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Merck

Improved method for rapid detection of phthalates in bottled water by gas chromatography-mass spectrometry.

Journal of chromatography. B, Analytical technologies in the biomedical and life sciences (2015-07-03)
Paz Otero, Sushanta Kumar Saha, Siobhan Moane, John Barron, Gerard Clancy, Patrick Murray
RESUMEN

An improved gas chromatography-mass spectrometry (GC-MS) method for simple, rapid and precise quantification of phthalates in drinking water is presented. This method was validated for bis (2-n-butoxyethyl) phthalate (DBEP), bis (2-n-ethylhexyl) phthalate (DEHP), butyl benzyl phthalate (BBP), di-butyl phthalate (DBP), diethyl phthalate (DEP), dihexyl phthalate (DHP), dimethyl phthalate (DMP), di-n-octyl phthalate (DNOP) and dinonyl phthalate (DINP). Linearity of 0.9984>r(2)>0.9975 in the range of 0.075-4.8μg/mL for the selected phthalates was obtained. Accuracy values were in the range of 93-114% and RSD% for the analysis of 1.2μg/mL of each phthalate was below 2.3% (n=9). This new method design has significantly improved the detection in terms of rapidity, specificity, repeatability and accuracy compared to available methods. The procedure has been applied to the analyses of three different brands of commercially available bottled mineral water and the corresponding plastic bottles. Phthalates were extracted with dichloromethane and re-constituted in cyclohexane prior to GC-MS analysis. When the validated GC-MS method was applied to the quantification of the selected phthalates in the samples, only DBP (up to 0.0675±0.0018μg/mL) and DEHP (up to 1.6848±0.1631μg/mL) were found. Furthermore, we provide specific data about the concentration of DBP and DEHP in bottled water attributable to migration of phthalates from respective plastic bottles.

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Sigma-Aldrich
Diclorometano, anhydrous, ≥99.8%, contains 40-150 ppm amylene as stabilizer
Sigma-Aldrich
Ciclohexano, anhydrous, 99.5%
Sigma-Aldrich
Diclorometano, suitable for HPLC, ≥99.9%, contains 40-150 ppm amylene as stabilizer
Supelco
Diclorometano, ≥99.9%
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Ciclohexano, JIS special grade
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Diclorometano, JIS special grade, ≥99.0%
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Diclorometano, SAJ first grade, ≥99.0%
Supelco
Dichloromethane solution, contains 10 % (v/v) methanol
Sigma-Aldrich
Ciclohexano, suitable for HPLC
Sigma-Aldrich
Ciclohexano, SAJ first grade, ≥99.0%