{"status":"ok","message-type":"work","message-version":"1.0.0","message":{"indexed":{"date-parts":[[2026,8,29]],"date-time":"2026-08-29T09:28:37Z","timestamp":1787995717818,"version":"build-2784847793"},"reference-count":40,"publisher":"MDPI AG","issue":"12","license":[{"start":{"date-parts":[[2021,6,12]],"date-time":"2021-06-12T00:00:00Z","timestamp":1623456000000},"content-version":"vor","delay-in-days":0,"URL":"https:\/\/creativecommons.org\/licenses\/by\/4.0\/"}],"funder":[{"DOI":"10.13039\/501100008530","name":"European Regional Development Fund","doi-asserted-by":"publisher","award":["T1E\u2206K-05678"],"award-info":[{"award-number":["T1E\u2206K-05678"]}],"id":[{"id":"10.13039\/501100008530","id-type":"DOI","asserted-by":"publisher"}]}],"content-domain":{"domain":[],"crossmark-restriction":false},"short-container-title":["Molecules"],"abstract":"<jats:p>This study aimed at an experimental design of response surface methodology (RSM) in the optimization of the dominant volatile fraction of Greek thyme honey using solid-phase microextraction (SPME) and analyzed by gas chromatography-mass spectrometry (GC-MS). For this purpose, a multiple response optimization was employed using desirability functions, which demand a search for optimal conditions for a set of responses simultaneously. A test set of eighty thyme honey samples were analyzed under the optimum conditions for validation of the proposed model. The optimized combination of isolation conditions was the temperature (60 \u00b0C), equilibration time (15 min), extraction time (30 min), magnetic stirrer speed (700 rpm), sample volume (6 mL), water: honey ratio (1:3 v\/w) with total desirability over 0.50. It was found that the magnetic stirrer speed, which has not been evaluated before, had a positive effect, especially in combination with other factors. The above-developed methodology proved to be effective in the optimization of isolation of specific volatile compounds from a difficult matrix, like honey. This study could be a good basis for the development of novel RSM for other monofloral honey samples.<\/jats:p>","DOI":"10.3390\/molecules26123612","type":"journal-article","created":{"date-parts":[[2021,6,14]],"date-time":"2021-06-14T22:25:46Z","timestamp":1623709546000},"page":"3612","update-policy":"https:\/\/doi.org\/10.3390\/mdpi_crossmark_policy","source":"Crossref","is-referenced-by-count":13,"title":["Response Surface Methodology to Optimize the Isolation of Dominant Volatile Compounds from Monofloral Greek Thyme Honey Using SPME-GC-MS"],"prefix":"10.3390","volume":"26","author":[{"ORCID":"https:\/\/orcid.org\/0000-0002-6237-6172","authenticated-orcid":false,"given":"Marinos","family":"Xagoraris","sequence":"first","affiliation":[{"name":"Laboratory of Chemistry, Department of Food Science and Human Nutrition, Agricultural University of Athens, 75 Iera Odos, 11855 Athens, Greece"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Alexandra","family":"Skouria","sequence":"additional","affiliation":[{"name":"Laboratory of Chemistry, Department of Food Science and Human Nutrition, Agricultural University of Athens, 75 Iera Odos, 11855 Athens, Greece"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0003-3329-9398","authenticated-orcid":false,"given":"Panagiota-Kyriaki","family":"Revelou","sequence":"additional","affiliation":[{"name":"Laboratory of Chemistry, Department of Food Science and Human Nutrition, Agricultural University of Athens, 75 Iera Odos, 11855 Athens, Greece"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0003-3218-1718","authenticated-orcid":false,"given":"Eleftherios","family":"Alissandrakis","sequence":"additional","affiliation":[{"name":"Laboratory of Quality and Safety of Agricultural Products, Landscape and Environment, Department of Agriculture, Hellenic Mediterranean University, Stavromenos, PC 71410 Heraklion, Crete, Greece"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-5853-4780","authenticated-orcid":false,"given":"Petros A.","family":"Tarantilis","sequence":"additional","affiliation":[{"name":"Laboratory of Chemistry, Department of Food Science and Human Nutrition, Agricultural University of Athens, 75 Iera Odos, 11855 Athens, Greece"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Christos S.","family":"Pappas","sequence":"additional","affiliation":[{"name":"Laboratory of Chemistry, Department of Food Science and Human Nutrition, Agricultural University of Athens, 75 Iera Odos, 11855 Athens, Greece"}],"role":[{"vocabulary":"crossref","role":"author"}]}],"member":"1968","published-online":{"date-parts":[[2021,6,12]]},"reference":[{"key":"ref_1","unstructured":"(2021, February 01). Greek Statistical Authority. Available online: https:\/\/www.statistics.gr\/el\/statistics\/agr."