Full evaporation headspace gas chromatography for sensitive determination of high boiling point volatile organic compounds in low boiling matrices

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• 作者：Didi Mana Kialengila ; Kris Wolfs ; John Bugalama ; Ann Van Schepdael ; Erwin Adams
• 关键词：Full evaporation technique ; Headspace-gas chromatography ; High boiling volatile compounds ; Sensitivity
• 刊名：Journal of Chromatography A
• 出版年：2013
• 出版时间：8 November, 2013
• 年：2013
• 卷：1315
• 期：Complete
• 页码：167-175
• 全文大小：1037 K

文摘

Determination of volatile organic components (VOC's) is often done by static headspace gas chromatography as this technique is very robust and combines easy sample preparation with good selectivity and low detection limits. This technique is used nowadays in different applications which have in common that they have a dirty matrix which would be problematic in direct injection approaches. Headspace by nature favors the most volatile compounds, avoiding the less volatile to reach the injector and column. As a consequence, determination of a high boiling solvent in a lower boiling matrix becomes challenging. Determination of VOCs like: xylenes, cumene, N,N-dimethylformamide (DMF), dimethyl sulfoxide (DMSO), N,N-dimethylacetamide (DMA), N-methyl-2-pyrrolidone (NMP), 1,3-dimethyl-2-imidazolidinone (DMI), benzyl alcohol (BA) and anisole in water or water soluble products are an interesting example of the arising problems. In this work, a headspace variant called full evaporation technique is worked out and validated for the mentioned solvents. Detection limits below 0.1 ¦Ìg/vial are reached with RSD values below 10 % . Mean recovery values ranged from 92.5 to 110 % . The optimized method was applied to determine residual DMSO in a water based cell culture and DMSO and DMA in tetracycline hydrochloride (a water soluble sample).