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J Agric Food Chem. 2013 Jan 23;61(3):561-8. doi: 10.1021/jf304470k. Epub 2013 Jan 9.

Optimization of headspace solid-phase microextraction coupled with gas chromatography-mass spectrometry for detecting methoxyphenolic compounds in pu-erh tea.

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  • 1Key Laboratory of Industrial Fermentation Microbiology Ministry of Education, College of Biotechnology, Tianjin University of Science and Technology, Tianjin 300457, People's Republic of China.


A method based on headspace solid-phase microextraction coupled with gas chromatography-mass spectrometry was developed for the analysis of volatile methoxyphenolic compounds in pu-erh tea. Six fibers with different polarities were initially evaluated. The 75 μm carboxen/polydimethylsiloxane fiber exhibited the highest extraction efficiency and was selected for further optimization. A Plackett-Burman design was used to screen for the brewing proportion of tea and water, amount of pu-erh tea, ionic strength, extraction time, extraction temperature, desorption time, rate of agitation, and equilibrium time. A Box-Behnken design was then applied to optimize the significant factors. Under optimal conditions, the proposed method affords a wide range of linearity, high linear regression coefficients (0.996-0.999), less than 9.0% repeatability of relative standard deviation, and limits of detection ranging from 2.31 to 21.80 ng/g. The proposed method has satisfactory accuracy, with recoveries of 79.08-113.9%. This method was successfully applied for the analysis of pu-erh tea samples.

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