Application of a fast and cost-effective in situ derivatization method prior to gas chromatography with mass spectrometry to monitor endocrine disruptors in water matrices

作者：Melo Armindo; Ferreira Isabel M P L V O; Mansilha Catarina^*

来源：Journal of Separation Science, 2015, 38(11): 1983-1989.

DOI：10.1002/jssc.201401463

• Derivatization
• Dispersive liquid-liquid microextraction
• Endocrine disruptors
• Experimental design
• Water

This work deals with the optimization of a rapid, cost-effective, and eco-friendly gas chromatography with mass spectrometry method for the simultaneous determination of four endocrine disruptor compounds in water matrices: estrone, 17 beta-estradiol, 17 alpha-ethinylestradiol, and bisphenol A, that are currently considered to be of main concern in the field of water policy and that could became candidates for future regulations. The method involves simultaneous derivatization and extraction of compounds by dispersive liquid-liquid microextraction followed by gas chromatography with mass spectrometry analysis. Derivatization and extraction parameters were optimized with the aid of experimental design approach. An excellent linear response was achieved for all analytes (r(2) >= 0.999). Limits of detection and quantification are 0.003-0.005 and 0.0094-0.0164 mu g/L, respectively. Intraday precision ranged between 1.1 and 12.6%, whereas interday precision ranged between 0.5 and 14.7%. For accuracy, bias values varied between -15.0 and 13.7%. Recoveries at three concentration levels ranged from 86.4 to 118.2%. The proposed method can be applied to the routine analysis of groundwater, river, sea, tap, and mineral water samples with excellent sensitivity, precision, and accuracy.

• 出版日期2015-6