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Multi-class, multi-residue analysis of pesticides, polychlorinated biphenyls, polycyclic aromatic hydrocarbons, polybrominated diphenyl ethers and novel flame retardants in fish using fast, low-pressure gas chromatography-tandem mass spectrometry.

Analytica chimica acta (2012-12-19)
Yelena Sapozhnikova, Steven J Lehotay
ABSTRACT

A multi-class, multi-residue method for the analysis of 13 novel flame retardants, 18 representative pesticides, 14 polychlorinated biphenyl (PCB) congeners, 16 polycyclic aromatic hydrocarbons (PAHs), and 7 polybrominated diphenyl ether (PBDE) congeners in catfish muscle was developed and evaluated using fast low pressure gas chromatography triple quadrupole tandem mass spectrometry (LP-GC/MS-MS). The method was based on a QuEChERS (quick, easy, cheap, effective, rugged, safe) extraction with acetonitrile and dispersive solid-phase extraction (d-SPE) clean-up with zirconium-based sorbent prior to LP-GC/MS-MS analysis. The developed method was evaluated at 4 spiking levels and further validated by analysis of NIST Standard Reference Materials (SRMs) 1974B and 1947. Sample preparation for a batch of 10 homogenized samples took about 1h/analyst, and LP-GC/MS-MS analysis provided fast separation of multiple analytes within 9min achieving high throughput. With the use of isotopically labeled internal standards, recoveries of all but one analyte were between 70 and 120% with relative standard deviations less than 20% (n=5). The measured values for both SRMs agreed with certified/reference values (72-119% accuracy) for the majority of analytes. The detection limits were 0.1-0.5ng g(-1) for PCBs, 0.5-10ng g(-1) for PBDEs, 0.5-5ng g(-1) for select pesticides and PAHs and 1-10ng g(-1) for flame retardants. The developed method was successfully applied for analysis of catfish samples from the market.

MATERIALS
Product Number
Brand
Product Description

Supelco
PCB No 77, analytical standard
Supelco
Supel QuE, Citrate Extraction Tube, pk of 50, suitable for EN 15662
Supelco
Supel QuE, Acetate Tube, pk of 50, AOAC® 2007.01
Supelco
Supel QuE, PSA Tube, pk of 50, suitable for EN 15662:2008 per BS
Supelco
Supel QuE, PSA Tube, pk of 50, AOAC® 2007.01
Supelco
Supel QuE, PSA/C18/ENVI-Carb Tube, pk of 50, AOAC® 2007.01
Supelco
Supel QuE, PSA Tube, pack of 100, AOAC® 2007.01
Supelco
Supel QuE, PSA/C18 Tube, pack of 100, AOAC® 2007.01
Supelco
Supel QuE, PSA/C18/ENVI-Carb Tube, pack of 100, AOAC® 2007.01
Supelco
Supel QuE, Z-Sep/C18 Tube, centrifuge tube volume 2 mL, pack of 100
Supelco
Supel QuE, Z-Sep+ with MgSO4 Tube, centrifuge tube volume 12 mL, pack of 50 ea
Supelco
Supel QuE, Z-Sep with MgSO4 Tube, centrifuge tube volume 12 mL, pack of 50 ea
Supelco
Supel QuE, Z-Sep+ Tube, centrifuge tube volume 2 mL, pack of 100 ea
Supelco
Supel QuE, Z-Sep Tube, centrifuge tube volume 2 mL, pack of 100 ea
Supelco
Supel QuE, Z-Sep+ with MgSO4 Tube, centrifuge tube volume 2 mL, pack of 100 ea
Supelco
Supel QuE, Z-Sep with MgSO4 Tube, centrifuge tube volume 2 mL, pack of 100 ea
Supelco
Supel QuE, PSA Tube, pack of 50 ea, suitable for EN 15662:2008 per BS, centrifuge tube volume 15 mL , Shaker Compatible
Supelco
Supel QuE, PSA/C18 Tube (Shaker Compatible), pk of 50, suitable for EN 15662:2008 per BS, centrifuge tube volume 15 mL , Shaker Compatible
Supelco
Supel QuE, PSA/ENVI-Carb Tube 1, pk of 50, suitable for EN 15662:2008 per BS, centrifuge tube volume 15 mL , Shaker Compatible
Supelco
Supel QuE, PSA/ENVI-Carb Tube 2, pk of 50, suitable for EN 15662:2008 per BS, centrifuge tube volume 15 mL , Shaker Compatible
Supelco
Supel QuE, PSA Tube, pk of 50, AOAC® 2007.01, centrifuge tube volume 15 mL , Shaker Compatible
Supelco
Supel QuE, PSA/C18 Tube, pk of 50, AOAC® 2007.01, centrifuge tube volume 15 mL , Shaker Compatible
Supelco
Supel QuE, PSA/C18/ENVI-Carb Tube, pk of 50, AOAC® 2007.01, centrifuge tube volume 15 mL , Shaker Compatible
Supelco
Supel QuE, Z-Sep+ Tube, pk of 50, centrifuge tube volume 15 mL , Shaker Compatible
Supelco
Supel QuE, Z-Sep Tube, pk of 50, centrifuge tube volume 15 mL , Shaker Compatible
Supelco
Supel QuE, Z-Sep with MgSO4 Tube, pk of 50, centrifuge tube volume 15 mL , Shaker Compatible
Supelco
Supel QuE, Z-Sep/C18 Tube, pk of 50, centrifuge tube volume 15 mL , Shaker Compatible
Supelco
Supel QuE, Z-Sep+ with MgSO4 Tube, pk of 50, centrifuge tube volume 15 mL , Shaker Compatible