http://dx.doi.org/10.4322/sc.2014.024

Analysis of steroids using solid phase microextraction-gas chromatography-mass spectrometry-mass spectrometry (SPME-GC-MS-MS)

Chopra, Shilpi; Gomes, Paulo C. F. L.; Dhandapani, Ramkumar; Snow, Nicholas H.

Palavras-chave: Steroids using Solid Phase Microextraction, SPME, Gas Chromatography-Mass Spectrometry-Mass Spectrometry, GC-MS-MS, SPME-GC-MS-MS, water analysis.

Resumo: Direct immersion SPME-GC-MS-MS was used for the analysis of steroids in water at part-per-trillion(ppt) and lower concentrations. The method was validated and extended to real sample analysis. The method were linear from 0.01 to 5 ng/ml with precision less than 10% relative standard deviation for a steroid mixture at 1 ng/ml. Limit of quantitation and limit of detection was found to be 200- 1200 pg/L and 30-200 pg/L respectively and recoveries ranged from 88-103 %. To understand the extraction efficiency of the fiber, a depletion study was performed. The fiber/ sample partition coefficients for the steroids were determined to be 1.0 x 104 to 1.5 x 104. The extraction was performed without derivatization or the use of an internal standard. SPME-GC-MS-MS effectively demonstrated ultra-trace level detection of steroids in water.


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