HPLC/ESI-MS/MS를 이용한 환경 시료중 Estrogens의 분석
The Analysis of Estrogen in Environmental Samples by HPLC/ESI-MS/MS
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Trace concentrations of estrogens such as 17β-estradiol (E2), 17α-estradiol (αE2), estrone (E1), estriol (E3),and 17α-ethinylestradiol (EE2) may have adverse effects on humans and the aquatic ecosystem. The environmental analysis of estrogens at physiologically active concentrations (low ng/L) requires the use of very sensitive and selective method. An analytical procedure for the simultaneous determination of five steroid estrogens in an aqueous environmental sample is described. The procedure includes solid phase extraction/clean-up with C18 cartridge, and analysis by liquid chromatography/tan dem mass spectrometry of five estrogens. After 500 mL of sample loading on C18 cartridge, sample was eluted with acetonitrile and dryness. The reconstituted analytes were separated on HPLC system with 0.1% formic acid and acetonitrile followed by analyzed using (-) electrospray ionization - mass spectrometer with multiple reaction monitoring mode. In the range of 0.05 - 1 ng/mL, the calibration curves were showed the good linearities (above r2=0.99). The limits of detection and limits of quatitation estimated for the estrogens in blank surface water were the concentration range of 0.055~0.154 ng/mL and 0.184~0.514 ng/mL, respectively. The absolute recovery, precision (intra-day)and accuracy in the low, medium and high (0.005~1.0 ng/mL) were in the range of 69.5~95.1%, 0.4 ~7.9%(RSD) and -9.1~9.3% (bias), respectively.
Abstract
Trace concentrations of estrogens such as 17β-estradiol (E2), 17α-estradiol (αE2), estrone (E1), estriol (E3),and 17α-ethinylestradiol (EE2) may have adverse effects on humans and the aquatic ecosystem. The environmental analysis of estrogens at physiologically active concentrations (low ng/L) requires the use of very sensitive and selective method. An analytical procedure for the simultaneous determination of five steroid estrogens in an aqueous environmental sample is described. The procedure includes solid phase extraction/clean-up with C18 cartridge, and analysis by liquid chromatography/tan dem mass spectrometry of five estrogens. After 500 mL of sample loading on C18 cartridge, sample was eluted with acetonitrile and dryness. The reconstituted analytes were separated on HPLC system with 0.1% formic acid and acetonitrile followed by analyzed using (-) electrospray ionization - mass spectrometer with multiple reaction monitoring mode. In the range of 0.05 - 1 ng/mL, the calibration curves were showed the good linearities (above r2=0.99). The limits of detection and limits of quatitation estimated for the estrogens in blank surface water were the concentration range of 0.055~0.154 ng/mL and 0.184~0.514 ng/mL, respectively. The absolute recovery, precision (intra-day)and accuracy in the low, medium and high (0.005~1.0 ng/mL) were in the range of 69.5~95.1%, 0.4 ~7.9%(RSD) and -9.1~9.3% (bias), respectively.
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