},{"key":"ref_2","unstructured":"(2021, February 01). Pan-Hellenic Center for Export Research and Studies. Available online: http:\/\/www.pse.gr\/node\/145."},{"key":"ref_3","doi-asserted-by":"crossref","unstructured":"Cianciosi, D., Forbes-Hern\u00e1ndez, T.Y., Afrin, S., Gasparrini, M., Reboredo-Rodriguez, P., Manna, P.P., Zhang, J., Bravo Lamas, L., Mart\u00ednez Fl\u00f3rez, S., and Agudo Toyos, P. (2018). Phenolic Compounds in Honey and Their Associated Health Benefits: A Review. Molecules, 23.","DOI":"10.3390\/molecules23092322"},{"key":"ref_4","doi-asserted-by":"crossref","first-page":"110590","DOI":"10.1016\/j.biopha.2020.110590","article-title":"Molecular Mechanism-Based Therapeutic Properties of Honey","volume":"130","author":"Talebi","year":"2020","journal-title":"Biomed. Pharmacother."},{"key":"ref_5","doi-asserted-by":"crossref","first-page":"309","DOI":"10.1016\/j.foodchem.2015.09.051","article-title":"Honey: Chemical Composition, Stability and Authenticity","volume":"196","author":"Gauche","year":"2016","journal-title":"Food Chem."},{"key":"ref_6","doi-asserted-by":"crossref","first-page":"227","DOI":"10.1007\/BF02491721","article-title":"Analysis of Volatile Compounds of Rosemary Honey. Comparison of Different Extraction Techniques","volume":"57","author":"Cabezudo","year":"2003","journal-title":"Chromatographia"},{"key":"ref_7","doi-asserted-by":"crossref","first-page":"1032","DOI":"10.1016\/j.foodchem.2006.07.068","article-title":"A Review of Volatile Analytical Methods for Determining the Botanical Origin of Honey","volume":"103","author":"Pino","year":"2007","journal-title":"Food Chem."},{"key":"ref_8","doi-asserted-by":"crossref","first-page":"130","DOI":"10.1080\/00218839.1983.11100574","article-title":"Identification of the Volatile Components of Some Piedmontese Honeys","volume":"22","author":"Bicchi","year":"1983","journal-title":"J. Apic. Res."},{"key":"ref_9","doi-asserted-by":"crossref","first-page":"91","DOI":"10.1002\/jsfa.1934","article-title":"Evaluation of Four Isolation Techniques for Honey Aroma Compounds","volume":"85","author":"Alissandrakis","year":"2004","journal-title":"J. Sci. Food Agric."},{"key":"ref_10","doi-asserted-by":"crossref","first-page":"512","DOI":"10.1007\/s11694-016-9418-9","article-title":"Characterization of Key Aroma Compounds in a Representative Aromatic Extracts from Citrus and Astragalus Honeys Based on Aroma Extract Dilution Analyses","volume":"11","author":"Uckun","year":"2016","journal-title":"Food Meas."},{"key":"ref_11","doi-asserted-by":"crossref","unstructured":"Ku\u015b, P.M., and Jerkovi\u0107, I. (2018). New Sample Preparation Method for Honey Volatiles Fingerprinting Based on Dehydration Homogeneous Liquid\u2013Liquid Extraction (DHLLE). Molecules, 23.","DOI":"10.3390\/molecules23071769"},{"key":"ref_12","doi-asserted-by":"crossref","first-page":"1169","DOI":"10.1007\/s00217-018-3034-3","article-title":"Chromatographic Fingerprint, Antioxidant Activity, and Colour Characteristic of Polish Goldenrod (Solidago virgaurea L.) Honey and Flower","volume":"244","author":"Makowicz","year":"2018","journal-title":"Eur. Food. Res. Technol."},{"key":"ref_13","doi-asserted-by":"crossref","first-page":"96","DOI":"10.1080\/00218839.1992.11101268","article-title":"Characteristic Aroma Profiles of Unifloral Honeys Obtained with a Dynamic Headspace GC-MS System","volume":"31","author":"Bouseta","year":"1992","journal-title":"J. Apic. Res."},{"key":"ref_14","doi-asserted-by":"crossref","first-page":"1030","DOI":"10.1016\/j.foodchem.2011.05.070","article-title":"Characterization of the Volatile Profile of Thistle Honey Using Headspace Solid-Phase Microextraction and Gas Chromatography-Mass Spectrometry","volume":"129","author":"Bianchi","year":"2011","journal-title":"Food Chem."