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A High Throughput Method for Measuring Polycyclic Aromatic Hydrocarbons in Seafood Using QuEChERS Extraction and SBSE.

Pfannkoch EA, Stuff JR, Whitecavage JA, Blevins JM, Seely KA, Moran JH - Int J Anal Chem (2015)

Bottom Line: National Oceanic and Atmospheric Administration (NOAA) Method NMFS-NWFSC-59 2004 is currently used to quantitatively analyze seafood for polycyclic aromatic hydrocarbon (PAH) contamination, especially following events such as the Deepwater Horizon oil rig explosion that released millions of barrels of crude oil into the Gulf of Mexico.Stir bar sorptive extraction (SBSE) is an effective technique to extract trace PAHs in water and the quick, easy, cheap, effective, rugged, and safe (QuEChERS) extraction strategy effectively extracts PAHs from complex food matrices.This study uses SBSE to concentrate PAHs and eliminate matrix interference from QuEChERS extracts of seafood, specifically oysters, fish, and shrimp.

View Article: PubMed Central - PubMed

Affiliation: GERSTEL Inc., 701 Digital Drive, Suite J, Linthicum, MD 21090, USA.

ABSTRACT
National Oceanic and Atmospheric Administration (NOAA) Method NMFS-NWFSC-59 2004 is currently used to quantitatively analyze seafood for polycyclic aromatic hydrocarbon (PAH) contamination, especially following events such as the Deepwater Horizon oil rig explosion that released millions of barrels of crude oil into the Gulf of Mexico. This method has limited throughput capacity; hence, alternative methods are necessary to meet analytical demands after such events. Stir bar sorptive extraction (SBSE) is an effective technique to extract trace PAHs in water and the quick, easy, cheap, effective, rugged, and safe (QuEChERS) extraction strategy effectively extracts PAHs from complex food matrices. This study uses SBSE to concentrate PAHs and eliminate matrix interference from QuEChERS extracts of seafood, specifically oysters, fish, and shrimp. This method provides acceptable recovery (65-138%) linear calibrations and is sensitive (LOD = 0.02 ppb, LOQ = 0.06 ppb) while providing higher throughput and maintaining equivalency between NOAA 2004 as determined by analysis of NIST SRM 1974b mussel tissue.

No MeSH data available.


Related in: MedlinePlus

Total ion chromatography of PAHs in oysters spiked at 25 ng/g.
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Related In: Results  -  Collection


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fig1: Total ion chromatography of PAHs in oysters spiked at 25 ng/g.

Mentions: Since PAHs are ubiquitous, precautions must be taken to ensure background contamination is minimized. Oysters were chosen as the first matrix to test the QuEChERS/SBSE method in seafood because oysters are considered a difficult matrix since the high fat content in oysters may introduce high background interferences [12]. Prior to this study, we have performed SBSE in aqueous solutions containing water-miscible organic solvents for compounds with high Ko/w and found the relative percentage of organic solvent must be optimized for efficient extraction of the target analytes. Based on our previous studies and a study by Ochiai et al. [16], 20% ACN was selected because the log⁡⁡Ko/w for the PAHs of interest ranged between 3.3 and 6.75. Therefore, to perform the SBSE on the QuEChERS extracts, 1.0 mL of the acetonitrile layer was diluted into 4.0 mL water or buffer resulting in a final solution containing 20% ACN. When the optimized extraction conditions were used with the oyster matrix, including the addition of 0.1 M NaHCO3, excellent signal to noise ratio in the SIM mode was obtained (Figure 1). SBSE also provided a concentration factor up to 1000x compared to liquid injection, which enabled quantification of very low levels of analytes. Preliminary SBSE extraction studies evaluated extraction times of 30, 60, and 90 minutes, 4 hours, and 16 hours (overnight) to estimate near-equilibrium conditions. Based on these studies, SBSE extraction time for this matrix was evaluated at 90 minutes or 16 hours. No significant improvement in signal was seen with overnight extraction (data not shown); therefore, a 90-minute extraction was used for all subsequent testing. In addition, incorporating 0.1 M NaHCO3 during SBSE greatly reduced interference due to organic acids and improved signal-to-noise ratios (Figure 2 (A and B)). With routine instrument maintenance, the optimized conditions provided stable chromatography for >200 samples.


