Abstract
This paper focuses on the study of volatile and semi-volatile compounds of honey, using for the first-time vacuum-assisted solid-phase microextraction and gas chromatography-mass spectrometry (Vac-SPME/GC–MS) to reaffirm the geographical features of honey. An emphasis was put on the Vac-SPME method, and its comparison with HS-SPME method, and its application to characterize the volatile and semi-volatile profile of honey. Ten multiflower honey samples from mountainous and steppe regions were taken for the analysis. Determination of volatiles and semi-volatile was conducted using gas chromatograph with mass spectrometric detector. Chromatographic data processing was conducted through chemometrics tools. The extraction parameters were optimized using design of the experiments based on the protocol of SPME. The optimal parameters of vacuum-assisted solid-phase microextraction to characterize the volatile and semi-volatile profile of honey sample were 30 min for extraction time, 60 °C for extraction temperature, and 30 min for the incubation time. Geographical location influences on the composition of honey, so it is important to differentiate them. Hence, pattern recognition method principal component analysis (PCA) was conducted to reaffirm the geographical origin of mountain and steppe honey samples. Analysis revealed a considerable variation in the composition of mountain and steppe honey. Results suggest the developed methodology to be accurate and reliable for the geographical classification of honey.
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References
Alimzhanova MB, Kenessov BN, Nauryzbayev MK, Koziel JA (2012) Effects of moisture content and solvent additive on headspace solid-phase microextraction of total petroleum hydrocarbons from soil. Eurasian Chem J 14:331–335. https://doi.org/10.18321/ectj131
Anupama D, Bhat KK, Sapna VK (2003) Sensory and physico-chemical properties of commercial samples of honey. Food Res Int 36:183–191. https://doi.org/10.1016/S0963-9969(02)00135-7
Barth OM (2004) Melissopalynology in Brazil: a review of pollen analysis of honeys, propolis and pollen loads of bees. Sci Agric 61:342–350. https://doi.org/10.1590/s0103-90162004000300018
Bianchin JN, Nardini G, Merib J et al (2014) Screening of volatile compounds in honey using a new sampling strategy combining multiple extraction temperatures in a single assay by HS-SPME-GC-MS. Food Chem 145:1061–1065. https://doi.org/10.1016/j.foodchem.2013.08.139
Brunton NP, Cronin DA, Monahan FJ (2001) The effects of temperature and pressure on the performance of Carboxen/PDMS fibres during solid phase microextraction (SPME) of headspace volatiles from cooked and raw turkey breast. Flavour Fragr J 16:294–302. https://doi.org/10.1002/ffj.1000
Castro-Vázquez L, Díaz-Maroto MC, de Torres C, Pérez-Coello MS (2010) Effect of geographical origin on the chemical and sensory characteristics of chestnut honeys. Food Res Int 43:2335–2340. https://doi.org/10.1016/j.foodres.2010.07.007
Chen H, Jin L, Fan C, Wang W (2017) Non-targeted volatile profiles for the classification of the botanical origin of Chinese honey by solid-phase microextraction and gas chromatography–mass spectrometry combined with chemometrics. J Sep Sci 40:4377–4384. https://doi.org/10.1002/jssc.201700733
Cuevas-Glory LF, Pino JA, Santiago LS, Sauri-Duch E (2007) A review of volatile analytical methods for determining the botanical origin of honey. Food Chem 103:1032–1043. https://doi.org/10.1016/j.foodchem.2006.07.068
Dimou M, Katsaros J, Klonari KT, Thrasyvoulou A (2006) Discriminating pine and fir honeydew honeys by microscopic characteristics. J Apic Res 45:16–21. https://doi.org/10.1080/00218839.2006.11101319
Duru ME, Taş M, Çayan F et al (2021) Characterization of volatile compounds of Turkish pine honeys from different regions and classification with chemometric studies. Eur Food Res Technol 247:2533–2544. https://doi.org/10.1007/s00217-021-03817-8
El Sohaimy SA, Masry SHD, Shehata MG (2015) Physicochemical characteristics of honey from different origins. Ann Agric Sci 60:279–287. https://doi.org/10.1016/j.aoas.2015.10.015
Erejuwa OO, Sulaiman SA, Wahab MSA (2012) Honey - a novel antidiabetic agent. Int J Biol Sci 8:913–934. https://doi.org/10.7150/ijbs.3697
Erejuwa OO (2019) Honey: profile and features: applications to diabetes, 2nd edn. Elsevier Inc.
