Unifloral Autumn Heather Honey from Indigenous Greek Erica manipuliflora Salisb.: SPME/GC-MS Characterization of the Volatile Fraction and Optimization of the Isolation Parameters

Abstract

For long heather honey has been a special variety due to its unique organoleptic characteristics. This study aimed to characterize and optimize the isolation of the dominant volatile fraction of Greek autumn heather honey using solid-phase microextraction (SPME) followed by gas chromatography-mass spectrometry (GC-MS). The described approach pointed out 13 main volatile components more closely related to honey botanical origin, in terms of occurrence and relative abundance. These volatiles include phenolic compounds and norisoprenoids, with benzaldehyde, safranal and p-anisaldehyde present in higher amounts, while ethyl 4-methoxybenzoate is reported for the first time in honey. Then, an experimental design was developed based on five numeric factors and one categorical factor and evaluated the optimum conditions (temperature: 60 °C, equilibration time: 30 min extraction time: 15 min magnetic stirrer velocity: 100 rpm sample volume: 6 mL water: honey ratio: 1:3 (v/w)). Additionally, a validation test set reinforces the above methodology investigation. Honey is very complex and variable with respect to its volatile components given the high diversity of the floral source. As a result, customizing the isolation parameters for each honey is a good approach for streamlining the isolation volatile compounds. This study could provide a good basis for future recognition of monofloral autumn heather honey.

Characterization of Ikaria Heather Honey by Untargeted Ultrahigh-Performance Liquid Chromatography-High Resolution Mass Spectrometry Metabolomics and Melissopalynological Analysis

“…Isophorone (tR = 7.74, with m/z 138.1045, Table 1), a norisoprenoid compound, was identified in Anama honey samples while its MS spectrum and MS/MS fragments are presented in Figure 6. Norisoprenoid compounds, usually identified by means of gas chromatography, have been reported as constituentsmarkers of heather honey from Greece (Xagoraris et al, 2021) and other countries (Castro-Vázquez et al, 2012); hence, this work comes to verify previous findings. Isophorone has also been reported as a constituent of essential oils of Eruca vesicaria, a plant found in Aegean Islands (Hichri et al, 2019) and in Crocus species from Greece (Lamari et al, 2018).…”

“…4ethylbenzaldehyde (tR = 7.73, with m/z 134.0731, Table 1) can be utilized as a discriminating chemical compound of Anama. Benzaldehyde has been identified as a Greek heather honey constituent using GC-MS (Xagoraris et al, 2021), while its ethylated derivative has been detected for the first time in this work in Anama heather honey samples by LC-HRMS. Cuminaldehyde (tR = 16.43, with m/z 148.0889, Table 1), another benzaldehyde derivative, was differentially increased in Anama honey.…”

“…However, the exact geographical origin of the Greek samples was not provided, while melissopalynological and physicochemical analyses were not conducted (Koulis et al, 2021). Another work performed by using solid-phase microextraction and gas chromatography-mass spectrometry has been focused on volatile constituents of Greek heather honey (Xagoraris et al, 2021).…”

Simultaneous qualitative and quantitative analyses of volatile components in Chinese honey of six botanical origins using headspace solid‐phase microextraction and gas chromatography–mass spectrometry

“…14 The most commonly used techniques for the detection of volatile compounds in honey are gas chromatography (GC) and gas chromatography-coupled mass spectrometry (GC-MS) combined with different sample extraction methods involving liquid-liquid extraction (LLE), 15 simultaneous steam distillation extraction (SDE), 16 dynamic headspace also known as purge and trap (DHS), 17 ultrasound-assisted extraction (USE), 18 solidphase extraction (SPE), 19 and solid-phase microextraction (SPME). [20][21][22] Among them, the SPME method has been validated to be fast, simple, inexpensive, highly sensitive, and solventfree. 3 Moreover, it can achieve a high level of automation and be easily connected with various analytical instruments online.…”

Authenticity of Honey: Characterization, Bioactivities and Sensorial Properties

“…Xagoraris et al [9] analyzed the main volatile compounds of 25 autumn heather honeys from the indigenous Greek Erica manipuliflora using solid-phase microextraction (SPME) methodology, followed by gas chromatography-mass spectrometry (GC-MS). This is the first study to identify a volatile profile of honey from E. manipuliflora.…”