Quality Control Of Honey Research Articles

Study of authenticity, quality characteristics and bioactivity in honey samples from different botanical origins and countries

Honey is a widely consumed commodity featuring beneficial nutritional properties resulting in a high market price. Therefore, honey is a target of fraudulent practices and analytical strategies to assess honey quality and origin are highly needed. Within this context, we performed a comprehensive analytical testing for 39 honey samples originating from Greece and other countries. Analytical parameters related to honey quality control (Directive 2001/110/EC) were monitored. In detail, hydroxymethylfurfural (HMF) and diastase activity were measured using spectrophotometric assays. Importantly, 6 samples imported by the American market exceeded the regulatory limit (40 mg/kg). The content of the main honey sugars was monitored using an accredited ultra-high-performance liquid chromatography coupled to evaporative light scattering detector (UHPLC-ELSD) and all samples were in line with the regulatory standards. In addition, chromatographic analysis was performed to determine 23 phenolic compounds as these are bioactive compounds contributing towards the health promoting effects of honey. Besides chemical characterisation, in vitro testing was also performed by monitoring the inhibitory effect of the honey samples towards acetylcholinesterase (AChE) and pancreatic lipase (PNLIP). Indeed, inhibition was noticed and in the case of PNLIP the monitored differences between Greek and samples from other countries were statistically significant. To assess honey sample authenticity, chemometric tools were employed, namely, principal component analysis (PCA), hierarchical cluster analysis (HCA) and linear discriminant analysis (LDA). The multivariate analysis revealed that the taxifolin content may be used as a marker for thyme honey from Cyprus while the total content of gallic and protocatechuic acids could be used as a marker for oak honeys. All in all, implementing several different methods based on different principles (both physicochemical and bioanalytical) in a complex analytical matrix such as honey is a great analytical challenge that we successfully faced and comprehensively demonstrated in this study.

Highly sensitive adulteration detection in kelulut honey utilizing fiber Bragg grating technology with Q-switched pulse erbium-doped fiber laser and innovative spider silk substrate

The growing field of photonics has seen significant developments in optical pulse fiber-based sensing technologies. In this research, a novel fiber Bragg grating using a Q-switched erbium-doped fiber laser source and innovative spider silk as a base material is presented, specifically designed for the detection of adulteration in pure kelulut honey. Kelulut honey has attracted much attention from Malaysian researchers as it is a highly prized, versatile local health remedy. During the experimental setup, concentrations of the adulterant isoglucose ranging from 0 % to 8 % and 10–50 % were intentionally added to the pure kelulut honey. The sensor showed remarkable sensitivity and detected subtle shifts in both the wavelength and radio frequency spectrum. The experimental results obtained emphasize the effectiveness of the proposed sensor and demonstrate its exceptional sensitivity in detecting adulteration in pure kelulut honey. This inherent property makes the derived pulse fiber laser sensor a promising tool for various applications in clinical detection and diagnosis as well as in the food industry. The results presented here not only contribute to the field of photonics but also have the potential to advance the quality control and authenticity assessment of kelulut honey in various fields.

3α-Hydroxylup-20(29)-ene-23,28-dioic Acid as a Phytogenic Chemical Marker for Authenticating Schefflera octophylla (Lour.) Harms Monofloral Honey.

The monofloral honey from Schefflera octophylla (Lour.) Harms (MH-Sco) are of high economic value due to their rarity and potential medicinal benefits. However, the limited investigations on the relationship of phytogenic components between the plant S. octophylla (P-Sco) and MH-Sco have an impact on MH-Sco authentication. Herein, the tentative phytogenic markers of MH-Sco were screened by comparing the metabolites of MH-Sco obtained by ultrahigh-performance liquid chromatography-quadrupole time-of-flight tandem mass spectrometry (UHPLC-Q-TOF-MS/MS)-based untargeted metabolomics with the identified phytogenic chemicals from P-Sco. Combined with the mass and NMR spectral information, 3α-hydroxylup-20(29)-ene-23,28-dioic acid (HLEDA) was finally identified as the phytogenic marker of MH-Sco. A targeted ultrahigh-performance liquid chromatography-triple quadrupole mass spectrometry (UHPLC-QqQ-MS/MS)-based method was established and validated based on the purified monomer standard to measure HLEDA levels in honey samples. HLEDA determined in MH-Sco was with the content from 0.303 to 0.440 mg/kg, while HLEDA was absent in honey samples from other botanical origins, indicating the reliability of HLEDA as a chemical marker in MH-Sco authentication. This study provides the theoretical basis and industry guidance for honey quality control for commercial consumption.

