Rapid and simultaneous analysis of tetrabromobisphenol A and hexabromocyclododecane in water by direct immersion solid phase microextraction: Uniform design to explore factors

Abstract

Direct immersion solid phase microextraction (DI-SPME) coupled to liquid chromatography-tandem mass spectrometry (LC-MS/MS) is of significant research interest because of its low solvent consumption, simple design, and efficient, sensitive, fast performance. In this work, a combination of these two methods (DI-SPME-LC-MS) for the determination of tetrabromobisphenol A (TBBPA) and hexabromocyclododecane (HBCD) in water was developed. Important factors, which included temperature, stirring rate, salt concentration, pH value and adsorption time, were evaluated in for the optimization of solid phase microextraction (SPME) method. The method was developed using spiked natural waters in a concentration range of 0.1–10 ng mL−1, and showed notable linearity with regression coefficients ranging between 0.992 and 0.999. The limits of detection varied from 0.01 to 0.04 ng mL−1 (at S/N = 3) and relative standard deviation (RSD < 11%) were obtained showing that the precision of the method was reliable. Recoveries were in relatively high levels for both analytes and ranged from 88% to 108%. Moreover, in comparison with the performance time of traditional sample pretreatment methods such as solid-phase extraction (SPE), accelerated solvent extraction (ASE), and liquid-liquid extraction (LLE), DI-SPME-LC-MS takes only approximately 35 min to perform. The optimized method was successfully applied for monitoring concentrations of TBBPA and HBCD in water.