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Optimization by experimental design of headspace sorptive extraction and solid-phase microextraction for the determination of terpenes in spices

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Abstract

Headspace sorptive extraction (HSSE) was compared with solid-phase microextraction (SPME), a reference method for the extraction of volatiles. HSSE and SPME were optimized by experimental design for the extraction of terpenes and terpenoids from spices. The different extraction parameters studied were the extraction time, the extraction temperature, the sample mass, and the equilibrium time (only for SPME). Extracts were obtained by HSSE and SPME from six spices: cinnamon, cumin, thyme, fennel seeds, nutmeg, and clove. Those extracts were analyzed by gas chromatography coupled to a mass spectrometer (GC-MS) qualitatively and quantitatively. The quantitative analysis was conducted using 28 standards. For each standard, calibration curves, limits of detection (LOD) and quantification (LOQ) were determined. The study shows that HSSE is selective, sensitive, and highly repeatable method for the extraction of volatile terpenes and terpenoids from spices and allows to produce extracts concentrated in the μg/g range of terpenes.

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References

  • Abdelwahab SI, Mariod AA, Mohamed M et al (2017) Chemical composition and antioxidant properties of the essential oil of Cinnamomum altissimum Kosterm. (Lauraceae). Arab J Chem 10:131–135

    Article  CAS  Google Scholar 

  • Abilleira E, de Renobales M, Nájera AI, Virto M, Gordoa JCR, Pérez-Elortondo FJ, Albisu M, Barron LJR (2010) An accurate quantitative method for the analysis of terpenes in milk fat by headspace solid-phase microextraction coupled to gas chromatography-mass spectrometry. Food Chem 120:1162–1169

    Article  CAS  Google Scholar 

  • Adiani V, Gupta S, Chatterjee S, et al (2015) Activity guided characterization of antioxidant components from essential oil of nutmeg (Myristica fragrans). J Food Sci Technol 52

    Article  CAS  Google Scholar 

  • Baltussen E, Sandra P, David F, Cramers C (1999) Stir bar sorptive extraction (SBSE), a novel extraction technique for aqueous samples: theory and principles. J Microcolumn Sep 11:737–747

    Article  CAS  Google Scholar 

  • Barba C, Thomas-Danguin T, Guichard E (2017) Comparison of stir bar sorptive extraction in the liquid and vapour phases, solvent-assisted flavour evaporation and headspace solid-phase microextraction for the (non)-targeted analysis of volatiles in fruit juice. LWT Food Sci Technol 85:334–344

    Article  CAS  Google Scholar 

  • Bezerra MA, Santelli RE, Oliveira EP, Villar LS, Escaleira LA (2008) Response surface methodology (RSM) as a tool for optimization in analytical chemistry. Talanta 76:965–977

    Article  CAS  Google Scholar 

  • Bicchi C, Iori C, Rubiolo P, Sandra P (2002) Headspace sorptive extraction (HSSE), stir bar sorptive extraction (SBSE), and solid phase microextraction (SPME) applied to the analysis of roasted Arabica coffee and coffee brew. J Agric Food Chem 50:449–459

    Article  CAS  Google Scholar 

  • Bicchi C, Cordero C, Liberto E, Rubiolo P, Sgorbini B, Sandra P (2005) Impact of phase ratio, polydimethylsiloxane volume and size, and sampling temperature and time on headspace sorptive extraction recovery of some volatile compounds in the essential oil field. J Chromatogr A 1071:111–118

    Article  CAS  Google Scholar 

  • Bicchi C, Liberto E, Matteodo M, Sgorbini B, Mondello L, Zellner B'A, Costa R, Rubiolo P (2008) Quantitative analysis of essential oils: a complex task. Flavour Fragr J 23:382–391

    Article  CAS  Google Scholar 

  • Cacho JI, Campillo N, Viñas P, Hernández-Córdoba M (2015) Evaluation of three headspace sorptive extraction coatings for the determination of volatile terpenes in honey using gas chromatography-mass spectrometry. J Chromatogr A 1399:18–24

