Improved sample treatment for the determination of bisphenol A and its chlorinated derivatives in sewage sludge samples by pressurized liquid extraction and liquid chromatography–tandem mass spectrometry

• Published in: Talanta (Oxford) 2012-11, Vol.101, p.1-10
• Main Authors: DORIVAL-GARCIA, N, ZAFRA-GOMEZ, A, NAVALON, A, VILCHEZ, J. L
• Format: Article
• Language: English
• Subjects: Analysis methods; Analytical chemistry; Applied sciences; Benzhydryl Compounds - analysis; Benzhydryl Compounds - chemistry; Bisphenol A; Chemistry; Chlorination; Chlorine - chemistry; Chromatographic methods and physical methods associated with chromatography; Chromatography; Chromatography, Liquid - methods; Derivatives; Endocrine disrupting chemicals; Exact sciences and technology; Extraction; Hydrogen-Ion Concentration; LC–MS/MS; Limit of Detection; Liquid-Liquid Extraction - methods; Liquids; Mass spectrometry; Matrix effect; Other chromatographic methods; Phenols - analysis; Phenols - chemistry; Pollution; Pressurized liquid extraction; Reproducibility of Results; Sewage; Sewage sludge; Solvents; Spectrometric and optical methods; Tandem Mass Spectrometry - methods; Wastes
• ISSN: 0039-9140; 1873-3573
• DOI: 10.1016/j.talanta.2012.08.045

A selective, sensitive, robust and accurate method for the determination of bisphenol A (BPA) and its chlorinated derivatives in sewage sludge samples using liquid chromatography–tandem mass spectrometry (LC–MS/MS) is presented. Prior to instrumental analysis, an extraction procedure using pressurized liquid extraction (PLE) was carried out in order to obtain the highest recoveries and improve sensitivity. After LC separation, the MS conditions, in negative atmospheric pressurized chemical ionization (APCI) mode, were individually optimized for each analyte to obtain maximum sensitivity in the selected reaction monitoring (SRM) mode. The use of two reactions for each compound allowed simultaneous quantification and identification in one run. The analytes were separated in less than 6min. BPA-d16 was used as internal standard. The limits of detection of the method ranged from 4 to 8ngg−1 and the limits of quantification from 14 to 26ngg−1, while inter- and intra-day variability was under 6% in all cases. Due to the absence of certified materials, the method was validated using matrix-matched calibration and a recovery assay with spiked samples. Recovery rates ranged from 97.7% to 100.6%. The method was satisfactorily applied for the determination BPA and its chlorinated derivatives in sewage sludge samples collected from wastewater treatment plants (WWTPs) located in the province of Granada (Spain). The sludge samples came from a conventional activated sludge (AS) plant and from a membrane bioreactor (MBR) pilot plant. ► Method to identify and quantify BPA and chlorinated derivatives in sewage sludge. ► A pressurized liquid extraction procedure is optimized prior to LC–MS/MS analysis. ► Solid phase extraction (SPE) is not necessary to improve the results of the analysis. ► Validation of the method: quality parameters, accuracy (trueness and precision). ► Samples from a conventional activated sludge and from a membrane bioreactor (MBR) plants.