Journal
FOOD ADDITIVES AND CONTAMINANTS PART A-CHEMISTRY ANALYSIS CONTROL EXPOSURE & RISK ASSESSMENT
Volume 35, Issue 3, Pages 458-466Publisher
TAYLOR & FRANCIS LTD
DOI: 10.1080/19440049.2017.1411617
Keywords
UHPLC-MS; MS; stilbenes; confirmatory; serum; acid treatment
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A simple and accurate ultra-high-performance liquid chromatography tandem mass spectrometry (UHPLC-MS/MS) method was developed and validated for the first time as a confirmatory method for the simultaneous determination of stilbenes - hexestrol and diethylstibestrol in serum. Extraction was based on a simple acid denaturation of protein followed by liquid-liquid extraction using methyl tert butyl ether. Extracts were directly injected into the UHPLC-MS/MS without further purification. Excellent recoveries in the range 82-99% and 91-128% were obtained for hexestrol and diethylstibestrol, respectively. Both within-day repeatability and between-day reproducibility were generally satisfactory with RSD <20%. The linearity of the internal standard based matrix-matched calibration curve measured as the coefficient of regression (r(2)) was generally >0.99 for both hexestrol and diethylstibestrol. Both matrix effect and uncertainties associated with sample preparation and instrumental analysis were significantly reduced with the use of a deuterated compound (hexestrol-d4) as internal standard. The LOD and LOQ were 0.09 and 0.08ng/ml, and 0.28 and 0.25ng/ml, respectively, for hexestrol and diethylstibestrol. The method was found to be suitable for the simultaneous determination of hexestrol and diethylstibestrol in serum.
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