Analysis Of Honey Samples Research Articles

Development of a new microextraction method based on elevated temperature dispersive liquid–liquid microextraction for determination of triazole pesticides residues in honey by gas chromatography-nitrogen phosphorus detection

In the present study, a rapid, highly efficient, and reliable sample preparation method named “elevated temperature dispersive liquid–liquid microextraction” followed by gas chromatography-nitrogen-phosphorus detection was developed for the extraction, preconcentration, and determination of five triazole pesticides (penconazole, hexaconazole, diniconazole, tebuconazole, and difenoconazole) in honey samples. In this method the temperature of high-volume aqueous phase was adjusted at an elevated temperature and then a disperser solvent containing an extraction solvent was rapidly injected into the aqueous phase. After cooling to room temperature, the phase separation was accelerated by centrifugation. Various parameters affecting the extraction efficiency such as type and volume of the extraction and disperser solvents, temperature, salt addition, and pH were evaluated. Under the optimum extraction conditions, the method resulted in low limits of detection and quantification within the range 0.05–0.21ngg−1 in honey (15–70ngL−1 in solution) and 0.15–1.1ngg−1 in honey (45–210ngL−1 in solution), respectively. Enrichment factors and extraction recoveries were in the ranges of 1943–1994 and 97–100%, respectively. The method precision was evaluated at 1.5ngg−1 of each analyte, and the relative standard deviations were found to be less than 4% for intra-day (n=6) and less than 6% for inter-days. The method was successfully applied to the analysis of honey samples and difenoconazole was determined at ngg−1 levels.

Quantification of saccharides in honey samples through surface-assisted laser desorption/ionization mass spectrometry using HgTe nanostructures.

Quantification of monosaccharides and disaccharides in five honey samples through surface-assisted laser desorption/ionization mass spectrometry (SALDI-MS) using HgTe nanostructures as the matrix and sucralose as an internal standard has been demonstrated. Under optimal conditions (1× HgTe nanostructure, 0.2mM ammonium citrate at pH9.0), the SALDI-MS approach allows detection of fructose and maltose at the concentrations down to 15 and 10μM, respectively. Without conducting tedious sample pretreatment and separation, the SALDI-MS approach allows determination of the contents of monosaccharides and disaccharides in honey samples within 30min, with reproducibility (relative standard deviation <15%). Unlike only sodium adducts of standard saccharides detected, sodium adducts and potassium adducts with differential amounts have been found among various samples, showing different amounts of sodium and potassium ions in the honey samples. The SALDI-MS data reveal that the contents of monosaccharides and disaccharides in various honey samples are dependent on their nectar sources. In addition to the abundant amounts of monosaccharides and disaccharides, oligosaccharides in m/z range of 650 - 2700 are only detected in pomelo honey. Having advantages of simplicity, rapidity, and reproducibility, this SALDI-MS holds great potential for the analysis of honey samples.

Instrumental Neutron Activation Analysis of Honey Samples from Lokoja and Suleija North Central Nigeria

Instrumental Neutron Activation Analysis (INAA) using Ghana Research Reactor (GHARR-1) at the Ghana Atomic Energy Commission (GHAEC) operating at 15kW at a thermal flux of 5 x10n cms was used to determine nine elements in honey samples from Lokoja and Suleija North Central Nigeria. The elements were; Al, Br, Ca, Cl, K, Mg, Mn, Na, and V. The concentration of the elements varied in the different samples ranging from few ppm to few percentages.

Melittopalynological Investigations of Honey from Sunderban region, West Bengal, India

In the present study, nectar sources to honey bees were studied based on microscopical analysis of honey samples collected in mangrove forest of Sunderbans, West Bengal, India. In all 12 honey samples were col- lected, 9 from Apis mellifera colonies and 3 from A. dorsata colonies. Qualitative and quantitative Melittopal- ynological analysis of the honey samples collected from A. mellifera showed that six samples were unifloral and three samples were multifloral. Ceriops decandra is predominant pollen type in 5 samples and Aegiceras corniculatum in one sample. The secondary pollen types were of Bruguiera gymnorrhiza, Sonneratia apetala and Bunium persicum .A total of 37 plant species served as sources of bee forage to A. mellifera. C. decandra was predominant pollen type in two samples and as secondary pollen type in one sample of A. dorsata. Kandelia candel pollen is associated as sec- ondary source in all the three samples of A. dorsata .I t is not found in A. mellifera samples.