},{"key":"ref_15","doi-asserted-by":"crossref","first-page":"735","DOI":"10.1007\/s00217-016-2787-9","article-title":"Stir Bar Sorptive Extraction Coupled with GC\/MS Applied to Honey: Optimization of Method and Comparative Study with Headspace Extraction Techniques","volume":"243","author":"Petretto","year":"2016","journal-title":"Eur. Food Res. Technol."},{"key":"ref_16","doi-asserted-by":"crossref","first-page":"8152","DOI":"10.1021\/jf071442y","article-title":"Comparison of the Volatile Composition in Thyme Honeys from Several Origins in Greece","volume":"55","author":"Alissandrakis","year":"2007","journal-title":"J. Agric. Food Chem."},{"key":"ref_17","doi-asserted-by":"crossref","unstructured":"Xagoraris, M., Revelou, P.-K., Dedegkika, S., Kanakis, C.D., Papadopoulos, G.K., Pappas, C.S., and Tarantilis, P.A. (2021). SPME-GC-MS and FTIR-ATR Spectroscopic Study as a Tool for Unifloral Common Greek Honeys\u2019 Botanical Origin Identification. Appl. Sci., 11.","DOI":"10.3390\/app11073159"},{"key":"ref_18","doi-asserted-by":"crossref","first-page":"575","DOI":"10.1016\/S0308-8146(03)00013-X","article-title":"Ultrasound-Assisted Extraction of Volatile Compounds from Citrus Flowers and Citrus Honey","volume":"82","author":"Alissandrakis","year":"2003","journal-title":"Food Chem."},{"key":"ref_19","doi-asserted-by":"crossref","first-page":"793","DOI":"10.1002\/jssc.200301368","article-title":"Analysis of Volatile Composition of Honey by Solid Phase Microextraction and Gas Chromatography-Mass Spectrometry","volume":"26","author":"Soria","year":"2003","journal-title":"J. Sep. Sci."},{"key":"ref_20","doi-asserted-by":"crossref","first-page":"579","DOI":"10.1007\/s00217-008-0966-z","article-title":"SPME Followed by GC\u2013MS: A Powerful Technique for Qualitative Analysis of Honey Volatiles","volume":"228","author":"Soria","year":"2008","journal-title":"Eur. Food Res. Technol."},{"key":"ref_21","doi-asserted-by":"crossref","first-page":"1288","DOI":"10.1016\/j.foodchem.2010.11.079","article-title":"A Headspace Solid-Phase Microextraction Method Development and Its Application in the Determination of Volatiles in Honeys by Gas Chromatography","volume":"126","author":"Plutowska","year":"2011","journal-title":"Food Chem."},{"key":"ref_22","doi-asserted-by":"crossref","first-page":"1061","DOI":"10.1016\/j.foodchem.2013.08.139","article-title":"Screening of Volatile Compounds in Honey Using a New Sampling Strategy Combining Multiple Extraction Temperatures in a Single Assay by HS-SPME-GC-MS","volume":"145","author":"Bianchin","year":"2014","journal-title":"Food Chem."},{"key":"ref_23","doi-asserted-by":"crossref","unstructured":"Robotti, E., Campo, F., Riviello, M., Bobba, M., Manfredi, M., Mazzucco, E., Gosetti, F., Calabrese, G., Sangiorgi, E., and 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., 1\u201314.","DOI":"10.1155\/2017\/6437857"},{"key":"ref_24","doi-asserted-by":"crossref","first-page":"198","DOI":"10.1016\/j.lwt.2018.04.043","article-title":"Volatile Profile of Monofloral Honeys Produced in Brazilian Semiarid Region by Stingless Bees and Key Volatile Compounds","volume":"94","author":"Sousa","year":"2018","journal-title":"LWT"},{"key":"ref_25","doi-asserted-by":"crossref","first-page":"965","DOI":"10.1016\/j.talanta.2008.05.019","article-title":"Response Surface Methodology (RSM) as a Tool for Optimization in Analytical Chemistry","volume":"76","author":"Bezerra","year":"2008","journal-title":"Talanta"},{"key":"ref_26","unstructured":"(2021, May 20). Government Gazette B-239\/23-2-2005 Annex II Article 67 of Greek Food Code 2005. Available online: http:\/\/www.minagric.gr\/images\/stories\/docs\/agrotis\/MeliMelissokomia\/KYATaytopoiisi.pdf."},{"key":"ref_27","doi-asserted-by":"crossref","first-page":"363","DOI":"10.1016\/j.foodres.2013.11.032","article-title":"Characterization and Classification of Thymus capitatus (L.) Honey According to Geographical Origin Based on Volatile Compounds, Physicochemical Parameters and Chemometrics","volume":"55","author":"Karabagias","year":"2014","journal-title":"Food Res. Int."