Comprehensive Elemental Profiling of Romanian Honey: Exploring Regional Variance, Honey Types, and Analyzed Metals for Sustainable Apicultural and Environmental Practices.

We investigated the mineral concentrations of 61 honey samples from eight Romanian regions, employing advanced techniques to assess 30 chemical elements. Potassium emerged as the dominant element, showcasing significant variations across geographical locations. Essential minerals like calcium, magnesium, sodium, and manganese maintained consistent levels, while zinc, copper, and chromium were present in smaller proportions. Critically, lead and cadmium levels exceeded established safety limits in some samples, suggesting potential environmental contamination. Additionally, elevated levels of lithium, strontium, nickel, and aluminum were detected, hinting at possible atmospheric pollution. These findings highlight the importance of regional analysis, as mineral content varied significantly between locations. Furthermore, correlation analysis revealed interdependencies among elements, suggesting shared environmental influences. Advanced statistical techniques like hierarchical clustering and principal component analysis effectively captured the impact of geographical origin on honey composition. These insights contribute valuable information for future efforts in honey quality control, traceability systems, and regulatory measures. By providing valuable insights into environmental influences on honey composition, this study informs future research endeavors and paves the way for the development of robust regulatory measures to ensure honey safety for consumers.

Dynamic variation in the aroma characteristics of Rhus chinensis honey at different stages after capping

The ripening characteristics after capping of honey are favourable for improving its quality. However, research on the variation and formation of aroma characteristics of honey in this process is lacking. Therefore, the present study was carried out with different stages of Rhus chinensis honeys (RCHs) after capping and identified 192 volatiles with varying levels of concentration. “Fruity” was the main aroma characteristic of RCHs at different stages after capping, mainly contributed by (E)-β-damascenone. Methyl salicylate might be a potential indicator for differentiating RCHs at different stages after capping. The metabolic pathway analyses revealed that the aroma compounds in RCHs undergo transformation at different stages after capping, which subsequently affects its aroma characteristics formation. This work is the first to study the dynamic changes in honey aroma characteristics after capping from multiple perspectives, and the results are of great significance for understanding the aroma characteristics after capping and quality control of honey.

Honey produced by apini and meliponini in Brazil: multivariate analysis of physicochemical parameters, sugar and metabolite profiles

The objective of this study was to investigate honey samples from two bee tribes grouped in Meliponini (stingless bee) and Apini (Apis mellifera) honeys from Brazil, in order to compare their chemical composition. Thirty-four honey samples were collected and evaluated by proton NMR spectroscopy, HPLC and physicochemical parameters, using chemometric methods. Principal component analysis (PCA) was able to discriminate Apini and Meliponini goups. Additionally, the partial least squares discriminant analysis (PLS-DA) models were able to predict the Apini and Meliponini honey samples with sensitivity, specificity and accuracy values close to 100%. Frequency values between 4.00 − 3.00 ppm, corresponding to the sugar region, were important for the classification by the PLS-DA model using NMR data. For the PLS-DA model using physicochemical data, the main parameters for classification were water activity, reducing sugar, moisture, refractive index, total soluble solids, maltose and glucose. Since stingless honeys have no regulation, the data presented in this study can compose a database to assist in the establishment of regulatory criteria. Moreover, the chemometric models proposed can be used as a tool for the quality control of honey, especially for authentication purposes.

