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
Abstract 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, informa...
| Main Authors: | , , , , , |
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| Format: | Article |
| Language: | English |
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SpringerOpen
2018-02-01
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| Series: | Journal of Analytical Science and Technology |
| Subjects: | |
| Online Access: | http://link.springer.com/article/10.1186/s40543-018-0139-z |
| _version_ | 1818916586434592768 |
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| author | N. Carro J. Cobas I. García M. Ignacio A. Mouteira B. Silva |
| author_facet | N. Carro J. Cobas I. García M. Ignacio A. Mouteira B. Silva |
| author_sort | N. Carro |
| collection | DOAJ |
| description | Abstract 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- 1, respectively. This method was successfully applied to the analysis of wild mussel samples coming from two Galician Rías. The found levels were very low compared to other marine systems, below parts per million. Conclusions The main advantages of the optimized method lie in the rapidity and the low amount of sorbents and volume of solvent used, as well as the selectivity and sensitivity of triple quadrupole MS/MS. |
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| id | doaj.art-8b9d867ebe5c4983ab18a2ffcc898ddf |
| institution | Directory Open Access Journal |
| issn | 2093-3371 |
| language | English |
| last_indexed | 2024-12-20T00:20:32Z |
| publishDate | 2018-02-01 |
| publisher | SpringerOpen |
| record_format | Article |
| series | Journal of Analytical Science and Technology |
| spelling | doaj.art-8b9d867ebe5c4983ab18a2ffcc898ddf2022-12-21T20:00:12ZengSpringerOpenJournal of Analytical Science and Technology2093-33712018-02-01911910.1186/s40543-018-0139-zDevelopment 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 spectrometryN. Carro0J. Cobas1I. García2M. Ignacio3A. Mouteira4B. Silva5Instituto Tecnolóxico para o Control do Medio Mariño de Galicia, INTECMAR, Consellería do Mar, Xunta de GaliciaInstituto Tecnolóxico para o Control do Medio Mariño de Galicia, INTECMAR, Consellería do Mar, Xunta de GaliciaInstituto Tecnolóxico para o Control do Medio Mariño de Galicia, INTECMAR, Consellería do Mar, Xunta de GaliciaInstituto Tecnolóxico para o Control do Medio Mariño de Galicia, INTECMAR, Consellería do Mar, Xunta de GaliciaInstituto Tecnolóxico para o Control do Medio Mariño de Galicia, INTECMAR, Consellería do Mar, Xunta de GaliciaInstituto Tecnolóxico para o Control do Medio Mariño de Galicia, INTECMAR, Consellería do Mar, Xunta de GaliciaAbstract 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- 1, respectively. This method was successfully applied to the analysis of wild mussel samples coming from two Galician Rías. The found levels were very low compared to other marine systems, below parts per million. Conclusions The main advantages of the optimized method lie in the rapidity and the low amount of sorbents and volume of solvent used, as well as the selectivity and sensitivity of triple quadrupole MS/MS.http://link.springer.com/article/10.1186/s40543-018-0139-zSCCPsBivalve molluskSoxtecGC-QqQ-MS/MS |
| spellingShingle | N. Carro J. Cobas I. García M. Ignacio A. Mouteira B. Silva 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 Journal of Analytical Science and Technology SCCPs Bivalve mollusk Soxtec GC-QqQ-MS/MS |
| title | 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 |
| title_full | 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 |
| title_fullStr | 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 |
| title_full_unstemmed | 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 |
| title_short | 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 |
| title_sort | 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 |
| topic | SCCPs Bivalve mollusk Soxtec GC-QqQ-MS/MS |
| url | http://link.springer.com/article/10.1186/s40543-018-0139-z |
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