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Sensitive Determination of Natural and Synthetic Steroidal Hormones of a Free and Conjugated Form in Surface Water by Gas Chromatography-Mass Spectrometry

  • Shin, Ho-Sang (Department of Environmental Education, Kongju National University) ;
  • Oh, Jin-Aa (Department of Environmental Science, Kongju National University) ;
  • Shin, Sun-Kyoung (Division of Chemicals Behavior Research, Department of Environmental Health Risk Research, National Institute of Environmental Research, Environmental Research Complex)
  • Received : 2010.09.18
  • Accepted : 2010.12.27
  • Published : 2011.03.20

Abstract

A method based on the TMS derivatives and acidic hydrolysis was developed for the simultaneous determination of free and conjugated steroidal hormones in surface water. A silylation of five natural and two synthetic steroidal hormones was achieved with N-methyl-N-(trimethylsilyl) trifluoroacetamide/$NH_4I$ (1000:3) under catalysis of dithioerythritol for 60 min at $80^{\circ}C$. TMS derivatives of the steroid hormones containing multifunctional groups offer a single derivative product under this condition. The accuracy of the analytes was in the range of 87 to 110% at a concentration of 20 and 50 ng/L with relative standard deviations of less than 10%. The method detection limit was in the range of 0.01 to 0.02 ng/L for surface water. Natural steroidal hormones were detected in a concentration range of 0 to 1.03 ng/L in free form and 0 to 14.6 ng/L in conjugated form, respectively. We found that most of the natural hormonal steroids exist in conjugate forms (43 to 100%) in river water.

Keywords

References

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