPs. Furthermore, problems with the selection of analytical standards due to batch dependent technical mixtures and different environmentally occurring mixtures can be overcome by using this robust method. The calibration was performed using synthetic mixtures mimicking a variety of different technically produced SCCP mixtures with average chlorine contents between 49 and 67% and different C-number distributions. By this means, the calibration is also traceable. The method was based on the integration of selected m/z value (mass/charge relation value) signals over the full retention range of the compounds. Quantification was performed using multiple linear regression calibration with two selected m/z signals, and verified with two other mass combinations. The selection of the m/z values used for quantification was carried out by means of an orthogonal calibration design. A stepwise procedure was utilized to produce the best quantification results, with the minimum number of quantification m/z signals, together with the minimization of potential interferences to be encountered in water analysis. The weighted sum of the peak areas of two m/z values, m/z 327 and 423, led to a sum determination which was applicable to the different SCCP mixtures most likely to be found in the aquatic environment. The problem with the very different response factors of the selected m/z values in GC-ECNI-MS, caused by the differing chlorine content of the SCCP mixtures, was overcome as well by forming the weighted sum of the two selected peak areas. The method was especially suitable for water analysis because of the low detection limit achieved by GC-ECNI-MS for chlorinated compounds.

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“…Soxhlet extraction and PLE are the most frequently used methods for CP extraction from biota and sediments. Three methods have been used for extracting or pre-concentrating CPs in water (i) SPE (Castells et al ., 2004;Dick et al ., 2010), (ii) SPME (Castells et al ., 2004) and (iii) liquid-liquid extraction (LLE; Moore et al ., 2004). GPC (Tomy et al ., 2000;Fridén et al ., 2005;Thomas et al ., 2006;Ismail et al ., 2009), concentrated sulfuric acid treatment, or sulfuric acid-silica gel column chromatography (Iino et al ., 2005) have all been used to remove co-extracted lipids from extracts.…”

Section: Methodsmentioning

confidence: 99%

Organic Micropollutants

Law

Webster

Theobald

et al. 2011

Chemical Marine Monitoring

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Solid-phase extraction versus solid-phase microextraction for the determination of chlorinated paraffins in water using gas chromatography–negative chemical ionisation mass spectrometry

Cited by 46 publications

References 20 publications

Parameters optimization using experimental design for headspace solid phase micro-extraction analysis of short-chain chlorinated paraffins in waters under the European water framework directive

Parameters optimization using experimental design for headspace solid phase micro-extraction analysis of short-chain chlorinated paraffins in waters under the European water framework directive

Determination of the Sum of Short Chain Polychlorinated n‐Alkanes with a Chlorine Content of Between 49 and 67% in Water by GC‐ECNI‐MS and Quantification by Multiple Linear Regression

Organic Micropollutants

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