A guide for quality control of honey: Application of UV–vis scanning spectrophotometry and NIR spectroscopy for determination of chemical profiles of floral honey produced in southern Brazil

This study aimed to determine the chemical profile of floral honey by ultraviolet and visible spectrophotometry (UV–vis) and near-infrared (NIR) vibrational spectroscopy, and via analysis of the total phenolic content, considering the harvest year (2018–2019 and 2019–2020), geographic and botanical origins, and seasonality of samples (n = 116) collected in southern Brazil. The total phenolic content (TPC) of honey showed great variation by geographic origin and for both harvests, with a higher overall average in the 2019–2020 (3.81–7.22 mg/mL) compared to the 2018–2019 (2.49–6.17 mg/mL), which seemed to be related to climatic factors, mainly precipitation. The visual inspection of the UV–vis spectra (280–320 nm) revealed two samples with distinct chemical compositions, being these further confirmed as outlier by PCA. UV–vis (260–360 nm) coupled to PCA was able to distinguish honey with higher and lower TPC. The NIR spectral data set revealed discrepancies among honey according to the harvest seasons, with bands associated with higher water content and lower carbohydrate amounts in the 2018–2019-collected samples; the contrary has been noted for the 2019–2020. Thus, UV–vis and NIR spectroscopies coupled to PCA proved to be a useful approach to distinguish honey samples as to possible adulterations and geographic origin associated with their higher and lower phenolic contents.

Metabolomic analysis reveals linkage between chemical composition and sensory quality of different floral honey samples

Honey has a distinct flavor characterized by various volatiles and non-volatiles from diverse origins. In this study, metabolomics combined with sensory analysis was performed to identify relationships between chemical profile and sensory quality of honey. Targeted metabolomic analysis was conducted to determine volatile and non-volatile profiles of seven different honey. Volatile profile was analyzed using headspace solid-phase microextraction (HS-SPME) coupled to GC − MS. LC − MS/MS, HPLC − UV, and HPLC-RI were employed to analyze flavonoids, organic acids, and sugars, respectively. Authentic standards were utilized for confirmation of metabolites. Sensory evaluation included quantitative descriptive analysis and consumer acceptance test. The results showed that sucrose (sweetness) was responsible for a positive hedonic perception, while organic acids and flavonoids (sourness, astringency, bitterness) negatively affected consumer acceptance. Volatiles with floral notes (e.g. decyl formate) were preferred, but others with off-flavors (e.g. 2-methylbenzofuran) were not preferred by consumers. Flavor familiarity was strongly correlated with the consumer acceptance of honey, indicating that the balance between volatiles and non-volatiles is significant for honey flavor quality. This work demonstrates the role of key flavor compounds in honey quality, and may be applicable to the quality control of honey.

Rapid and Automated Method for Detecting and Quantifying Adulterations in High-Quality Honey Using Vis-NIRs in Combination with Machine Learning.

Honey is one of the most adulterated foods, usually through the addition of sweeteners or low-cost honeys. This study presents a method based on visible near infrared spectroscopy (Vis-NIRs), in combination with machine learning (ML) algorithms, for the correct identification and quantification of adulterants in honey. Honey samples from two botanical origins (orange blossom and sunflower) were evaluated and adulterated with low-cost honey in different percentages (5%, 10%, 15%, 20%, 25%, 30%, 35%, 40%, 45%, and 50%). The results of the exploratory analysis showed a tendency to group the samples according to botanical origin, as well as the presence of adulteration. A supervised analysis was performed to detect the presence of adulterations. The best performance with 100% accuracy was achieved by support vector machines (SVM) and random forests (RF). A regression study was also carried out to quantify the percentage of adulteration. The best result was obtained by support vector regression (SVR) with a coefficient of determination (R2) of 0.991 and a root mean squared error (RMSE) of 1.894. These results demonstrate the potential of combining ML with spectroscopic data as a method for the automated quality control of honey.

Physicochemical Characterization and Sugar Profile of Argentinian Honeys from the Phytogeographic Provinces Paranaense and Pampeana in Misiones

The characterization of honeys from the Biomes and vegetation units of the Phytogeographical Provinces (PP) located in the Province of Misiones (Argentina) was performed by analysis of sugar profile and physicochemical parameters (Free Acidity, pH, Electrical Conductivity (EC), colour and contents of moisture, ash, total soluble solids and hydroxymethylfurfural) used for quality control of honey. The honeys analysed were authentic and traceable, and met the specifications of the national and/or international standards for the evaluated parameters, denoting blossom origin and confirming high quality, maturity and freshness. The influence of biome and Vegetation Units (VU) on physical and chemical parameters of the studied honeys was defined regarding both flora and pedoclimatic conditions. Honeys from VU-27 presented significantly higher contents of fructose, ash and total soluble solids, pH and EC and lower moisture content than those from VU-3. To the authors’ best knowledge, sugar profiles, free acidity and contents of ash and total soluble solids in honeys from the different PPs, vegetation units and Biomes of Misiones are reported for the first time. This study contributes to the classification of honeys from Misiones, helping to increase added value and access new markets.