Guyot-Declerck C, Renson S, Bouseta A, Collin S (2002) Floral quality and discrimination of Lavandula stoechas, Lavandula angustifolia, and Lavandula angustifolia x latifolia honeys. Food Chem 79:453–459. https://doi.org/10.1016/S0308-8146(02)00216-9
Habib HM, Al Meqbali FT, Kamal H et al (2014) Bioactive components, antioxidant and DNA damage inhibitory activities of honeys from arid regions. Food Chem 153:28–34. https://doi.org/10.1016/j.foodchem.2013.12.044
Jerkovic I, Tuberoso CIG, Marijanovic Z et al (2015) Antioxidant capacity and chemical profiles of Satureja montana L. honey: hotrienol and syringyl derivatives as biomarkers. Chem Biodivers 12:1047–1056. https://doi.org/10.1002/cbdv.201400183
Jolliffe I (2021) A 50-year personal journey through time with principal component analysis. J Multivar Anal 104820. https://doi.org/10.1016/j.jmva.2021.104820
Karabagias IK, Badeka A, Kontominas MG (2020) A decisive strategy for monofloral honey authentication using analysis of volatile compounds and pattern recognition techniques. Microchem J 152:104263. https://doi.org/10.1016/j.microc.2019.104263
Karabagias IK, Karabagias VK, Nayik GA et al (2022) A targeted chemometric evaluation of the volatile compounds of Quercus ilex honey in relation to its provenance. Lwt 154:112588. https://doi.org/10.1016/j.lwt.2021.112588
Kaškoniene V, Rimantas P, Violeta C (2008a) Composition of Volatile Compounds of Honey of Various Floral Origin and Beebread Collected in Lithuania Composition of Volatile Compounds of Honey of Various Floral Origin and Beebread Collected in Lithuania. Eksteryte. https://doi.org/10.1016/j.foodchem.2008.05.021
Kaškoniene V, Venskutonis PR, Čeksteryte V (2008b) Composition of volatile compounds of honey of various floral origin and beebread collected in Lithuania. Food Chem 111:988–997. https://doi.org/10.1016/j.foodchem.2008.05.021
Khalil MI, Sulaiman SA, Gan SH (2010) High 5-hydroxymethylfurfural concentrations are found in Malaysian honey samples stored for more than one year. Food Chem Toxicol 48:2388–2392. https://doi.org/10.1016/j.fct.2010.05.076
Łozowicka B, Kaczyński P, Iwaniuk P (2021) Analysis of 22 free amino acids in honey from Eastern Europe and Central Asia using LC-MS/MS technique without derivatization step. J Food Compos Anal 98. https://doi.org/10.1016/j.jfca.2021.103837
Manyi-loh CE, Ndip RN, Clarke AM (2011) Volatile compounds in honey : a review on their involvement in aroma , botanical origin determination and potential biomedical activities. 9514–9532. https://doi.org/10.3390/ijms12129514
Marijanovic Z, Kres P, Marulic M (2009) Screening of Volatile Composition of Lavandula Hybrida R Everchon II Honey Using Headspace Solid-Phase Microextraction and Ultrasonic Solvent Extraction. Chem Biodivers 6:421–430
Mascrez S, Psillakis E, Purcaro G (2020) A multifaceted investigation on the effect of vacuum on the headspace solid-phase microextraction of extra-virgin olive oil. Anal Chim Acta 1103:106–114. https://doi.org/10.1016/j.aca.2019.12.053
Mastelic J, Marijanovic Z (2006) A variety of volatile compounds as markers in unifloral honey from dalmatian sage ( Salvia officinalis L.). Chem Biodivers 3:1307–1316
Nayik GA, Nanda V (2015) Characterization of the volatile profile of unifloral honey from Kashmir Valley of India by using solid-phase microextraction and gas chromatography–mass spectrometry. Eur Food Res Technol 240:1091–1100. https://doi.org/10.1007/s00217-015-2413-2
Pawliszyn J (2012) 2 - Theory of solid-phase microextraction. In: Pawliszyn JBT-H of SPM (ed). Elsevier, Oxford, pp 13–59
Peña RM, Barciela J, Herrero C, García-Martín S (2004) Solid-phase microextraction gas chromatography-mass spectrometry determination of monoterpenes in honey. J Sep Sci 27:1540–1544. https://doi.org/10.1002/jssc.200301705
Pico J, Gerbrandt EM, Castellarin SD (2022) Optimization and validation of a SPME-GC / MS method for the determination of volatile compounds, including enantiomeric analysis, in northern highbush blueberries ( Vaccinium corymbosum L.). Food Chem 368:130812. https://doi.org/10.1016/j.foodchem.2021.130812
Pita-calvo C, Vázquez M (2016) SC. Trends Food Sci Technol. https://doi.org/10.1016/j.tifs.2016.11.015
Plutowska B, Chmiel T, Dymerski T, Wardencki W (2011) A headspace solid-phase microextraction method development and its application in the determination of volatiles in honeys by gas chromatography. Food Chem 126:1288–1298. https://doi.org/10.1016/j.foodchem.2010.11.079