    Article  CAS  Google Scholar 

  • David F, Sandra P (2007) Stir bar sorptive extraction for trace analysis. J Chromatogr A 1152:54–69. https://doi.org/10.1016/j.chroma.2007.01.032

    Article  PubMed  CAS  Google Scholar 

  • De Sousa DP (2011) Analgesic-like activity of essential oils constituents. Molecules 16:2234–2252

    Google Scholar 

  • Fonsêca DV, Salgado PRR, Aragão Neto H d C et al (2016) Ortho-eugenol exhibits anti-nociceptive and anti-inflammatory activities. Int Immunopharmacol 38:402–408

    Article  CAS  Google Scholar 

  • Forney CF, Song J (2017) Flavors and aromas: chemistry and biological functions. In: Fruit and Vegetable Phytochemicals: Chemistry and Human Health: Second Edition. pp 515–539

    Chapter  Google Scholar 

  • Guerrero ED, Marín RN, Mejías RC, Barroso CG (2006) Optimisation of stir bar sorptive extraction applied to the determination of valatile compounds in vinegars. J Chromatogr A 1104:47–53

    Article  CAS  Google Scholar 

  • Hevia K, Castro R, Natera R, González-García JA, Barroso CG, Durán-Guerrero E (2016) Optimization of head space sorptive extraction to determine volatile compounds from oak wood in fortified wines. Chromatographia 79:763–771. https://doi.org/10.1007/s10337-016-3088-y

    Article  CAS  Google Scholar 

  • Jeleń HH, Gracka A (2015) Analysis of black pepper volatiles by solid phase microextraction-gas chromatography: a comparison of terpenes profiles with hydrodistillation. J Chromatogr A 1418:200–209

    Article  CAS  Google Scholar 

  • Jeleń HH, Majcher M, Dziadas M (2012) Microextraction techniques in the analysis of food flavor compounds: a review. Anal Chim Acta 738:13–26

    Article  CAS  Google Scholar 

  • Kaefer CM, Milner JA (2008) The role of herbs and spices in cancer prevention. J Nutr Biochem 19:347–361

    Article  CAS  Google Scholar 

  • Lundstedt T, Seifert E, Abramo L, Thelin B, Nyström Å, Pettersen J, Bergman R (1998) Experimental design and optimization. Chemom Intell Lab Syst 42:3–40

    Article  CAS  Google Scholar 

  • Mancini E, Senatore F, Del Monte D et al (2015) Studies on chemical composition, antimicrobial and antioxidant activities of five Thymus vulgaris L. essential oils. Molecules 20:12016–12028

    Article  CAS  Google Scholar 

  • Opara EI, Chohan M (2014) Culinary herbs and spices: their bioactive properties, the contribution of polyphenols and the challenges in deducing their true health benefits. Int J Mol Sci 15:19183–19202

    Article  CAS  Google Scholar 

  • Patel K, Ruiz C, Calderon R, Marcelo M, Rojas R (2016) Characterisation of volatile profiles in 50 native Peruvian chili pepper using solid phase microextraction–gas chromatography mass spectrometry (SPME–GCMS). Food Res Int 89:471–475

    Article  CAS  Google Scholar 

  • Prieto A, Basauri O, Rodil R, Usobiaga A, Fernández LA, Etxebarria N, Zuloaga O (2010) Stir-bar sorptive extraction: a view on method optimisation, novel applications, limitations and potential solutions. J Chromatogr A 1217:2642–2666

    Article  CAS  Google Scholar 

  • Rakhi NK, Tuwani R, Mukherjee J, Bagler G (2018) Data-driven analysis of biomedical literature suggests broad-spectrum benefits of culinary herbs and spices. PLoS One:1–20

  • Robotti E, Campo F, Riviello M, Bobba M, Manfredi M, Mazzucco E, Gosetti F, Calabrese G, Sangiorgi E, Marengo E (2017) Optimization of the extraction of the volatile fraction from honey samples by SPME-GC-MS, experimental design, and multivariate target functions. J Chem 2017:1–14

