Shuqin Yu - Trace analysis of diethylstilbestrol, dienestrol and hexestrol in environmental water by Nylon 6 nanofibers mat-based solid-phase extraction coupled with Liquid Chromatography-Mass Spectrometry

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        A simple, rapid and sensitive method for the determination of   diethylstilbestrol (DES), dienestrol (DE) and hexestrol (HEX) was   developed by using the Nylon 6 nanofibers mat-based solid-phase   extraction (SPE) coupled with liquid chromatography-tandem mass   spectrometry (LC-MS). These estrogens were separated within 8 min   by LC using an ODS column and methanol/water (80/20, v/v) at a   flow rate of 1.0 mL min–1.   Electrospray ionization conditions in the negative ion mode were   optimized for MS detection of the estrogens. Under the optimum   SPE conditions, all target analytes in 50 mL environmental water   samples can be completely extracted by 1.5 mg Nylon 6 nanofibers   mat at flow rate of 3.0 mL min–1    and easily eluted by passage of 500 µL mobile phase. By using the   novel SPE-LC/MS method, good linearity of the calibration curve   (r    2   ≥ 0.9992) was obtained in the concentration range from 0.10 ng   L–1    to 1.0 mg L–1    (except for DE which was 0.20 ng L–1    to 1.0 mg L–1)   for all analytes examined. The limits of detection (S/N = 3) of   the three estrogens ranged from 0.05 ng L–1    to 0.10 ng L–1.   This method was applied successfully to the analysis of   environmental water samples without any other pretreatment and   interference peaks. Several water samples were collected from   Jinchuan River and Xuanwu Lake, and in Jinchuan River water DES   was detected at 0.13 ng L–1.   The recoveries of estrogens spiked into tap water were above   98.2%, and the relative standard deviations were below   4.78%.


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