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.

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.

[1]  N. Rose,et al.  Current-use brominated flame retardants in water, sediment, and fish from English lakes. , 2009, Environmental science & technology.

[2]  Glenn R Wilson,et al.  Determination of parent and substituted polycyclic aromatic hydrocarbons in high-fat salmon using a modified QuEChERS extraction, dispersive SPE and GC-MS. , 2011, Journal of agricultural and food chemistry.

[3]  J. Cochran.  Fast gas chromatography-time-of-flight mass spectrometry of polychlorinated biphenyls and other environmental contaminants. , 2002, Journal of chromatographic science.

[4]  A. Covaci,et al.  Novel brominated flame retardants: a review of their analysis, environmental fate and behaviour. , 2011, Environment international.

[5]  J. M. Keller,et al.  Determination of polybrominated diphenyl ethers in environmental standard reference materials , 2007, Analytical and bioanalytical chemistry.

[6]  R. Hites,et al.  Novel flame retardants, 1,2-bis(2,4,6-tribromophenoxy)ethane and 2,3,4,5,6-pentabromoethylbenzene, in United States' environmental samples. , 2005, Environmental science & technology.

[7]  C. Marvin,et al.  Dechlorane plus levels in sediment of the lower Great Lakes. , 2008, Environmental science & technology.

[8]  C. Marvin,et al.  Isomers of dechlorane plus in Lake Winnipeg and Lake Ontario food webs. , 2007, Environmental science & technology.

[9]  Ed Sverko,et al.  Compounds structurally related to Dechlorane Plus in sediment and biota from Lake Ontario (Canada). , 2010, Environmental science & technology.

[10]  P. Ivester,et al.  The content of favorable and unfavorable polyunsaturated fatty acids found in commonly eaten fish. , 2008, Journal of the American Dietetic Association.

[11]  Yoko S Johnson.  Determination of polycyclic aromatic hydrocarbons in edible seafood by QuEChERS-based extraction and gas chromatography-tandem mass spectrometry. , 2012, Journal of food science.

[12]  H. Stapleton,et al.  Measurement of flame retardants and triclosan in municipal sewage sludge and biosolids. , 2012, Environment international.

[13]  A. Schecter,et al.  Polybrominated Diphenyl Ethers (PBDEs) and Hexabromocyclodecane (HBCD) in Composite U.S. Food Samples , 2009, Environmental health perspectives.

[14]  Steven J Lehotay,et al.  Fast and easy multiresidue method employing acetonitrile extraction/partitioning and "dispersive solid-phase extraction" for the determination of pesticide residues in produce. , 2003, Journal of AOAC International.

[15]  Steven J Lehotay,et al.  Fast, low-pressure gas chromatography triple quadrupole tandem mass spectrometry for analysis of 150 pesticide residues in fruits and vegetables. , 2011, Journal of chromatography. A.

[16]  L. Birnbaum,et al.  Brominated flame retardants: cause for concern? , 2003, Environmental health perspectives.

[17]  A. Gelbin,et al.  Retention-time database of 126 polybrominated diphenyl ether congeners and two bromkal technical mixtures on seven capillary gas chromatographic columns. , 2005, Journal of chromatography. A.

[18]  S. Tittlemier,et al.  Identilication of the novel cycloaliphatic brominated flame retardant 1,2-dibromo-4-(1,2-dibromoethyl)cyclohexane in Canadian Arctic beluga (Delphinapterus leucas). , 2008, Environmental science & technology.

[19]  A. G. Frenich,et al.  Trace determination of organotin compounds in water, sediment and mussel samples by low-pressure gas chromatography coupled to tandem mass spectrometry. , 2003, Rapid communications in mass spectrometry : RCM.

[20]  S. Sakai,et al.  Brominated flame retardants and other polyhalogenated compounds in indoor air and dust from two houses in Japan. , 2009, Chemosphere.

[21]  C. Tohyama,et al.  The 2005 World Health Organization reevaluation of human and Mammalian toxic equivalency factors for dioxins and dioxin-like compounds. , 2006, Toxicological sciences : an official journal of the Society of Toxicology.

[22]  Y. Sun,et al.  Organochlorine Pesticides in Tissues of Catfish (Silurus asotus) from Guanting Reservoir, People's Republic of China , 2006, Bulletin of environmental contamination and toxicology.

[23]  Koichi Saito,et al.  Development of a accelerated solvent extraction and gel permeation chromatography analytical method for measuring persistent organohalogen compounds in adipose and organ tissue analysis. , 2004, Chemosphere.

