Advertisement

Analysis of Steroid Estrogens in River Sediment by High Performance Liquid Chromatography-Electrospray Ionization-Mass Spectrometry

  • Sarva Mangala PraveenaEmail author
  • Nur’Aqilah Hamin
  • Siti Quistina Noorain Abdul Razak
  • Ahmad Zaharin Aris
Research Paper

Abstract

This paper describes analysis of steroid estrogens (estrone, estradiol, estriol, and 17α-ethynylestradiol) in river sediment using high performance liquid chromatography (Perkin Elmer FX15) electrospray ionization-mass spectrometry. River sediment samples were prepared by ultrasonic extraction with methanol-dichloromethane, followed by solid phase extraction involving C18 SPE cartridge (500 mg/6 cc). Dissolution was performed using ethyl acetate and methanol, and elution was performed with methanol in ethyl acetate (15 % v/v). The extracts were analyzed by HPLC–MS/MS in multiple reaction monitoring and negative modes with a Zorbax C18 column. Elution was carried out with a gradient of 0.2 % formic acid and methanol with 0.2 % formic acid. The recovery rates from river sediment samples ranged from 90 to 114 %, with relative standard deviations in the range 0.8–17 %. Limit of quantification was determined at 0.02 µg/L all the investigated steroid estrogens. Linear regression analysis was performed for concentrations ranging between 0.02 and 200 µg/L. Coefficient of determination values of more than 0.996 were obtained for all the standard solution calibrations. The method was successfully applied to identify the target analytes in river sediment collected from Langat River (Malaysia) at concentrations of microgram-per-gram in sediment.

Keywords

Endocrine disrupting chemicals Steroid estrogens Liquid chromatography Mass spectrometry 

Notes

Acknowledgments

The authors would like to thank the Kurita Water Research Grant (Japan) for funding with vote number 6385300.

