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Optimization of Headspace Single-Drop Microextraction Coupled with Gas Chromatography–Mass Spectrometry for Determining Volatile Oxidation Compounds in Mayonnaise by Response Surface Methodology

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Abstract

In this assay, headspace single-drop microextraction (HS-SDME) coupled with gas chromatography–mass spectrometry (GC–MS) as a simple, low-cost and rapid method has been developed and validated for determining volatile oxidation compounds including hexanal and heptanal in mayonnaise. The main microextraction variables affecting the HS-SDME procedure such as extraction temperature and time, stirring rate, and amount of NaCl were optimized by response surface methodology employing a central composite design. Obtained results demonstrated that higher yield of extracted analytes could be achieved under the following optimal conditions: extraction temperature of 45 °C, extraction time of 16 min, stirring rate at 700 rpm, and addition of 2 g NaCl. The optimized HS-SDME/GC–MS method was validated for oxidized mayonnaise samples (50 °C/48 h) by calculating analytical parameters (linearity, precision, accuracy, and sensitivity). Good linearity (R 2 > 0.99) was observed by plotting calibration curves of extracted hexanal and heptanal over the concentration range of 0.025–10 μg g−1, and the repeatability of the method, expressed as relative standard deviation, were found to be 4.04 % for hexanal and 3.68 % for heptanal (n = 7). After the microextraction process of spiked mayonnaise sample, high levels of relative recovery were obtained for hexanal (107.33 %) and heptanal (91.43 %). The detection limits were 0.008 ng g−1 and 0.021 ng g−1 for hexanal and heptanal, respectively, while quantification limits of hexanal and heptanal were calculated to be 0.027 ng g−1 and 0.071 ng g−1, respectively. The possibility of the HS-SDME followed GC–MS to determine and quantify volatile oxidation compounds such as hexanal and heptanal was confirmed by analyzing commercial fresh mayonnaise stored at 4 and 25 °C during 3 months.

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Acknowledgments

The authors would like to thank the Institute of National Nutrition & Food Technology Research/Iran for financial assistance for this research. The authors also wish to thank Mahram Food Manufacturing Company for supplying samples in this study.

Conflict of Interest

Maryam Enteshari declares that she has no conflict of interest. Abdorreza Mohammadi has received research grants from National Nutrition and Food Technology Research Institute. Kooshan Nayebzadeh declares that he has no conflict of interest. Ebrahim Azadniya declares that he has no conflict of interest. This article does not contain any studies with human or animal subjects.

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Authors and Affiliations

  1. Department of Food Science and Technology, Faculty of Nutrition Science, Food Science and Technology/National Nutrition and Food Technology Research Institute, Shahid Beheshti University of Medical Sciences, Tehran, Iran

    Maryam Enteshari, Abdorreza Mohammadi, Kooshan Nayebzadeh & Ebrahim Azadniya

  2. Students’ Research Committee, Shahid Beheshti University of Medical Sciences, Tehran, Iran

    Maryam Enteshari

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  1. Maryam Enteshari
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  2. Abdorreza Mohammadi
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  3. Kooshan Nayebzadeh
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Correspondence to Abdorreza Mohammadi.

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Enteshari, M., Mohammadi, A., Nayebzadeh, K. et al. Optimization of Headspace Single-Drop Microextraction Coupled with Gas Chromatography–Mass Spectrometry for Determining Volatile Oxidation Compounds in Mayonnaise by Response Surface Methodology. Food Anal. Methods 7, 438–448 (2014). https://doi.org/10.1007/s12161-013-9643-3

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