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Optimization of Headspace Solid-Phase Micro-extraction (HS-SPME) for Analyzing Soy Sauce Aroma Compounds via Coupling with Direct GC-Olfactometry (D-GC-O) and Gas Chromatography-Mass Spectrometry (GC-MS)

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Abstract

The aim of this study was to develop an effective analytical procedure to analyse the aroma-active compounds of soy sauce using headspace solid-phase micro-extraction (HS-SPME) coupled to gas chromatography-mass spectrometry/olfactometry (GC-MS/O). Optimization of SPME focusing on type of fibre, exposure time, extraction temperature and ionic strength was supported by gas chromatography-mass spectrometry (GC-MS). The optimized HS-SPME conditions were as follows: carboxen/polydimethylsiloxane (CAR/PDMS) fibre, NaCl concentration of 270 g/L, extraction temperature of 45 °C and 30-min exposure time. Under these conditions, 25 aroma-active compounds were detected in soy sauce by HS-SPME-GC-O. 2-Methylbutanal (malty), 3-(methylthio)propanal (cooked potato-like), dimethyl trisufide (sulfury, cooked onion), 2-methoxyphenol (smoky) and 2-phenylethanol (flowery) were the most intense. The overall odour impression of the CAR/PDMS-fibre-derived SPME extract detected via human sniffing resembled that of original soy sauce. The intensity of aromas detected by D-GC-O correlated well with the total peak area of GC-MS analysis. Thus, SPME coupled with D-GC-O offers an automated facile method to allow in situ optimization of SPME performance and ultimately effective analysis of aromas.

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Acknowledgments

The authors gratefully acknowledge the National Science Technology Supporting Project for 12th Five-Year Plan (Nos. 2012BAD34B03 and 2012BAK17B11) and the National High Technology Research and Development Program of China (863 Program) (Nos. SS2012AA021302 and SS2013AA102106) for their financial supports.

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Correspondence to Mouming Zhao.

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Yunzi Feng declares that she has no conflict of interest. Guowan Su declares that he has no conflict of interest. Dongxiao Sun-Waterhouse declares that she has no conflict of interest. Yu Cai declares that she has no conflict of interest. Haifeng Zhao declares that he has no conflict of interest. Chun Cui declares that he has no conflict of interest. Mouming Zhao declares that he has no conflict of interest. This article does not contain any studies with human or animal subjects.

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Feng, Y., Su, G., Sun-Waterhouse, D. et al. Optimization of Headspace Solid-Phase Micro-extraction (HS-SPME) for Analyzing Soy Sauce Aroma Compounds via Coupling with Direct GC-Olfactometry (D-GC-O) and Gas Chromatography-Mass Spectrometry (GC-MS). Food Anal. Methods 10, 713–726 (2017). https://doi.org/10.1007/s12161-016-0612-5

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  • DOI: https://doi.org/10.1007/s12161-016-0612-5

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