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Optimization of Headspace Solid-Phase Microextraction Coupled with Gas Chromatography-Mass Spectrometry for Detecting Methoxyphenolic Compounds in Pu-erh Tea

  作者 DU LIPING; WANG CHAO; LI JIANXUN; XIAO DONGGUANG; LI CHANGWEN; XU YONGQUAN  
  选自 期刊  Journal of Agricultural and Food Chemistry;  卷期  2013年61-3;  页码  561-568  
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[摘要]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 mu m 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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