Development of an analytical method of 17.BETA.-estradiol in river water by liquid chromatography/tandem mass spectrometry.

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  • TAJIMA Haruhiko
    Chemicals Evaluation and Research Institute,Kurume Laboratory,19-14,Chuoh-machi,Kurume-shi,Fukuoka 830-0023
  • TSUJIMURA Kazunari
    Chemicals Evaluation and Research Institute,Kurume Laboratory,19-14,Chuoh-machi,Kurume-shi,Fukuoka 830-0023
  • YAMAGUCHI Masatoshi
    Faculty of Pharmaceutical Sciences,Fukuoka University,8-19-1,Nanakuma,Johnan-ku,Fukuoka 814-0180

Bibliographic Information

Other Title
  • 液体クロマトグラフィー／タンデム質量分析法による河川水及び下水放流水中の１７β‐エストラジオール分析法の開発
  • 液体クロマトグラフィー/タンデム質量分析法による河川水及び下水放流水中の17β-エストラジオール分析法の開発
  • エキタイ クロマトグラフィー タンデム シツリョウ ブンセキホウ ニ ヨル カセンスイ オヨビ ゲスイ ホウリュウ スイチュウ ノ 17 ベータ エスト ラジオ ール ブンセキホウ ノ カイハツ

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Abstract

A sensitive method for the determination of 17β-estradiol, estrone and estriol in river water has been developed, based on SPE cartridge extraction and HPLC coupled with negative electron ion spray tandem mass spectrometry(LC/MS/MS)in the multiple reaction monitoring mode(MRM).An internal standard calibration method using a stable isotopic labeled 17β-estradiol was employed for quantitation.The limit of detection(LOD)for these estrogens in river water was 0.3ng/l.Good linearities of the calibration curve were obtained in the concentration range from 0.4ng/l to 80ng/l.The correlation coefficients were>0.995 for all estrogens.The recoveries of these estrogens were 65.9∼96.9%.The relative standard deviations were 5.8∼11.1% for 0.4ng/l, 8.1∼11.8% for 0.8ng/l, 4.2∼12.6ng/l for 1.6ng/l.Using this method, the behavior and occurrence of estrogens in river water and the effluent of sewage treatment plants were investigated in Chikugo-river(Kyusyu, Japan).A few estrogens were detected in the river water by LC/MS/MS, and the levels were ND-0.6ng/l.However, in all samples of sewage-treatment plants, 17β-estradiol and estrone were detected, and the levels were 0.5∼4.2ng/l(17β-estradiol)and 5.3∼35.1ng/l(estrone).On the other hand, 17β-estradiol was detected in most samples, including river water, by ELISA(17/18);the levels in sewage-treatment plants were 6.0∼13.5 times higher than those by LC/MS/MS.The differences in these results might be due to the cross reaction of ELISA.

Journal

  • BUNSEKI KAGAKU

    BUNSEKI KAGAKU 49 (11), 843-848, 2000

    The Japan Society for Analytical Chemistry

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