Physicochemical Characterization Of Argentinian Honeys From The Phytogeographic Provinces Pampeana, Espinal And Monte Based On Their Sugar Profiles And Quality Parameters

The honeys from the Phytogeographic Provinces (PP) of the south of Buenos Aires province (Argentina) were characterised by the sugar composition and physicochemical parameters used for honey quality control. A large set (n=329) of traceable raw honey samples obtained from beekeepers were analysed and met the specifications of the national and/or international standards for the evaluated parameters, which denoted their blossom origin and confirmed their authenticity, good maturity and freshness. The influence of flora and the pedoclimatic conditions of each phytogeographical region, as well as their beekeeping practices, on the physical and chemical properties of honey allowed its characterization. Thus, the honeys from the southeast of Buenos Aires province were characterized by higher contents of moisture, fructose, maltose, erlose, hydroxymethylfurfural (HMF) and ash, pH and electrical conductivity (EC) and slightly lighter colours; while southwest honeys showed higher free acidities, sucrose content and ºBrix values. Honeys from the PP Espinal exhibited characteristic lower contents of fructose, HMF and ash and EC values, and larger amounts of sucrose. Honeys from the PP Monte presented typical lower moisture contents and slightly darker colours. Honeys from the PP Pampeana were typified by higher amounts of fructose.

Application of an Electronic Nose as a New Technology for Rapid Detection of Adulteration in Honey

This work demonstrates the application of an electronic nose (e-nose) for discrimination between authentic and adulterated honey. The developed e-nose is based on electrodes covered with ionogel (ionic liquid + gelatin + Fe3O4 nanoparticle) films. Authentic and adulterated honey samples were submitted to e-nose analysis, and the capacity of the sensors for discrimination between authentic and adulterated honey was evaluated using principal component analysis (PCA) based on average relative response data. From the PCA biplot, it was possible to note two well-defined clusters and no intersection was observed. To evaluate the relative response data as input for autonomous classification, different machine learning algorithms were evaluated, namely instance based (IBK), Kstar, Trees-J48 (J48), random forest (RF), multilayer perceptron (MLP), naive Bayes (NB), and sequential minimal optimization (SMO). Considering the average data, the highest accuracy was obtained for Kstar: 100% (k-fold = 3). Additionally, this algorithm was also compared regarding its sensitivity and specificity, both being 100% for both features. Thus, due to the rapidity, simplicity, and accuracy of the developed methodology, the technology based on e-noses has the potential to be applied to honey quality control.

ANALYSIS AND CHEMICAL PROFILING OF HONEY USING 1H-NMR SPECTROSCOPY, FTIR SPECTROSCOPY AND TLC USING VARIOUS CHROMOGENIC REAGENTS FOR DERIVATIZATION

Objective: Honey is a natural sweet substance known for various health benefits and is used in many traditional medicines and dietary supplements. It contains various bioactive constituents like sugars, amino acids, polyphenols, flavonoids and various minerals. Quality control of honey is an essential part for ensuring its health benefits and therapeutic usage. In the present study, honey was analyzed by using various spectroscopic approaches and physicochemical methods. Methods: The samples of honey were analyzed by Thin-layer Chromatography (TLC) derivatization, ATR-FTIR, and 1H-NMR fingerprint and the total phenolic content (TPC) and total flavonoid contents (TFC) were measured by Uv-Vis spectrophotometry and analysis were carried out for various physicochemical parameters of honey. Results: All the physicochemical parameters of the honey were as per the desired quality. The UV-Vis analysis was successfully used in the determination of total phenolics and flavonoid contents in the samples of honey. TLC analysis showed the presence of flavonoids, phytosterols, phenolics, sugars and carbohydrates in honey. The Thin-Layer chromatography analysis showed good resolution for various components of honey on the TLC plates. The FTIR analysis showed the presence of various functional groups characteristic of amino acids, carbohydrates and sugars, which was further supported by 1H NMR chemical profiling. Conclusion: In the present work, the application of various spectroscopic techniques and physicochemical tests were found to be useful in analysis of honey.

