PubMed · 14403771
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B HUEBNER. 1959-12-20. [Further experiences with nektar-mil].. https://pubmed.ncbi.nlm.nih.gov/14403771/
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An analytical method for the routine simultaneous determination of four nicotinoid insecticides (acetamiprid, imidacloprid, thiacloprid and thiamethoxam) in commercial multifloral honey was developed. Fortified honey samples, dissolved in water, were cleaned up through Extrelut NT20 column and, finally, insecticides were eluted with dichloromethane. The eluate was evaporated, the residue redissolved in methanol and then analyzed by LC-ESI(+)-MS. Average recoveries of the four analytes were in the range of 76% and 99% at both spiking levels 0.1 and 1.0 mg kg(-1). Relative standard deviations (RSDs) were less than 10% for all of the recovery tests. The detection limits (LODs) of the method ranged from 0.01 to 0.1 mg kg(-1) for the different insecticides studied. The developed method is linear over the range assayed, 0.5-5.0 microg mL(-1), with linear correlation coefficients higher than 0.9993.
A total of 73 different honeys from seven botanical origins [ling (Calluna vulgaris L.), heather (Erica sp.), rosemary (Rosmarinus officinalis L.), thyme (Thymus vulgaris L.), honeydew (Quercus sp.), spike lavender (Lavandula latifolia M.) and french lavender (Lavandula stoechas L.)] have been classified by applying discriminant analysis to their metal content data and other common physicochemical parameters. Fifteen minerals were identified and quantified using atomic emission spectroscopy (AES) for K and Na, and inductively coupled plasma atomic emission spectrometry (ICP-AES) for Mg, Ca, Al, Fe, Mn, Zn, B, Cu, Co, Cr, Ni, Cd and Pb. Moreover, eight physicochemical parameters were analysed following the Harmonised Methods of the International Honey Commision: ash content, moisture, insoluble matter, reducing sugars, apparent sucrose, diastase activity, free acidity and hydroxymethylfurfural. The honeys analysed were characterised and distinguished using chemometrics. ANOVA highlighted significant differences between the honeys in terms of the mean contents of all variables except apparent sucrose, HMF, Fe and Zn. Principal component analysis was used as a descriptive tool to visualise the data structure in two dimensions, finding relationships between variables and types of honey. Likewise, discriminant analysis, together with various methods (stepwise, forward and backward), was used to select the variables with the highest discriminating power, which allowed us to classify all of the botanical origins considered in this work, achieving a global success rate close to 90% following cross-validation.
Twenty-four Spanish thyme honey samples were analyzed using inductively coupled plasma optical emission spectrometry (ICP-OES). Twenty-four minerals were quantified for each honey. The elements Al, As, Ba, Ca, Cr, Cu, Fe, K, Li, Mg, Mn, Na, P, Pb, S, Se, Si, Sr, and Zn were detected in all samples; seven elements are very abundant (Ca, K, Mg, Na, P, S, and Si), and six are not abundant (Al, Cu, Fe, Li, Mn, and Zn). Eleven of them are trace elements (As, Ba, Cd, Co, Cr, Ni, Mo, Pb, Se, Sr, and V) at <1 mg kg(-)(1). Classification of thyme honeys according to their origin (coast, mountains) was achieved by pattern recognition techniques on the mineral data. By means of principal component analysis, a good separation by geographical origin is obtained when scores for the two first principal components are plotted. Classification functions of 11 metals (Al, As, Cr, Cu, K, Li, Mg, Na, P, S, and V) were obtained using stepwise discriminant analysis and applied to classify correctly approximately 100% of the honey samples.