References

  1. Aris AZ, Shamsuddin AS, Praveena SM (2014) Occurrence of 17α-ethynylestradiol (EE2) in the environment and effect on exposed biota: a review. Environ Int 69:104–119. doi: 10.1016/j.envint.2014.04.011 CrossRefGoogle Scholar
  2. Barel-Cohen K, Shore LS, Shemesh M, Wenzel A, Mueller J, Kronfeld-Schor N (2006) Monitoring of natural and synthetic hormones in a polluted river. J Environ Manage 78:16–23. doi: 10.1016/j.jenvman.2005.04.006 CrossRefGoogle Scholar
  3. Baronti C, Curini R, D’Ascenzo G, Di Corcia A, Gentili A, Samperi R (2000) Monitoring natural and synthetic estrogens at activated sludge sewage treatment plants and in a receiving river water. Environ Sci Technol 34:5059–5066. doi: 10.1021/es001359q CrossRefGoogle Scholar
  4. Cullum N (2013) Analysis of steroid residues in wastewater. Anglian Water Services, HungtingdonGoogle Scholar
  5. Hájková K, Pulkrabová J, Schůrek J, Hajšlová J, Poustka J, Nápravníková M, Kocourek V (2007) Novel approaches to the analysis of steroid estrogens in river sediments. Anal Bioanal Chem 387:1351–1363. doi: 10.1007/s00216-006-1026-9 CrossRefGoogle Scholar
  6. Jemal M, Ouyang Z, Teitz DS (1998) High performance liquid chromatography mobile phase composition optimization for the quantitative determination of a carboxylic acid compound in human plasma by negative ion electrospray high performance liquid chromatography tandem mass spectrometry. Rapid Commun Mass Spectrom 12(8):429–434CrossRefGoogle Scholar
  7. Jürgens MD, Williams RJ, Johnson AC (1999) Fate and behaviour of steroid oestrogens in rivers: a scoping study. R&D Technical Report P161. Environment Agency, BristolGoogle Scholar
  8. Koh YKK, Chiu TY, Boobis A, Cartmell E, Lester JN, Scrimshaw MD (2007) Determination of steroid estrogens in wastewater by high performance liquid chromatography-tandem mass spectrometry. J Chromatogr A 1173:81–87. doi: 10.1016/j.chroma.2007.09.074 CrossRefGoogle Scholar
  9. Koren L, Ng ESM, Soma KK, Wynne-Edwards KE (2012) Sample preparation and liquid chromatography-tandem mass spectrometry for multiple steroids in mammalian and avian circulation. PLoS One 7:e32496. doi: 10.1371/journal.pone.0032496 CrossRefGoogle Scholar
  10. Kuster M, De Alda MJ, Barceló D (2004) Analysis and distribution of estrogens and progestogens in sewage sludge, soils and sediments. TrAC Trends Anal Chem 23:790–798. doi: 10.1016/j.trac.2004.08.007 CrossRefGoogle Scholar
  11. Lai KM, Johnson KL, Scrimshaw MD, Lester JN (2000) Binding of waterborne steroid estrogens to solid phases in river and estuarine systems. Environ Sci Technol 34:3890–3894. doi: 10.1021/es9912729 CrossRefGoogle Scholar
  12. l-Odaini NA, Zakaria MP, Yaziz MI, Surif S, Kannan N (2013) Occurrence of synthetic hormones in sewage effluents and Langat River and its tributaries, Malaysia. Int J Environ Anal Chem 93:1457–1469. doi: 10.1080/03067319.2012.727810 CrossRefGoogle Scholar
  13. López de Alda MJ, Gil A, Paz E, Barceló D (2002) Occurrence and analysis of estrogens and progestogens in river sediments by liquid chromatography-electrospray-mass spectrometry. Analyst 127:1299–1304. doi: 10.1039/b207658f CrossRefGoogle Scholar
  14. Mikel C (2010) Letters to the editor a tale of two drug testing technologies: GC-MS and LC–MS/MS THE are independent medical examiners. Pain Phys 13:91–92.Google Scholar
  15. Nováková L, Matysová L, Solich P (2006) Advantages of application of UPLC in pharmaceutical analysis. Talanta 68:908–918. doi: 10.1016/j.talanta.2005.06.035 CrossRefGoogle Scholar
  16. Peck M, Gibson RW, Kortenkamp A, Hill EM (2004) Sediments are major sinks of steroidal estrogens in two United Kingdom rivers. Environ Toxicol Chem 23:945–952. doi: 10.1897/03-41 CrossRefGoogle Scholar
  17. Peng X, Wang Z, Yang C, Chen F, Mai B (2006) Simultaneous determination of endocrine-disrupting phenols and steroid estrogens in sediment by gas chromatography-mass spectrometry. J Chromatogr A 1116:51–56. doi: 10.1016/j.chroma.2006.03.017 CrossRefGoogle Scholar
  18. Ternes TA, Stumpf M, Mueller J, Haberer K, Wilken RD, Servos M (1999) Behavior and occurrence of estrogens in municipal sewage treatment plants—I. Investigations in Germany, Canada and Brazil. Sci Total Environ 225:81–90. doi: 10.1016/S0048-9697(98)00334-9 CrossRefGoogle Scholar
  19. Ternes TA, Andersen H, Gilberg D, Bonerz M (2002) Determination of estrogens in sludge and sediments by liquid extraction and GC/MS/MS. Anal Chem 74:3498–3504. doi: 10.1021/ac015717z CrossRefGoogle Scholar
  20. Zhang R, Tang J, Li J, Cheng Z, Chaemfa C, Liu D, Zheng Q, Song M, Luo C, Zhang G (2013) Occurrence and risks of antibiotics in the coastal aquatic environment of the Yellow Sea, North China. Sci Total Environ 450–451:197–204. doi: 10.1016/j.scitotenv.2013.02.024 CrossRefGoogle Scholar
  21. Zhang Z, Ren N, Kannan K, Nan J, Liu L, Ma W, Qi H, Li Y (2014) Occurrence of endocrine-disrupting phenols and estrogens in water and sediment of the Songhua River, Northeastern China. Arch Environ Contam Toxicol 66:361–369. doi: 10.1007/s00244-014-9998-5 CrossRefGoogle Scholar
  22. Zhao J-L, Ying G-G, Chen F, Liu Y-S, Wang L, Yang B, Liu S, Tao R (2011) Estrogenic activity profiles and risks in surface waters and sediments of the Pearl River system in South China assessed by chemical analysis and in vitro bioassay. J Environ Monit 13:813–821. doi: 10.1039/c0em00473a CrossRefGoogle Scholar

Copyright information

© Shiraz University 2016

Authors and Affiliations

  1. 1.Department of Environmental and Occupational Health, Faculty of Medicine and Health SciencesUniversiti Putra MalaysiaSerdangMalaysia
  2. 2.Department of Environmental Sciences, Faculty of Environmental StudiesUniversiti Putra MalaysiaSerdangMalaysia

Personalised recommendations