Identification of the botanical origins of honey based on nanoliter electrospray ionization mass spectrometry

The botanical origins of honey are important for the quality control and commercialization of honey. In this research, we established a nanoliter electrospray ionization mass spectrometry (Nano-ESI-MS) method to identify Castanopsis honey (CH), Eurya honey (EH), Dendropanax dentiger honey (DH), and Triadica cochinchinensis honey (TH). In total, 38 compounds were identified based on the collision-induced dissociation experiments by Nano-ESI-MS with 16 differential compounds and 7 quantified as potential differential markers. These four types of honey were distinguished from each other by their mass spectrometry data combined with multivariate analysis with three out of the 7 differential markers, i.e., phenethylamine, tricoumaroyl spermidine, and (+/–)-abscisic acid, identified as potential markers for CH, EH, and DH, respectively. Both the qualitative and quantitative results derived from Nano-ESI-MS were further verified by UPLC-Q/TOF-MS. Our studies provided the significant potential of the Nano-ESI-MS method in the identification of the botanical origins of different kinds of honey.

Evaluation of physicochemical properties of honey powder using rice and pea proteins as carriers

Honey is a special product widely appreciated because of its peculiar flavor and aroma as well as its beneficial effects on health due to its constituents. However, the use of honey in its natural form can present several disadvantages to the food industry because of its high viscosity and density. This work aimed to obtain honey powder using rice, pea, or a mixture of both proteins as carriers by spray drying and to characterize physiochemically. Also, the mass balance was performed to evaluate changes in humidity and temperature that occurred by the drying air during the process. The honey showed acceptable physicochemical parameters by the legislation of honey quality control in regard to color (143.43 ± 4.34) mm Pfund, free acidity (46.41 ± 0.53) meq/kg, pH (3.73 ± 0.03), fructose content (46.52 ± 0.56) g/100 g and glucose content (35.88 ± 0.16) g/100 g, which leads to the production of honey powder. Among the carriers tested, the honey powder using rice protein achieved the highest powder recovery yield at (64.88 ± 0.64) %. The physicochemical properties were evaluated and the phenolic compounds were not negatively affected by spray drying conditions, maintaining a value of gallic acid equivalent (GAE) content at (301.31 ± 20.95) mg/kg of honey. Therefore, this work shows honey as an alternative food ingredient in powdered form, including the growing market for using alternative protein.

Honey powder produced by spray drying as an ingredient: A new perspective using a plant-based protein as a carrier

Honey is an excellent alternative to be used in different applications by the food, pharmaceutical, and cosmetics industries. However, the use of honey in its liquid form can present several disadvantages due to its high viscosity and density. In addition, honey can naturally crystallize during storage time, limiting its application in new products by industries. Thus, an alternative to using liquid honey in industry is the powder form. The objective of this study was to obtain honey powder by spray drying using a plant-based protein as a carrier. The honey used as raw material showed acceptable physicochemical parameters by the legislation of honey quality control, such as pH of (4.0 ± 0.1), the water content of (20.70 ± 0.3) g/100 g, ash of (0.48 ± 0.02) g/100 g, the fructose content of (35.42 ± 0.14) g/100 g, (43.05 ± 0.46) g/100 g for glucose, (0.56 ± 0.02) g/100 g for sucrose, and 5-hydroxymethylfurfural (HMF) value of (37.47 ± 1.04) mg/kg of honey, leading to the production of the honey powder. The mixture of fresh honey and plant-based protein was made with dispersions of 15, 16 and 18 g/100 g of honey using isolated rice protein as a carrier (total solid at 30 g/100 g d.b.). Finally, the honey powder produced was physicochemically characterized. The dispersion with 16 g/100 g of honey achieved an intermediary sugar/honey recovery of 35.93 ± 0.82% and 68.54 ± 2.16% of total protein recovery, and the spray drying yield was satisfactory > 50%. The overall results suggested that this dispersion is the ideal formulation when commercialization of the honey powder as an ingredient is intended.

