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Determination of bisphenol-A in aqueous samples by means of new multi-layer solid-phase extraction cartridges and HPLC with UV detection

Nagahashi M., Kikuchi N., Tsukahara M., Makioka S., Miki T.

Acta Chromatographica

2001

No. 11

75-95

Research has been conducted on a new method of determining bisphenol-A, a reputed hormonal disrupter, by means of multi-layer solid-phase extraction and subsequent HPLC analysis. An isolation and concen-tration cartridge was used to isolate the analyte from aqueous samples. The bisphenol-A-containing fraction obtained from this cartridge was further purified on purification cartridge A or on purification cartridge A plus purification cartridge B. The clear bisphenol-A-containing fraction was analysed by a HPLC with UV detection; the detector was equipped with a cooling system to reduce the noise level. Conventional HPLC analysis was performed on a Zorbax ODS column. For samples containing less than a nanogram, a semi-micro ODS column was used. An Innertsil CN-3 column was also used to separate matrix compounds that interfered with the measurement of the bisphenol-A peak. By use of an internal standard satisfactory calibration curves were obtained from the two ODS columns; stability and linearity were adequate and CV values were satisfactory for amounts between 2 and 100 ng for the conventional column and between 0.2 and 40 ng for the semi-micro column. The sensitivity and reliability of the technique were tested by analysing seven river water samples and five other water samples from natural water sources. Some of these results were compared with those obtained by use of the method proposed in the Tentative Surveying Manual of Endocrine Disruptor, published by the Japanese Environmental Agency in 1998. Twenty canned non-alcoholic beverages were also analysed. Although the results obtained indicated that this analytical method was less sensitive than GC-MS, the instrumentation is approximately one-twentieth less costly. The method can be widely used for analysis of aqueous samples when there is no limitation on sample volume, for example in water analysis or in the food industry.

Separation and estimation of bisphenol a by liquid chromatography with UV detection

Nagahashi M., Kikuchi N., Migaki E., Watanabe S., Miki T.

Acta Chromatographica

2000

No. 10

110-122

Reliable HPLC separation and estimation of bisphenol A has been performed on a conventional ODS column with 40:60 acetonitrile–water as mobile phase and UV detection at 277 nm. Linear regression plots were obtained for the dependence of response on bisphenol A concentration in the working ranges 2 to 10 ng and 10 to 100 ng; the correlation coefficients for the plots were r = 0.9976 (n = 5) and r = 0.9987 (n = 6), respectively. Aqueous samples were applied to a solid-phase extraction cartridge packed with three layers, Bio-Rad AG 50W X8 [H+], ODS–silica, and Bio-Rad AG 1 X8 [formate–]. Eluent from this cartridge was passed through a normal-phase Florisil PR cartridge. These isolation and purification cartridges effectively separated and purified bisphenol A from spiked samples with recovery between 86 and 92%. The method was used to estimate bisphenol A in water samples.