Suitability of three-dimensional synchronous fluorescence spectroscopy for fingerprint analysis of honey samples with reference to their phenolic profiles

The suitability of a right-angle geometry three-dimensional synchronous fluorescence spectroscopy (3D-SFS) for the differentiation and classification of different honey types, including acacia, buckwheat, heather, linden, multiflower and rape honeys, was evaluated with reference to their phenolic profiles. The fraction of phenolic compounds was initially isolated and pre-concentrated from analyzed samples by means of polymeric reversed phase Strata X solid phase extraction (SPE) cartridges. A thoughtful analysis of 3D-SF spectra of resulting methanolic extracts of honey samples containing the separated fraction of phenolics and standards of phenolic acids and flavonoids revealed that the proposed methodology based on SPE and 3D-SFS is capable of discriminating honey samples due to different floral sources in a fast and straightforward way.

Colorimetric Detection of Reducing Sugar Based on Gold Nanoparticles via Click-reaction

A simple,rapid,and high-sensitive method for the detection of reducing sugar was established based on the click-reaction with gold nanoparticles( AuNP) as the chromogenic signal component. The quantitative detection of reducing sugar was accomplished by building two different kinds of functionalized AuNPs. The two AuNPs were got from a two-step reaction which were first modified with mercaptopropionic acid,and then fixed with alkynyl or azide group via amidation reaction,respectively. Meanwhile,the effects of reaction temperature and time on the efficiency of click-reaction have been examined. The results showed good linear correlation between the absorbance ratio A650 /520and the concentration of reducing sugar reacted at70 ℃ for 10 min,with a detection limit of the method was 0. 0015 μmol / L. This method can be directly applied for the analysis of honey samples with the recoveries of 98. 1%-103. 6%.

Multi-element determination in Brazilian honey samples by inductively coupled plasma mass spectrometry and estimation of geographic origin with data mining techniques

Multi-element analysis of honey samples was carried out with the aim of developing a reliable method of tracing the origin of honey. Forty-two chemical elements were determined (Al, Cu, Pb, Zn, Mn, Cd, Tl, Co, Ni, Rb, Ba, Be, Bi, U, V, Fe, Pt, Pd, Te, Hf, Mo, Sn, Sb, P, La, Mg, I, Sm, Tb, Dy, Sd, Th, Pr, Nd, Tm, Yb, Lu, Gd, Ho, Er, Ce, Cr) by inductively coupled plasma mass spectrometry (ICP-MS). Then, three machine learning tools for classification and two for attribute selection were applied in order to prove that it is possible to use data mining tools to find the region where honey originated. Our results clearly demonstrate the potential of Support Vector Machine (SVM), Multilayer Perceptron (MLP) and Random Forest (RF) chemometric tools for honey origin identification. Moreover, the selection tools allowed a reduction from 42 trace element concentrations to only 5.

Determination of a liquid chromatography–tandem mass spectrometry method for the determination of sulfonamides, trimethoprim and dapsone in honey and validation according to Commission Decision 2002/657/EC for banned compounds

This work reports a sensitive liquid chromatography–tandem mass spectrometry (LC–MS/MS) method for identification and quantification of seven sulfonamides, trimethoprim and dapsone in honey. The method is based on a solid-phase extraction (SPE) step of the target analytes with Oasis HLB cartridges after acidic hydrolysis of the honey sample to liberate the sugar-bound sulfonamides. Analysis was performed using liquid chromatography–tandem mass spectrometry (LC–MS/MS) in the positive electro-spray ionization (ESI) mode with two different isotopically labeled internal standards with the view to improve the quantitative performance of the method. The method validation has been performed according to the Commission Decision 2002/657/EC; the average recoveries, measured at three concentration levels (1.5, 2.5 and 5.0μgkg−1), have been estimated in the range 70 to 106% while the respective % relative standard deviations of the within-laboratory reproducibility ranged from 6 to 18%. Mean values of the expanded uncertainties calculated were in the range 22–41% at the 99% confidence level. Decision limit (CCα) and detection capability (CCβ) values were in the ranges 0.4–0.9 and 0.7–1.4μgkg−1, respectively. Matrix effects have been investigated demonstrating a moderate signal suppression/enhancement for most of the target compounds. The method described has been successfully applied to the analysis of honey samples; sulfamethoxazole, sulfathiazole and trimethoprim were detected in some cases.