Chemical composition of volatile components in the honey of some species of stingless bees

Using the technique of headspace solid-phase microextraction in combination with gas chromatography and mass spectrometric detection (HS-SPME/GC-MS), the composition of the volatile organic compounds (VOCs) of the honey of four species of stingless bees was studied in comparison with the honey of Apis mellifera bees. Peaks for 284 volatile components were registered on the chromatograms. Only eight components were present in all six studied samples. A high level of specificity in the composition of VOCs is a prerequisite for differentiating honey produced by different types of stingless bees and honey bees. Several specific features have been identified that are characteristic of the composition of VOCs in the honey of each species of stingless bees. These characteristics can be used to distinguish it from the honey of A. mellifera. The data obtained indicate the applicability of the HS-SPME/GC-MS technique for establishing the origin and for quality control of stingless bee honey.

Physicochemical Characterization Of Argentinian Honeys From The Phytogeographic Provinces Pampeana, Espinal And Monte Based On Their Sugar Profiles And Quality Parameters

The honeys from the Phytogeographic Provinces (PP) of the south of Buenos Aires province (Argentina) were characterised by the sugar composition and physicochemical parameters used for honey quality control. A large set (n=329) of traceable raw honey samples obtained from beekeepers were analysed and met the specifications of the national and/or international standards for the evaluated parameters, which denoted their blossom origin and confirmed their authenticity, good maturity and freshness. The influence of flora and the pedoclimatic conditions of each phytogeographical region, as well as their beekeeping practices, on the physical and chemical properties of honey allowed its characterization. Thus, the honeys from the southeast of Buenos Aires province were characterized by higher contents of moisture, fructose, maltose, erlose, hydroxymethylfurfural (HMF) and ash, pH and electrical conductivity (EC) and slightly lighter colours; while southwest honeys showed higher free acidities, sucrose content and ºBrix values. Honeys from the PP Espinal exhibited characteristic lower contents of fructose, HMF and ash and EC values, and larger amounts of sucrose. Honeys from the PP Monte presented typical lower moisture contents and slightly darker colours. Honeys from the PP Pampeana were typified by higher amounts of fructose.

Quality of Honey Produced by Four Species Of Stingless Bees in the Central Region of the State of Tocantins

Meliponiculture, the rational breeding of native stingless bees, is considered an excelente sustainable alternative to assist in the pollination process and is an economically viable activity. In the cerrado of Tocantins, the meliponine species that stand out most due to their wide distribution are: Scaptotrigona tubiba, Melipona fasciculata,M. rufiventris and Tetragonisca angustula. The bibliographic collection about these species is still little explored, hence there is a need for research to deepen the existing knowledge in the area. For this reason, the aim of this study was: a) to quantify the honey production of four meliponine species: T. angustula, M. fasciculata, M. rufiventris, and S. tubiba; b) to determine the physicochemical characteristics of the product; c) measure the biological parameters of the colony and d) evaluate the profile and sensory acceptance of honey in the municipalities, Palmas and Miracema, in the Tocantins. The study evaluated the biological parameters of the colony, honey production, and physicochemical analysis. The highest honey production came from the species T. angustula in the two collections for the municipality of Palmas. For Miracema, the species S. tubiba and M. fasciculata were evaluated, respectively. The physicochemical parameters evaluated fit the norms assigned to honey quality control. Results showed that honey from M. fasciculata was the sensory profile that obtained the best average among the characteristics observed in the study. There was a positive and negative correlation between the biological parameters, with a significant difference only between the characters’ height and diameter of the honey pot.

Study of Quality Factor (Q) and Phase Angle (θ) obtained per electrical impedance to characterization and detection adulteration in honey.

The quality control of honey is very important for the food industry and for the final consumer. Honey has constantly been the target of adulteration, usually with the aim of illegally increasing profit. However, the analytical methods used in the fraud investigation sometimes are very complex and beyond time-consuming. Electrical measurements appear as a good alternative to the traditional methods of analysis due to its practicality and low costs. In order to show the applicability of some electrical parameters derived from the impedance technique for honey quality control analysis, in the present study, samples were purposefully adulterated with syrup to simulate adulteration conditions. Then, they were submitted to electrical impedance analysis with frequency scanned from 10 Hz to 2 MHz. The impedance module (Z), the phase angle and the quality factor (Q) data were collected and studied. The results showed that there is a linear correlation between the frequencies relative to the peaks of the Q for samples and adulterant concentration with coefficient of determination of ~0.992. The proposal to use the Q as a property to be used in methodologies of analysis is the main contribution from this study, since it is traditionally little mentioned in the literature.