[24]  Miss A.O. Penney.  (b) , 1974, The New Yale Book of Quotations.

[25]  Steven J Lehotay,et al.  Ruggedness and other performance characteristics of low-pressure gas chromatography-mass spectrometry for the fast analysis of multiple pesticide residues in food crops. , 2004, Journal of chromatography. A.

[26]  K. Ravindra,et al.  Low-pressure gas chromatography-ion trap mass spectrometry for the fast determination of polycyclic aromatic hydrocarbons in air samples. , 2006, Journal of chromatography. A.

[27]  A. Covaci,et al.  Persistent chlorinated pesticides and polychlorinated biphenyls in selected fish species from Lake Tanganyika, Burundi, Africa. , 2002, Environmental pollution.

[28]  H. Neels,et al.  Fast analysis of decabrominated diphenyl ether using low-pressure gas chromatography-electron-capture negative ionization mass spectrometry. , 2008, Journal of chromatography. A.

[29]  D. Schlenk,et al.  Pesticides and PCBs in sediments and fish from the Salton Sea, California, USA. , 2004, Chemosphere.

[30]  J. Douwes,et al.  Occurrence of alternative flame retardants in indoor dust from New Zealand: indoor sources and human exposure assessment. , 2012, Chemosphere.

[31]  A. Schecter,et al.  A comparison of dioxins, dibenzofurans and coplanar PCBs in uncooked and broiled ground beef, catfish and bacon. , 1998, Chemosphere.

[32]  M. Wong,et al.  Residual levels of DDTs and PAHs in freshwater and marine fish from Hong Kong markets and their health risk assessment. , 2007, Chemosphere.

[33]  Shinsuke Tanabe,et al.  Temporal trends of brominated flame retardants in coastal waters of Japan and South China: retrospective monitoring study using archived samples from es-Bank, Ehime University, Japan. , 2008, Marine pollution bulletin.

[34]  Yawei Wang,et al.  Evaluation of Soxhlet extraction, accelerated solvent extraction and microwave-assisted extraction for the determination of polychlorinated biphenyls and polybrominated diphenyl ethers in soil and fish samples. , 2010, Analytica chimica acta.

[35]  I. Meerts,et al.  In vitro estrogenicity of polybrominated diphenyl ethers, hydroxylated PDBEs, and polybrominated bisphenol A compounds. , 2001, Environmental health perspectives.

[36]  Jana Hajslova,et al.  Implementation of comprehensive two-dimensional gas chromatography–time-of-flight mass spectrometry for the simultaneous determination of halogenated contaminants and polycyclic aromatic hydrocarbons in fish , 2012, Analytical and Bioanalytical Chemistry.

[37]  Ian T Cousins,et al.  Modelling PCB bioaccumulation in a Baltic food web. , 2007, Environmental pollution.

[38]  Jana Hajslova,et al.  Simplified and rapid determination of polychlorinated biphenyls, polybrominated diphenyl ethers, and polycyclic aromatic hydrocarbons in fish and shrimps integrated into a single method. , 2011, Analytica chimica acta.

[39]  C. D. de Wit,et al.  Brominated flame retardants in the Arctic environment--trends and new candidates. , 2010, The Science of the total environment.

[40]  Heather M. Stapleton,et al.  Alternate and new brominated flame retardants detected in U.S. house dust. , 2008 .

[41]  C. Marvin,et al.  Enantioselective bioaccumulation of hexabromocyclododecane and congener-specific accumulation of brominated diphenyl ethers in an eastern Canadian Arctic marine food web. , 2008, Environmental science & technology.

[42]  Shui Miao,et al.  High throughput analysis of 150 pesticides in fruits and vegetables using QuEChERS and low-pressure gas chromatography-time-of-flight mass spectrometry. , 2010, Journal of chromatography. A.

[43]  W. Vilegas,et al.  Application of low-pressure gas chromatography-ion-trap mass spectrometry to the analysis of the essential oil of Turnera diffusa (Ward.) Urb. , 2004, Journal of chromatography. A.

[44]  A. Polder,et al.  A comparison of PCB bioaccumulation factors between an arctic and a temperate marine food web. , 2010, The Science of the total environment.

[45]  C. Marvin,et al.  The analysis of halogenated flame retardants by GC-HRMS in environmental samples. , 2009, Journal of chromatographic science.

[46]  S. Tittlemier,et al.  Structure characterization and thermal stabilities of the isomers of the brominated flame retardant 1,2-dibromo-4-(1,2-dibromoethyl)cyclohexane. , 2008, Chemosphere.

[47]  H. Campbell,et al.  Diet , 1906, The Hospital.