Analysis of Inorganic Cations in Honey by Capillary Zone Electrophoresis with Indirect UV Detection

An indirect UV detection method based on capillary electrophoresis was developed to separate eleven metal cations completely, including alkali, alkaline earth and transition metal, which are related to evaluate the quality of honey. The background electrolyte contains 15 mmol/L chromophore imidazole, and acetic acid (pH = 3.7), which functioned as pH adjustor and complexing reagent. The selected cations can be completely separated within 8 min under hydrodynamic mode injection with a running voltage of 20 kV at 25°C. Limit of detection, linearity, reproducibility relative standard deviation of migration time and recoveries are in the range of 0.01-0.21 mg/L, 0.06-60.0 mg/L, 2.1-3.4% and 95.4-104.1%, respectively. The applicability of the method is shown by the analysis of honey samples, including a comparison with results of pretreatment and unpretreatment of eight samples. The results demonstrate that the developed method can conveniently be used in routine analysis of honey.

Development of a fast capillary electrophoresis method for determination of carbohydrates in honey samples

In this study, the determination of fructose, glucose and sucrose by capillary electrophoresis (CE) was investigated. The tendency of the analyte to undergo electromigration dispersion and the buffer capacity were evaluated using the Peakmaster® software and considered in the optimization of the background electrolyte, which was composed of 20mmolL−1 sorbic acid, 0.2mmolL−1 CTAB and 40mmolL−1 NaOH at pH 12.2. Under optimal CE conditions, the separation of the substances investigated was achieved in less than 2min. The detection limits for the three analytes were in the range of 0.022 and 0.029gL−1 and precision measurements within 0.62–4.69% were achieved. The proposed methodology was applied in the quantitative analysis by direct injection of in honey samples to determine the main sugars presents. The samples were previously dissolved in deionized water and filtered with no other sample treatment. The mean values for fructose, glucose and sucrose were in the ranges of 33.65–45.46g 100g−1, 24.63–35.06g 100g−1 and <0.22–1.32g 100g−1, respectively. The good analytical performance of the method makes it suitable for implementation in food laboratories for the routine analysis of honey samples.

Environmental and health risk assessments of genetically modified eucalypts in Brazil

Motivated by the Brazilian Ministry of Agriculture, Farming and Supply (MAPA), we created in 2009 the “Collaborating Center in Agriculture Defense Relative to the Biosafety of Genetically Modified Eucalypts” (Project “CDA Eucalyptus”) in order to collect information and conduct research to assess the biosafety of GM eucalypts in the Brazilian context. The Normative Resolution Nr. 5 of the National Biosafety Technical Commission (CTNBio) is the official document presenting all information needed to propose the commercial release of GMOs in Brazil. Based on this document and along with the personnel of the Suzano Paper & Cellulose Co., we conducted a series of experiments with GM and non-GM eucalypts planted in a test field in the state of Sao Paulo to start collecting the necessary information. Two independent groups of transgenic plants, harboring two different transgene constructions along with non-GM control plants are being assayed. The genetic traits, the identity or names of the transgenes as well as the identity of each tree individual will not be revealed due to intellectual property request still pending. Each group of plants was represented by four independent events in triplicates (2 groups x 4 events x 3 clonal trees + 3 non-GM clonal trees), therefore totaling 27 individuals under analysis. Samples were identified by random numbers and all assays were conducted in a simple-blind or a double-blind fashion. Tests concluded until now included (i) the detection of transgene regulatory sequences in purified DNA samples by conventional PCR and RT-qPCR, confirming the expected sampling conducted; (ii) extraction, chemical characterization and analysis of the antifungal effects of essential (volatile) oils extracted from leaves; (iii) pollen germination in vitro; (iv) flower morphology; (v) seed production; (vi) initial seedling development; (vii) leaf allelopathy; (viii) measurements of total phenolic compounds in leaves and roots; and (ix) effects of leaf extracts on the viability of human colon cells. All results obtained from experiments (ii) to (ix) revealed no statistical differences between GM- and non-GM-derived samples. A second round of experiments will be conducted to confirm these results. Proteomic and transcriptomic profiling of GM and non-GM trees are under analysis, as well as a series of experiments that include the chemical, nutritional and biological analysis of honey samples derived from bee hives located in fields of GM versus non-GM plants; and bee (Apis mellifera) population dynamics.