},{"key":"ref_28","doi-asserted-by":"crossref","first-page":"83","DOI":"10.1002\/sscp.201700027","article-title":"Volatile Metabolites or Pollen Characteristics as Regional Markers of Monofloral Thyme Honey?","volume":"1","author":"Karabagias","year":"2018","journal-title":"Sep. Sci. Plus"},{"key":"ref_29","doi-asserted-by":"crossref","first-page":"9514","DOI":"10.3390\/ijms12129514","article-title":"Volatile Compounds in Honey: A Review on Their Involvement in Aroma, Botanical Origin Determination and Potential Biomedical Activities","volume":"12","author":"Ndip","year":"2011","journal-title":"Int. J. Mol. Sci."},{"key":"ref_30","doi-asserted-by":"crossref","first-page":"175","DOI":"10.1080\/00218839.1988.11100798","article-title":"The Effect of Heat on the Volatile Flavour Fraction from a Unifloral Honey","volume":"27","author":"Visser","year":"1988","journal-title":"J. Apic. Res."},{"key":"ref_31","doi-asserted-by":"crossref","first-page":"1925","DOI":"10.1021\/jf00045a018","article-title":"Solid-Phase Microextraction for Flavor Analysis","volume":"42","author":"Yang","year":"1994","journal-title":"J. Agric. Food Chem."},{"key":"ref_32","doi-asserted-by":"crossref","first-page":"1843","DOI":"10.1021\/ac00062a008","article-title":"Headspace Solid-Phase Microextraction","volume":"65","author":"Zhang","year":"1993","journal-title":"Anal. Chem."},{"key":"ref_33","unstructured":"Helrich, K. (1990). Official Methods of Analysis of Association of Official Analytical Chemists, Association of Official Analytical Chemists. [15th ed.]."},{"key":"ref_34","unstructured":"Bogdanov, S. (2009). Harmonides Methods of the International Honey Commission, Swiss Bee Research Centre FAM. Available online: https:\/\/www.ihc-platform.net\/ihcmethods2009.pdf."},{"key":"ref_35","doi-asserted-by":"crossref","first-page":"139","DOI":"10.1080\/0005772X.1978.11097714","article-title":"Methods of melissopalynology","volume":"59","author":"Louveaux","year":"1978","journal-title":"Bee World"},{"key":"ref_36","doi-asserted-by":"crossref","first-page":"3319","DOI":"10.1002\/jsfa.10961","article-title":"Botanical origin discrimination of Greek honeys: Physicochemical parameters versus Raman spectroscopy","volume":"101","author":"Xagoraris","year":"2021","journal-title":"J. Sci. Food Agric."},{"key":"ref_37","doi-asserted-by":"crossref","first-page":"1","DOI":"10.1111\/j.2517-6161.1951.tb00067.x","article-title":"On the Experimental Attainment of Optimum Conditions","volume":"13","author":"Box","year":"1951","journal-title":"J. R. Stat. Soc. Ser. B Stat Methodol."},{"key":"ref_38","doi-asserted-by":"crossref","unstructured":"Al-Suod, H., Ratiu, I.-A., G\u00f3recki, R., and Buszewski, B. (2019). Pressurized liquid extraction of cyclitols and sugars: Optimization of extraction parameters and selective separation. J. Sep. Sci.","DOI":"10.1002\/jssc.201801269"},{"key":"ref_39","doi-asserted-by":"crossref","unstructured":"Al-Suod, H., Ratiu, I., Krakowska-Sieprawska, A., Lahuta, L., G\u00f3recki, R., and Buszewski, B. (2019). Supercritical fluid extraction in isolation of cyclitols and sugars from chamomile flowers. J. Sep. Sci.","DOI":"10.1002\/jssc.201900539"},{"key":"ref_40","unstructured":"Adams, R.P. (2007). Identification of Essential Oil Components by Gas Chromatography\/Mass Spectrometry, Allured Pub Corp. [4th ed.]."}],"container-title":["Molecules"],"original-title":[],"language":"en","link":[{"URL":"https:\/\/www.mdpi.com\/1420-3049\/26\/12\/3612\/pdf","content-type":"unspecified","content-version":"vor","intended-application":"similarity-checking"}],"deposited":{"date-parts":[[2025,10,11]],"date-time":"2025-10-11T06:13:42Z","timestamp":1760163222000},"score":1,"resource":{"primary":{"URL":"https:\/\/www.mdpi.com\/1420-3049\/26\/12\/3612"}},"subtitle":[],"short-title":[],"issued":{"date-parts":[[2021,6,12]]},"references-count":40,"journal-issue":{"issue":"12","published-online":{"date-parts":[[2021,6]]}},"alternative-id":["molecules26123612"],"URL":"https:\/\/doi.org\/10.3390\/molecules26123612","relation":{},"ISSN":["1420-3049"],"issn-type":[{"value":"1420-3049","type":"electronic"}],"subject":[],"published":{"date-parts":[[2021,6,12]]}}}