Alkaline Digestion and Solid Phase Extraction Method for Perfluorinated Compounds in Mussels and Oysters from South China and Japan

  • M. K. So
  • S. Taniyasu
  • P. K. S. LamEmail author
  • G. J. Zheng
  • J. P. Giesy
  • N. Yamashita


Perfluorinated compounds (PFCs), such as perfluorooctane sulfonate (PFOS), have been identified in the coastal waters of China and Japan. An alkaline digestion method, coupled with solid-phase extraction (SPE), and high-performance liquid chromatography interfaced with high-resolution electrospray tandem mass spectrometry was developed to determine PFCs in mussel and oyster samples from coastal waters of south China and Japan. These techniques produced adequate recoveries and reporting limits with small quantities of PFCs. Concentrations of individual PFCs in mussels and oysters from south China and Japan ranged from 113.6 to 586.0 pg/g, wet weight (ww) for PFOS, 63.1 to 511.6 pg/g, ww for perfluorohexane sulfonate, 9.3 to 30.1 pg/g, ww for perfluorobutane sulfonate and 37.8 to 2957.0 pg/g, ww for perfluorooctane sulfonamide. The quantification of perfluorinated carboxylates was compromised by interferences from carboxylates in the procedural blanks. Perfluoroundecanoate and perfluorononanoate had relatively great blank interferences, which resulted in relatively poor limits of quantification for these compounds. Some PFCs were only identified in a limited number of samples: perfluorododecanoate in samples from Tokyo Bay, Japan (195.9 pg/g, ww); and perfluorodecanoate in Fuzhou, China (131.7 pg/g, ww) and Tokyo Bay (118.6 pg/g, ww). The greatest concentrations of perfluorooctanoate, perfluoroheptanoate, and perfluorohexanoate were observed in samples from Tokyo Bay and Bei Hai, south China.


Target Analytes Procedural Blank Oyster Tissue Perfluorooctane Sulfonate Electrospray Tandem Mass Spectrometry 
These keywords were added by machine and not by the authors. This process is experimental and the keywords may be updated as the learning algorithm improves.



This study was supported by the Area of Excellence Scheme under the University Grants Committee of the Hong Kong Special Administration Region, China (Project No. AoE/P-04/2004), and a RGC-CERG (cityU1401/05M).