Liquid Chromatographic Determination of Resveratrol and Piceid Isomers in Honey

In this work, a liquid chromatography method with diode array and fluorescence detection and electrospray ionization mass spectrometry (LC-DAD-FLD and LC-ESI-MS) has been developed for the determination of residues of resveratrol in all its forms (free isomers and glycosylates) in honey. This procedure involves a solid-phase extraction on polymeric cartridges for the isolation of trans/cis-isomers of resveratrol and piceid from diluted honey samples. Chromatographic separation of the analytes was performed in isocratic mode on a C18 column (150 mm × 4.6 mm i.d., 5 μm) operated at 30 °C. The mobile phase consisted of a mixture of water with 1% formic acid and acetonitrile (75/25, v/v), and the flow rate was set at 1.0 mL/min. Average analyte recoveries were from 71% to 113% in replica sets of fortified honey samples. The detection limits when using LC-DAD-FLD were between 40 and 120 μg/kg, meanwhile for LC-ESI-MS were between 1.4 and 14.6 μg/kg. The proposed method was applied to the analysis of honey samples collected from treated beehives in experimental apiaries after a preliminary field trial, and they were not found any residues over the detection limits of the studied compounds.

Espectro polínico de mel de tiúba (Melipona fasciculata Smith, 1854, Hymenoptera, Apidae)

O espectro polínico do mel de Melipona fasciculata Smith foi analisado com o objetivo de identificar os recursos nectaríferos utilizados por essa espécie. A identificação das plantas visitadas foi realizada com base na análise dos tipos polínicos encontrados em 12 amostras de mel coletadas, mensalmente, em uma colônia localizada no município de Palmeirândia, na área da Baixada Ocidental Maranhense (02º40'47,6S, 44º52'39,8"W), Brasil. As análises quantitativas e qualitativas foram realizadas com o objetivo de determinar as porcentagens e classes de frequência dos tipos polínicos presentes nas amostras de mel. Foram encontrados 45 tipos polínicos, sendo Pontederia parviflora Alexander (Pontederiaceae), espécie mais frequente em todo o período de amostragem (38,6%), pólen dominante em Outubro (86%), Junho (85%), Julho (76%), Agosto (49%) e Setembro (51%) e pólen acessório em Dezembro, Janeiro e Março. Mimosa caesalpiniifolia Benth (Mimosaceae) foi a segunda espécie mais frequente (22,8%) sendo pólen dominante em Novembro (46%), Abril (74%) e Maio (72%). Myrcia eximia DC (Myrtaceae) foi considerada pólen isolado importante. As famílias mais representativas no espectro polínico das amostras de mel foram Pontederiaceae e Mimosaceae. 50% dos méis foram biflorais, havendo também méis monoflorais (41,7%) e heteroflorais (8,3%).

Caracterização físico-química de méis de Apis mellifera L. da região noroeste do Estado do Rio Grande do Sul

O objetivo deste trabalho foi determinar a composição físico-química de méis de Apis mellifera L. produzidos em dois anos consecutivos na região noroeste do Estado do Rio Grande do Sul, Brasil. As características físico-químicas de 36 amostras de mel foram comparadas utilizando o teste T de Student e a adequação aos padrões da legislação brasileira da qualidade do mel foi verificada. Os resultados das análises dos méis variaram para as características analisadas conforme segue: pH (3,3-4,4), umidade (14,7-19,8%), acidez total (16,9-49,2meq kg-1), hidroximetilfurfural (0,15-48,3mg kg-1), açúcares redutores (60,1-75,9%), açúcares não-redutores (1,35-5,99%), cinzas (0,05-0,47%) e sólidos insolúveis (0,016-0,27g kg-1). A análise estatística das amostras de mel produzidas em dois anos consecutivos mostrou que houve diferença significativa na umidade, na acidez e na hidroximetilfurfural. Os méis produzidos nesta região apresentam boa qualidade e características físico-químicas compatíveis aos padrões da legislação brasileira.

