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Anal Chim Acta. 2006 Sep 01;577(1):62-7. doi: 10.1016/j.aca.2006.06.030. Epub 2006 Jun 18.

Simultaneous determination of preservatives in soft drinks, yogurts and sauces by a novel solid-phase extraction element and thermal desorption-gas chromatography.

Analytica chimica acta

Lili Wang, Xiao Zhang, Yiping Wang, Wei Wang

Affiliations

  1. College of Chemical Engineering and Materials Science, Zhejiang University of Technology, Hangzhou, Zhejiang 310014, PR China. [email protected]

PMID: 17723654 DOI: 10.1016/j.aca.2006.06.030

Abstract

A novel solid-phase extraction element combined with thermal desorption-gas chromatography (TD-GC) using a pyrolysis-GC system was applied for the determination of the five preservatives - benzoic acid, sorbic acid, and methyl, ethyl and propyl esters of p-hydroxybenzoic acid - in soft drinks, yogurts and sauces. The extraction element is made of a titanium (Ti) tubing (30 mm x 1.2 mm i.d.x1.6 mm o.d.) coated with a chemically bonded layer of polydimethylsiloxane (PDMS) to a thickness of 500 microm. A sample pH of 2.0, sample volume of 5 ml, extraction time of 45 min with addition of salt (15% m/v NaCl) and TD temperature from 40 to 280 degrees C at a heating rate of 40 degrees Cmin(-1) and maintained at 280 degrees C for 9 min, were selected as optimum extraction and desorption conditions. The linearity of the method was satisfactory over a concentration range of 2-1000 mg L(-1) for benzoic acid and sorbic acid, 0.2-300 mg L(-1) for methyl ester of p-hydroxybenzoic acid, and 0.02-300 mg L(-1) for ethyl and propyl esters of p-hydroxybenzoic acid, and the correlation coefficients were higher than 0.997. The limit of detection ranged from 0.002 to 0.2 mg L(-1). The potential of the proposed method was assessed by applying it to the determination of preservatives in real samples. The recoveries (92-106%) and precisions (R.S.D.s of 0.9-4.6% (n=5)) of the method were examined by analyzing soft drink, yogurt and sauce samples spiked at levels of between 20 and 100 mg L(-1). This simple, accurate and highly sensitive method may be used in the determination of the preservatives in various water-based food samples.

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