Development of a sample enrichment probe method for the gas chromatography-mass spectrometry analysis of hormones in water
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Date
2019
Authors
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Publisher
University of Namibia
Abstract
A simple sample enrichment probe (SEP) sampling method was developed for the
determination of endogenous steroid hormones (estrone, I 7P-estradiol and
testosterone) in water using gas chromatography-mass spectrometry (GC-MS). SEPs constructed of thin stainless steel rods of inert material or sections of a polyimide coated megabore GC column provided at one end with a short sleeve of
polydimethylsiloxane (PDMS) rubber as the sorbent material were used. The selected target hormones were estrone, I 7P-estradiol and testosterone. Extraction of the steroid hormones was performed by direct immersion of the SEP in water samples. To maximise the extraction efficiency of the SEP method to extract the analytes, several parameters affecting the extraction efficiency of the SEP method, such as extraction time, extraction temperature, pH and ionic strength were optimised. Due to challenges encountered with the GC-MS the method was only partially validated using ultra-pure water samples spiked with hormones at different concentration levels. Under the optimal conditions, the method showed satisfactory linearity over a concentration range of 1-10 μg/mL (for estrone and testosterone) and 2-10 μg/mL (for estradiol), with regression squares (R2) ranging between 0.988-0.996. Acceptable reproducibility in the range of 2-17 % RSD was achieved. The obtained limits of quantitation (LOQs) were 0.5 μg/mL for the three steroids. Although the SEP-GC-MS method gave very high LOQs when compared to existing SPME and SBSE methods, it proved to be a simple and cost-effective alternative to these methods.
Description
A thesis submitted in partial fulfilment of the requirements for the degree of Master Science (Chemistry)
Keywords
Chromatography-mass spectrometry, Polydimethylsiloxane, Steroid hormones