Study of QuEChERS and Magnetic Dispersive Solid Phase Extraction for the Determination of Steroids in Human Urine by LC-MS/MS

• Main Authors: Chen, Yi-An, 陳怡安
• Other Authors: Lee, Hui-Ling
• Format: Others
• Language: zh-TW
• Published: 2016
• Online Access: http://ndltd.ncl.edu.tw/handle/82572418247160757150

碩士 === 輔仁大學 === 化學系 === 104 === Endocrine disrupting chemicals (EDCs) are typically identified as compounds that can interact with steroids synthesis, transport and metabolism. In this way, steroids may impact endocrine system abnormal and hormone dependent cancers. In this study, human urine samples can be pre-concentrated and clean-up by sample preparation and simultaneous determination of six steroids hormones (progesterone, 17α-hydroxyprogesterone, dehydroepiandrosterone, testosterone, cortisol, and cortisone) combined with liquid chromatography tandem mass spectrometry (LC-MS/MS). The sample preparation methods included QuEChERS (Quick, Easy, Cheap, Effective, Rugged, and Safe) and magnetic solid phase extraction (mSPE). The QuEChERS optimal parameters, extraction solvent for the liquid–liquid extraction (LLE) was 600 µL of methyl tert-butyl ether (MTBE) and clean-up with 10 mg of hydroxyapatite (HAp). In addition to, the mSPE optimal adsorption material and eluted solvent were 10 mg Fe3O4@SiO2@C18 and 400 µL of MTBE, respectively. The coefficients of correlation (r2) for the calibration curves were greater than 0.9997. The limits of detection (LOD) and limits of quantification (LOQ) were determined to within 0.03 to 0.57 ng/mL and 0.10 to 1.89 ng/mL. The recoveries of steroids in spike urine by QuEChERS and mSPE were 87.55% to 110.93% and 92.72 % to 107.48, respectively, with a standard deviation range from 1.82 to 18.68 and 3.75 to 14.03, respectively. These results shown that two sample preparations could be simple and rapid extraction steroids and remove matrix effect from human urine sample.