  1. Fu J, Mai B, Sheng G, Zhang G, Wang X, Peng P, Xiao X, Ran R, Cheng F, Peng X, Wang Z, Tang UW (2003) Persistent organic pollutants in environment of the Pearl River Delta, China: An overview. Chemosphere 52:1411–1422CrossRefGoogle Scholar
  2. Hoff PT, Van de Vijver K, Van Dongen W, Esmans EL, Blust R, De Coen WM (2003) Perfluorooctane sulfonic acid in bib (Trisopterus luscus) and plaice (Pleuronectes platessa) from the Western Scheldt and the Belgian North Sea: Distribution and biochemical effects. Environ Toxicol Chem 22:608–614CrossRefGoogle Scholar
  3. Kannan K, Koistinen J, Beckmen K, Evans T, Gorzelany JF, Hansen KJ, Jones PD, Helle E, Nyman M, Giesy JP (2001) Accumulation of perfluorooctane sulfonate in marine mammals. Environ Sci Technol 35:1593–1598Google Scholar
  4. Kannan K, Hansen KJ, Wade TL, Giesy JP (2002) Perfluorooctane sulfonate in oysters, Crassostrea virginica, from the Gulf of Mexico and the Chesapeake Bay, USA. Arch Environ Contam Toxicol 42:313–318Google Scholar
  5. Kuklenyik Z, Reich JA, Tully JS, Needham LL, Calafat AM (2004) Automated solid-phase extraction and measurement of perfluorinated organic acids and amides in human serum and milk. Environ Sci Technol 38:3698–3704CrossRefGoogle Scholar
  6. Mai BX, Fu JM, Sheng GY, Kang YH, Lin Z, Zhang G, Min YS, Zeng EY (2002) Chlorinated and polycyclic aromatic hydrocarbons in riverine and estuarine sediments from Pearl River Delta, China. Environ Pollut 117:457–474CrossRefGoogle Scholar
  7. Martin JW, Mabury SA, Solomon KR, Muir DCG (2003a) Dietary accumulation of perfluorinated acids in juvenile rainbow trout (Oncorhynchus mykiss). Environ Toxicol Chem 22:189–195Google Scholar
  8. Martin JW, Mabury SA, Solomon KR, Muir DCG (2003b) Bioconcentration and tissue distribution of perfluorinated acids in rainbow trout (Oncorhynchus mykiss). Environ Toxicol Chem 22:196–204Google Scholar
  9. Martin JW, Kannan K, Berger U, Voogt PD, Field J, Franklin J, Giesy JP, Harner T, Muir DCG, Scott B, Kaiser M, Järnberg U, Jones KC, Mabury SA, Schroeder H, Simcik M, Sottani C, Bavel BV, Kärrman A, Lindström G, Leeuwen SV (2004a) Analytical challenges hamper perfluoroalkyl research. Environ Sci Technol 248A–255AGoogle Scholar
  10. Martin JW, Smithwick MM, Braune BM, Hoekstra PF, Muir DCG, Mabury SA (2004b) Identification of long-chain perfluorinated acids in biota from the Canadian Arctic. Environ Sci Technol 38:373–380Google Scholar
  11. Monirith I, Ueno D, Takahashi S, Nakata H, Sudaryanto A, Subramanian A, Karuppiah S, Ismail A, Muchtar M, Zheng J, Richardson BJ, Prudente M, Hue ND, Tana TS, Tkalin AV, Tanabe S (2003) Asia-Pacific mussel watch: monitoring contamination of persistent organochlorine compounds in coastal waters of Asian countries. Mar Pollut Bull 46:281–300Google Scholar
  12. Moody CA, Martin JW, Kwan WC, Muir DCG, Mabury SA (2002) Monitoring perfluorinated surfactants in biota and surface water samples following an accidental release of fire-fighting foam into Etobicoke Creek. Environ Sci Technol 36:545–551CrossRefGoogle Scholar
  13. Olsen GW, Burris JM, Mandel JH, Zobel LR (1999) Serum perfluorooctane sulfonate and hepatic and lipid clinical chemistry tests in fluorochemical production employees. J Occup Environ Med 41:799–806Google Scholar
  14. Olsen GW, Hansen KJ, Stevenson LA, Burris JM, Mandel JH (2003) Human donor liver and serum concentrations of perfluorooctanesulfonate and other perfluorochemicals. Environ Sci Technol 37:888–891Google Scholar
  15. So MK, Taniyasu S, Yamashita N, Giesy JP, Zheng J, Fang Z, Im SH, Lam PKS (2004) Perfluorinated compounds in coastal waters of Hong Kong, South China and Korea. Environ Sci Technol 38:4056–4063CrossRefGoogle Scholar
  16. Tomy GT, Tittlemier SA, Palace VP, Budakowski WR, Braekevelt E, Brinkworth L, Friesen K (2004) Biotransformation of N-ethyl perfluorooctanesulfonamide by rainbow trout (Onchorhynchus mykiss) liver microsomes. Environ Sci Technol 38:758–762Google Scholar
  17. Van de Vijver KI, Hoff PT, Van Dongen W, Esmans EL, Blust R, De Coen WM (2003) Exposure patterns of perfluorooctane sulfonate in aquatic invertebrates from the Western Scheldt estuary and the Southern North Sea. Environ Toxicol Chem 22:2037–2041Google Scholar
  18. Van de Vijver KI, Hoff PT, Das K, Van Dongen W, Esmans EL, Siebert U, Bouquegneau JM, Blust R, De Coen WM (2004) Baseline study of perfluorochemicals in harbour porpoises (Phocoena phocoena) from Northern Europe. Mar Pollut Bull 48:992–997Google Scholar
  19. Yang YH, Sheng GY, Fu JM, Min YS (1997) Organochlorinated compounds in waters of the Pearl River Delta region. Environ Monit Assess 44:569–575Google Scholar

Copyright information

© Springer Science+Business Media, Inc. 2005

Authors and Affiliations

  • M. K. So
    • 1
  • S. Taniyasu
    • 2
  • P. K. S. Lam
    • 1
    Email author
  • G. J. Zheng
    • 1
  • J. P. Giesy
    • 1
    • 3
  • N. Yamashita
    • 2
  1. 1.Centre for Coastal Pollution and Conservation, Department of Biology and ChemistryCity University of Hong KongKowloonPeoples Republic of China
  2. 2.National Institute of Advanced Industrial Science and Technology (AIST)TsukubaJapan
  3. 3.Department of ZoologyNational Food Safety and Toxicology Center, Center for Integrative Toxicology, Michigan State UniversityEast LansingUSA

Personalised recommendations