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The Analytical Scientist / App Notes / 2016 / Sensitive online SPE determination of bisphenol A in water samples

Sensitive online SPE determination of bisphenol A in water samples

09/12/2016

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Abstract:

In this application note a method for the sensitive determination of bisphenol A (BPA) from water samples is presented. The use of online SPE coupling avoids time consuming and manual sample preparation steps, making the method well-suited for routine analyses of BPA in low concentration samples like drinking water.

Introduction

Solid-phase extraction (SPE) is an effective preparation method for concentrating analytes prior to HPLC analysis. Classically, this method is done offline via time consuming steps. The advantages of online coupling result in a reduction of analysis time, sample contamination, and analyte loss. This automated method is perfectly suited for pre-concentration of Bisphenol A (BPA) in drinking water. This substance is known for its endocrine effects similar to the hormone estrogen even at very low dosage and is associated with environmental and health problems. Derived from various studies a maximum entry of <1 µg/ml is expected in cold drinking water. In warmed-up water (70°C) a concentration of up to 30 µg/ml is possible. All these facts make it inevitable to establish a fast HPLC method that reaches very low detection limits for BPA.

Experimental preparation of standard solution

All standards were prepared and diluted with LC-MS grade water to eliminate matrix effects during calibration and to ensure high quality of the standard.

Schematic arrangement of the involved system components for the HPLC system coupled to online SPE extraction
Experimental preparation of standard solution

All standards were prepared and diluted with LC-MS grade water to eliminate matrix effects during calibration and to ensure high quality of the standard.

Analytical HPLC method parameters
SPE method parameters
Results

After calibration by direct injection, the recovery rate is determined with the online SPE column in the flow path. Differing concentrations down to 0.07 ng/ml have been extracted from prepared water samples with constant extraction time. Afterwards the extraction time was varied using a solution with a constant concentration of 0.1 ng/ml. A recovery rate of 98% for BPA was found.

Chromatogram of three different concentrations with the same online SPE extraction time
Conclusion

The presented automated method is well-suited for the sensitive analysis of BPA in water samples like drinking water. For a lower detection limit, the online SPE extraction time can simply be increased. The method makes time consuming manual sample preparation steps obsolete.


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