Pontes M, Marques JC, Cˆ JS (2007) Screening of volatile composition from Portuguese multifloral honeys using headspace solid-phase microextraction-gas chromatography – quadrupole mass spectrometry. 74:91–103. https://doi.org/10.1016/j.talanta.2007.05.037
Prdun S, Svečnjak L, Valentić M, et al (2021) Characterization of bee pollen: physico-chemical properties, headspace composition and ftir spectral profiles. Foods 10. https://doi.org/10.3390/foods10092103
Psillakis E (2017) Analytica Chimica Acta vacuum-assisted headspace solid-phase microextraction : a tutorial review. Anal Chim Acta 986:12–24. https://doi.org/10.1016/j.aca.2017.06.033
Psillakis E, Yiantzi E, Sanchez-Prado L, Kalogerakis N (2012) Vacuum-assisted headspace solid phase microextraction: improved extraction of semivolatiles by non-equilibrium headspace sampling under reduced pressure conditions. Anal Chim Acta 742:30–36. https://doi.org/10.1016/j.aca.2012.01.019
Radovic BS, Careri M, Mangia A et al (2001) Contribution of dynamic headspace GC-MS analysis of aroma compounds to authenticity testing of honey. Food Chem 72:511–520. https://doi.org/10.1016/S0308-8146(00)00263-6
Rao PV, Krishnan KT, Salleh N, Gan SH (2016) Biological and therapeutic effects of honey produced by honey bees and stingless bees: a comparative review. Rev Bras Farmacogn 26:657–664. https://doi.org/10.1016/j.bjp.2016.01.012
Revell LE, Morris B (2014) Analysis of volatile compounds in New Zealand unifloral honeys by SPME – GC – MS and chemometric-based classification of floral source. 81–91. https://doi.org/10.1007/s11694-013-9167-y
Risticevic S, Lord H, Górecki T et al (2010) Protocol for solid-phase microextraction method development. Nat Protoc 5:122–139. https://doi.org/10.1038/nprot.2009.179
Sagandykova GN, Alimzhanova MB, Nurzhanova YT, Kenessov B (2017) Determination of semi-volatile additives in wines using SPME and GC–MS. Food Chem 220:162–167. https://doi.org/10.1016/j.foodchem.2016.09.164
Soria AC, Martínez-Castro I, Sanz J (2003) Analysis of volatile composition of honey by solid phase microextraction and gas chromatography-mass spectrometry. J Sep Sci 26:793–801. https://doi.org/10.1002/jssc.200301368
Soria AC, Sanz J, Martínez-Castro I (2009) SPME followed by GC-MS: a powerful technique for qualitative analysis of honey volatiles. Eur Food Res Technol 228:579–590. https://doi.org/10.1007/s00217-008-0966-z
Vakinti M, Mela SM, Fernández E, Psillakis E (2019) Room temperature and sensitive determination of haloanisoles in wine using vacuum-assisted headspace solid-phase microextraction. J Chromatogr A 1602:142–149. https://doi.org/10.1016/j.chroma.2019.03.047
Vazquez L, Celeiro M, Sergazina M, et al (2021) Optimization of a miniaturized solid-phase microextraction method followed by gas chromatography mass spectrometry for the determination of twenty four volatile and semivolatile compounds in honey from Galicia (NW Spain) and foreign countries. Sustain Chem Pharm 21. https://doi.org/10.1016/j.scp.2021.100451
Yeh CH, Tsai WY, Chiang HM et al (2014) Headspace solid-phase microextraction analysis of volatile components in Phalaenopsis Nobby’s Pacific Sunset. Molecules 19:14080–14093. https://doi.org/10.3390/molecules190914080
Acknowledgements
The authors would like to thank the Ministry of Education and Science of the Republic of Kazakhstan for supporting Ph.D. student Madina Mamedova.
Funding
This work was supported by the Ministry of Science and Higher Education of the Republic of Kazakhstan (AP09058561) “Efficient Development of Highly Sensitive Food Analysis Methods Based on Miniaturized Solid Phase Microextraction ” 2021-2023.
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Madina Mamedova: writing— original draft preparation, conceptualization, investigation, formal analysis, visualization, funding acquisition, writing—review and editing.
Mereke Alimzhanova: supervision, conceptualization, funding acquisition, data curation, writing— original draft preparation, writing—review and editing.
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Mamedova, M., Alimzhanova, M.B. Determination of Biomarkers in Multifloral Honey by Vacuum-Assisted Headspace Solid-Phase Microextraction. Food Anal. Methods 16, 1180–1190 (2023). https://doi.org/10.1007/s12161-023-02499-0
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DOI: https://doi.org/10.1007/s12161-023-02499-0