A High Throughput Method for Measuring Polycyclic Aromatic Hydrocarbons in Seafood Using QuEChERS Extraction and SBSE.

Pfannkoch EA, Stuff JR, Whitecavage JA, Blevins JM, Seely KA, Moran JH - Int J Anal Chem (2015)

Total ion chromatography of PAHs in oysters spiked at 25 ng/g.
© Copyright Policy - open-access
Related In: Results  -  Collection

Show All Figures
getmorefigures.php?uid=PMC4383357&req=5

fig1: Total ion chromatography of PAHs in oysters spiked at 25 ng/g.
Mentions: Since PAHs are ubiquitous, precautions must be taken to ensure background contamination is minimized. Oysters were chosen as the first matrix to test the QuEChERS/SBSE method in seafood because oysters are considered a difficult matrix since the high fat content in oysters may introduce high background interferences [12]. Prior to this study, we have performed SBSE in aqueous solutions containing water-miscible organic solvents for compounds with high Ko/w and found the relative percentage of organic solvent must be optimized for efficient extraction of the target analytes. Based on our previous studies and a study by Ochiai et al. [16], 20% ACN was selected because the log⁡⁡Ko/w for the PAHs of interest ranged between 3.3 and 6.75. Therefore, to perform the SBSE on the QuEChERS extracts, 1.0 mL of the acetonitrile layer was diluted into 4.0 mL water or buffer resulting in a final solution containing 20% ACN. When the optimized extraction conditions were used with the oyster matrix, including the addition of 0.1 M NaHCO3, excellent signal to noise ratio in the SIM mode was obtained (Figure 1). SBSE also provided a concentration factor up to 1000x compared to liquid injection, which enabled quantification of very low levels of analytes. Preliminary SBSE extraction studies evaluated extraction times of 30, 60, and 90 minutes, 4 hours, and 16 hours (overnight) to estimate near-equilibrium conditions. Based on these studies, SBSE extraction time for this matrix was evaluated at 90 minutes or 16 hours. No significant improvement in signal was seen with overnight extraction (data not shown); therefore, a 90-minute extraction was used for all subsequent testing. In addition, incorporating 0.1 M NaHCO3 during SBSE greatly reduced interference due to organic acids and improved signal-to-noise ratios (Figure 2 (A and B)). With routine instrument maintenance, the optimized conditions provided stable chromatography for >200 samples.

Bottom Line: National Oceanic and Atmospheric Administration (NOAA) Method NMFS-NWFSC-59 2004 is currently used to quantitatively analyze seafood for polycyclic aromatic hydrocarbon (PAH) contamination, especially following events such as the Deepwater Horizon oil rig explosion that released millions of barrels of crude oil into the Gulf of Mexico.Stir bar sorptive extraction (SBSE) is an effective technique to extract trace PAHs in water and the quick, easy, cheap, effective, rugged, and safe (QuEChERS) extraction strategy effectively extracts PAHs from complex food matrices.This study uses SBSE to concentrate PAHs and eliminate matrix interference from QuEChERS extracts of seafood, specifically oysters, fish, and shrimp.

View Article: PubMed Central - PubMed

Affiliation: GERSTEL Inc., 701 Digital Drive, Suite J, Linthicum, MD 21090, USA.

ABSTRACT
National Oceanic and Atmospheric Administration (NOAA) Method NMFS-NWFSC-59 2004 is currently used to quantitatively analyze seafood for polycyclic aromatic hydrocarbon (PAH) contamination, especially following events such as the Deepwater Horizon oil rig explosion that released millions of barrels of crude oil into the Gulf of Mexico. This method has limited throughput capacity; hence, alternative methods are necessary to meet analytical demands after such events. Stir bar sorptive extraction (SBSE) is an effective technique to extract trace PAHs in water and the quick, easy, cheap, effective, rugged, and safe (QuEChERS) extraction strategy effectively extracts PAHs from complex food matrices. This study uses SBSE to concentrate PAHs and eliminate matrix interference from QuEChERS extracts of seafood, specifically oysters, fish, and shrimp. This method provides acceptable recovery (65-138%) linear calibrations and is sensitive (LOD = 0.02 ppb, LOQ = 0.06 ppb) while providing higher throughput and maintaining equivalency between NOAA 2004 as determined by analysis of NIST SRM 1974b mussel tissue.

No MeSH data available.


Related in: MedlinePlus