GC-MS Determination of Steroid Estrogens in Water after Solid Phase Extraction Separation and Derivatization

GC-MS with SPE separation and derivatization was applied to the simultaneous determination of estrone (E1), 17β-estradiol (E2), 17α-ethynylestradoil (EE2) and estriol (E3) in water.The sample was separated on Oasis HLB SPE column and the column was eluted with acetone. The eluate was derivatized with pyridine and N-Methyl-N-(trimethylsilyl)trifluoroacetamide at 40 ℃ for 20 min, and the derivates were then analyzed by GC-MS. The linearity ranges of E1, E2, EE2 and E3 were 5.00-500 μg·L-1 and 10.0-500 μg·L-1, respectively. The detection limits (3S/N) and the limits of quantification (10S/N) were in the ranges of 1.5-3.0 μg·L-1 and 5.0-10 μg·L-1 respectively. Recovery found by standard addition method were in the range of 86.8%-93.8% and RSDs (n=7) found were in the range of 7.1%-11%.