Simultaneous Determination of Four Estrogens in Compost Based on Ultrasonic Solvent Extraction, Solid-Phase Extraction Clean-Up and Analysis by UHPLC-MS/MS
A rapid, cost
effective and reliable analytical method was developed and validated for the
simultaneous determination of four estrogens (17 β-estradiol, 17 α-ethinylestradiol,
estrone, and estriol) in compost samples from the biodegradation of biological
infectious hazardous wastes. Ultrasonic solvent extraction, using methanol as
extraction solvent, coupled with SPE clean-up, using cartridges HLB 60 mg - 6
ml Supelco® and acetonitrile for reconstitution of eluents, was used
for the simultaneous extraction of the four estrogens. Mean recoveries in the
range of 98% - 107% were obtained. All compounds were separated in a single
gradient run by UHPLC KinetexTM 2.6 μm XB-C18 100 Å LC (50 × 4.6 mm) column. Analytes
were detected via multiple reaction monitoring (MRM) using an AB SCIEX
API-5000TM triple quadrupole (Applied Biosystems/MDS SCIEX) with electrospray
ionization in negative mode. Isocratic mobile phase of Water:ACN (50:50)
resulted to be the optimum. Limits of detection and quantification were on the
order of 0.66 ng·g-1 and 2 ng·g-1 for all the estrogens.
These limits were lower than most of the values reported in the literature for
similar matrices. Suitable level of linearity, good repeatability and
reproducibility with coefficients of variation is lower than 11.7%, 6.8% and
8.3%, respectively.
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