Distribution of Paenibacillus larvae spores inside honey bee colonies and its relevance for diagnosis

One of the most important factors affecting the development of honey bee colonies is infectious diseases such as American foulbrood (AFB) caused by the spore forming Gram-positive bacterium Paenibacillus larvae. Colony inspections for AFB clinical symptoms are time consuming. Moreover, diseased cells in the early stages of the infection may easily be overlooked. In this study, we investigated whether it is possible to determine the sanitary status of a colony based on analyses of different materials collected from the hive. We analysed 237 bee samples and 67 honey samples originating from 71 colonies situated in 13 apiaries with clinical AFB occurrences. We tested whether a difference in spore load among bees inside the whole hive exists and which sample material related to its location inside the hive was the most appropriate for an early AFB diagnosis based on the culture method. Results indicated that diagnostics based on analysis of honey samples and bees collected at the hive entrance are of limited value as only 86% and 83%, respectively, of samples from AFB-symptomatic colonies were positive. Analysis of bee samples collected from the brood nest, honey chamber, and edge frame allowed the detection of all colonies showing AFB clinical symptoms. Microbiological analysis showed that more than one quarter of samples collected from colonies without AFB clinical symptoms were positive for P. larvae. Based on these results, we recommend investigating colonies by testing bee samples from the brood nest, edge frame or honey chamber for P. larvae spores.

Pollen analysis of honey samples from 13 local government areas of Ebonyi State, Nigeria

Pollen analysis of honey samples from 13 local government areas of Ebonyi State, Nigeria

Espectro polínico de amostras de mel de &lt;em&gt;Melipona mandacaia&lt;/em&gt; Smith, 1863 (Hymenoptera: Apidae)

The pollen spectrum from honey samples of Melipona mandacaia stingless bee was analyzed aiming at elucidating the alimentary resources used by that species. The identification of the visited plants was based on the analysis of pollen from honey samples collected in 11 hives located in São Gabriel county, in the semiarid area of Bahia State, Brazil (11º14’S and 41º52’W). The quantitative and qualitative analyses of honey samples were conducted in order to determine the pollen types percentages and frequency classes. Twenty-six pollen types were found, being the Piptadenia rigida type (Mimosaceae) considered dominant. Ricinus communis (Euphorbiaceae), Mimosa verrucata (Mimosaceae) and M. arenosa (Mimosaceae) were considered important isolated pollen. The most representative families found in the pollen spectrum of the honey samples were Mimosaceae, Euphorbiaceae, Asteraceae and Anacardiaceae

The analysis of honey samples for residues of nitrobenzene and petroleum from the possible use of Frow mixture in hives

A headspace gas chromatography–mass spectrometry method has been established for the analysis of honey samples for nitrobenzene and petroleum residues. These substances may be used as components of ‘Frow mixture’ applied to treat hives for the control of Acarine (infestation by parasitic mites) in honey bees. The method had a detection limit of 2 μg/kg for nitrobenzene and 0.5 μg/kg (or better) for four indicator substances of petroleum—toluene, o-xylene, ethylbenzene and naphthalene. The method was applied in a small survey of 49 retail honey samples. No sample contained detectable nitrobenzene or petroleum residues defined as the presence of all four indicator hydrocarbons. Two honey samples contained low levels of toluene (19 and 62 μg/kg) and one of these two samples also contained o-xylene (2 μg/kg). The origin of these very low levels was not investigated. These analytical findings indicate that, for honey samples entering the UK market, either the use of Frow mixture to fumigate bee hives is not commonly practiced or that chemical residues from the treatment are not persistent.

PIXE and XRF analysis of honey samples

The systematic determination of trace-element concentrations in honey samples was done by the PIXE method using a 2 MeV proton beam and by the total reflection XRF method. The different kinds of honey samples were collected in the period of spring–summer in three places of Poland: in the centre of Warsaw (a highly polluted region) and about 100 km east of Warsaw and 70 km southwest of Warsaw (as regions free from industrial and transport pollution). The measured samples have shown that the concentrations of trace elements are similar in the honey samples from these places.

Detection of honey adulteration with beet sugar using stable isotope methodology

A usual aspect of our work involves the analysis of honey samples for later sale, following current Spanish legislation. Such analyses essentially consist of studying pollen sediments, and sensory and physicochemical analyses. With this background, it seemed appropriate to investigate possible adulterations due to the addition of sugar (beet and cane). To do this, we selected 49 samples of honey obtained from 14 floral types and used them for pollinic and sensory analyses and to detect possible adulterations due to the addition of beet sugar products (treating the oligosaccharide fraction contained in the honey with the galactose oxidase reaction) or due to corn syrup addition (with normal δ 13C stable carbon isotope ratios). After classifying the samples according to the results of the pollen and sensory analyses, further assays were conducted. From the results it was concluded that 15% of the samples had been adulterated with beet sugar and 4% with cane sugar. The implementation of many analyses for each sample means that the results can be intercorrelated very well.