Determination of 8 environmental estrogens in fruit by high performance liquid chromatography tandem mass spectrometry
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(Department of Preventive Medicine, Medical College of Hunan Normal University,Hunan Changsha 410006,China)

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    Abstract:

    To establish a high performance liquid chromatography-mass spectrometry (HPLC-MS/MS) method for the simultaneous determination of 8 environmental estrogens, including bisphenol A, 4-n-nonylphenol, estrone, 17β-estradio, estradiol, ethinyl estradiol, 4-octylpheno and diethy lstilbestrol in fruits.Methods Fruit samples were ultrasonic extracted by acetonitrile and cleaned up on a HLB solid phase extraction column. The extract was evaporated to dryness under nitrogen, and the residue was redissolved in methanol. The gradient elution of 8 environmental estrogens was carried out by a ACQUITY UPLC BEH C18 column (2.1 mm×100 mm, 1.7 μm) using acetonitrile-methanol (4∶1, V/V) and 0.1% ammonia aqueous solution as the mobile phase. The target compounds were confirmed and quantified by HPLC-MS/MS under multiple reaction monitoring (MRM) mode with external standard method. Results 8 environmental estrogens and impurity could be well separated, and it showed good linearity in the range of 5-100 μg/L (each r≥0.99). The detection limit of the method was 0.17-0.51 μg/kg, the limit of quantification was 1.33-2.55 μg/kg, the average recovery was 67.77%-110.49%, and the precision was 1.08%-12.74%. The method was applied to fruit samples, bisphenol A was detected in all samples, most samples were detected 4-n-nonylphenol and ethinyl estradiol, some were detected 17β-estradiol and remaining 4 environmental estrogens were not detected. Conclusion The method is rapid, sensitive and accurate, and was suitable for the determination and confirmation of 8 environmental estrogens in fruit.

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QU Fang, LYU Yuan, LI Lin, LIU Qiang, LI Min-lu, WEI Xuan-dong, HU Jing, YI Yin-sha. Determination of 8 environmental estrogens in fruit by high performance liquid chromatography tandem mass spectrometry[J].中国食品卫生杂志,2016,28(4):445-450.

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  • Received:April 15,2016
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  • Online: August 18,2016
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