    Article  CAS  Google Scholar 

  • Rodrigues C, Portugal FCM, Nogueira JMF (2012) Static headspace analysis using polyurethane phases – application to roasted coffee volatiles characterization. Talanta 89:521–525. https://doi.org/10.1016/j.talanta.2011.12.010

    Article  PubMed  CAS  Google Scholar 

  • Santana De Oliveira M, Almeida Da Costa W, Santiago Pereira D et al (2016) Chemical composition and phytotoxic activity of clove (Syzygium aromaticum) essential oil obtained with supercritical CO2. J Supercrit Fluids 118:185–193

    Article  CAS  Google Scholar 

  • Sghaier L, Vial J, Sassiat P, Thiebaut D, Watiez M, Breton S, Rutledge DN, Cordella CBY (2016) An overview of recent developments in volatile compounds analysis from edible oils: technique-oriented perspectives. Eur J Lipid Sci Technol 118:1853–1879

    Article  CAS  Google Scholar 

  • Srinivasan K (2005) Plant foods in the management of diabetes mellitus: spices as beneficial antidiabetic food adjuncts. Int J Food Sci Nutr 56:299–414

    Article  Google Scholar 

  • Stalikas C, Fiamegos Y, Sakkas V, Albanis T (2009) Developments on chemometric approaches to optimize and evaluate microextraction. J Chromatogr A 1216:175–189

    Article  CAS  Google Scholar 

  • Van den Dool H, Kratz PD (1963) A generalization of the retention index system including linear temperature programmed gas-liquid partition chromatography. J Chromatogr 11:463–471

    Article  Google Scholar 

  • Wardencki W, Curyło J, Namieśnik J (2007) Trends in solventless sample preparation techniques for environmental analysis. J Biochem Biophys Methods 70:275–288

    Article  CAS  Google Scholar 

  • Weldegergis BT, Tredoux AGJ, Crouch AM (2007) Application of a headspace sorptive extraction method for the analysis of volatile components in south african wines. J Agric Food Chem 55:8696–8702

    Article  CAS  Google Scholar 

  • Yashin A, Yashin Y, **a X, Nemzer B (2017) Antioxidant activity of spices and their impact on human health: a review. Antioxidants 6:1–18

    Article  CAS  Google Scholar 

  • Zwenger S, Basu C (2008) Plant terpenoids: applications and future potentials. Biotechnol Mol Biol Rev 3:1

    Google Scholar 

Download references

Funding

This work has been financially supported by “Association Nationale Recherche Technologie” with the CIFRE Contract no. 2016/0447.

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Authors and Affiliations

  1. Université de Strasbourg, CNRS, IPHC UMR 7178, F-67000, Strasbourg, France

    Zélie Triaux, Eric Marchioni & Christophe Marcic

  2. Benephyt, 16 rue d’Austerlitz, 67000, Strasbourg, France

    Zélie Triaux & Hugues Petitjean

  3. Twistaroma, 74 Route du Rhin, 67400, Illkirch-Graffenstaden, France

    Damien Steyer

Authors
  1. Zélie Triaux
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  2. Hugues Petitjean
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  3. Eric Marchioni
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  4. Damien Steyer
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  5. Christophe Marcic
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Correspondence to Christophe Marcic.

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Zélie Triaux declares that she has no conflict of interest. Hugues Petitjean declares that he has no conflict of interest. Eric Marchioni declares that he has no conflict of interest. Damien Steyer declares that he has no conflict of interest. Christophe Marcic declares that he has no conflict of interest.

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Triaux, Z., Petitjean, H., Marchioni, E. et al. Optimization by experimental design of headspace sorptive extraction and solid-phase microextraction for the determination of terpenes in spices. Food Anal. Methods 12, 2764–2776 (2019). https://doi.org/10.1007/s12161-019-01622-4

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  • DOI: https://doi.org/10.1007/s12161-019-01622-4

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