A new method, based on stir bar sorptive extraction (SBSE) with in situ derivatization and thermal desorption (TD)-gas chromatography-mass spectrometry (GC-MS) is described for the determination of trace amounts of bisphenol A (BPA) in river water, urine, plasma, and saliva samples. The derivatization conditions with acetic acid anhydride and the SBSE conditions such as sample volumes and extraction time are investigated. Then, the stir bar is subjected to TD followed by GC-MS. The detection limits of BPA in river water, urine, plasma, and saliva samples are 1-5, 20, 100, and 20pgml(-1) (ppt), respectively. Calibration for BPA was shown to be linear with a correlation coefficient of >0.99. The average recoveries of BPA in all samples are higher than 95% (R.S.D. < 10%) with correction using an added surrogate standard, 13C12-bisphenol A. This simple, accurate, sensitive, and selective analytical method may be applicable to the determination of trace amounts of BPA in liquid samples.
"In agreement with previous data  , the sensitivity for BPs increased between 5 and 10-fold when using EG-Silicone stir bars compared with the obtained with those coated with PDMS and preconcentrating the analytes not derivatized. Nevertheless, the preconcentration of underivatized BPs using EG-Silicone SBSE stir bars is still less sensitive than those methods that include derivatization , such as in-tube silylation or in situ acetylation [19–23,29], although the method described here can be considered simpler than those involving derivatization since derivatization reagents are not used. "
[Show abstract][Hide abstract] ABSTRACT: An easy to perform analytical method for the determination of three bisphenol compounds (BPs) in commonly used personal care products (PCPs) is presented. Ethylene glycol-silicone (EG-Silicone) coated stir bars, which have recently become commercially available, are evaluated in this study for the simultaneous determination of bisphenol A (BPA), bisphenol F (BPF) and bisphenol Z (BPZ) by stir bar sorptive extraction (SBSE) in combination with thermal desorption-gas chromatography-mass spectrometry (TD-GC-MS). This new sorptive extraction phase allows the analysis of these compounds without any previous derivatization procedure. Different parameters affecting both SBSE extraction and thermal desorption were carefully optimized, using experimental designs based on the Taguchi orthogonal arrays. The procedure was applied to analyzing easily bought PCPs, providing detection limits of about 8ngg(-1), with precisions lower than 11% in terms of relative standard deviation. Recovery studies performed at two different concentration levels provided satisfactory values for all the compounds. The analyzed personal care samples contained BPA at concentration levels ranging from 30.9 to 88.3ngg(-1).
Journal of pharmaceutical and biomedical analysis 02/2013; 78-79C:255-260. DOI:10.1016/j.jpba.2013.02.023 · 2.98 Impact Factor
[Show abstract][Hide abstract] ABSTRACT: This paper reviews the recent developments in bioanalysis sample preparation techniques and gives an update on basic principles, theory, applications and possibilities for automation, and a comparative discussion on the advantages and limitation of each technique. Conventional liquid-liquid extraction (LLE), protein precipitation (PP) and solid-phase extraction (SPE) techniques are now been considered as methods of the past. The last decade has witnessed a rapid development of novel sample preparation techniques in bioanalysis. Developments in SPE techniques such as selective sorbents and in the overall approach to SPE, such as hybrid SPE and molecularly imprinted polymer SPE, have been addressed. Considerable literature has been published in the area of solid-phase micro-extraction and its different versions, e.g. stir bar sorptive extraction, and their application in the development of selective and sensitive bioanalytical methods. Techniques such as dispersive solid-phase extraction, disposable pipette extraction and micro-extraction by packed sorbent offer a variety of extraction phases and provide unique advantages to bioanalytical methods. On-line SPE utilizing column-switching techniques is rapidly gaining acceptance in bioanalytical applications. PP sample preparation techniques such as PP filter plates/tubes offer many advantages like removal of phospholipids and proteins in plasma/serum. Newer approaches to conventional LLE techniques (salting-out LLE) are also covered in this review article.
"The methods most frequently used for the determination of bisphenol A in environmental water are gas chromatography (GC) (Kawaguchi et al., 2004; Liu et al., 2004) and liquid chromatography (LC) (Shin et al., 2001; Watabe et al., 2004), both coupled to mass spectrometry (MS). These methods are highly sensitive and specific, but require time-consuming pre-treatment steps and thus do not allow rapid processing of multiple samples. "
[Show abstract][Hide abstract] ABSTRACT: This work describes a very simple, fast and sensitive method based on the use of the optical immunosensor "RIver ANAlyser" (RIANA) to the determination of bisphenol A in a waters. RIANA is based on a rapid solid-phase indirect inhibition immunoassay that takes place at an optical transducer chip chemically modified with an analyte derivative. Fluorescence produced by labelled antibodies bound to the transducer is detected by photodiodes and can be correlated with the analyte concentration. The sensor surface can be regenerated thus allowing the performance of several measurements (around 300) with the same transducer. Each test cycle, including one regeneration step, is accomplished in 15 min. The detection limit achieved in the direct determination of bisphenol A in water with this system was 0.014 microg/L. Satisfactory repeatability, with relative standard deviations (RSD) ranging between 1.48% and 6.93% were obtained. The immunosensor method developed was applied to the monitoring of bisphenol A in various types of water collected in a waterworks (from the river water source to the finished drinking water) and validated against the results obtained in the same approach by a more traditional method, based on solid-phase extraction followed by liquid chromatography-mass spectrometry. Results obtained by both techniques were in general good agreement (considering the typical overestimation bias of immunoassays), and served to prove the satisfactory removal efficiency of the overall purification process applied in the waterworks and, in particular, of the sand filtration step.
Water Research 01/2006; 39(20):5071-9. DOI:10.1016/j.watres.2005.09.023 · 5.53 Impact Factor
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