Identification of adulterants added to beeswax: Estimation of detectable minimum percentages

Jiménez, Juan J.; Bernal, José; Nozal, Marı́a J.; Martín, Margarita; Toribio, Laura

doi:10.1002/ejlt.200800263

Cited by 17 publications

(23 citation statements)

References 15 publications

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“…This method was used for the first time for the analysis of beeswax hydrocarbons by White et al (1960) and Downing et al (1961). Gas chromatography with different kinds of detection (FID, MS) is now commonly used in studies of beeswax composition (Aichholz and Lorbeer, 1996, 1999, 2000Jimenez et al, 2003Jimenez et al, , 2004Jimenez et al, , 2006Jimenez et al, , 2007Jimenez et al, , 2009Serra Bonvehi and Ornantes Bermejo, 2012;Maia and Nunes, 2013), and the majority of compounds belonging to certain homologous series have been characterized. However, some beeswax constituents remain unknown despite the use of the most recent chromatography techniques.…”

Section: Introductionmentioning

confidence: 99%

Determination of Beeswax Hydrocarbons by Gas Chromatography with a Mass Detector (GC -MS ) Technique

Waś

Szczesna

Rybak-Chmielewska

2014

Journal of Apicultural Science

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a b s t r a c t here we describe a method of hydrocarbon (alkanes, alkenes, dienes) identification and quantitative determination of linear saturated hydrocarbons (n-alkanes) in beeswax using gas chromatography with a mass detector technique (gc-ms). beeswax hydrocarbons were isolated using a solid-phase extraction (spe) technique with neutral aluminum oxide (alumina -n, 1000 mg, 6 mL), then were separated on a non-polar gas chromatography column Zb-5ht inferno (20 m×0.18 mm×0.18 µm). qquantitative analysis of n-alkanes was conducted by the method of internal standard with squalane used as the internal standard. the basic parameters of validation (linearity and working range, limit of determination, repeatability and reproducibility, recovery) were determined. for all of the identified compounds, satisfactory (≥0.997) coefficients of correlation in the working ranges of the method (from 0.005 to 5.0 g/100 g) were obtained. the elaborated method was characterized by satisfactory repeatability and within-laboratory reproducibility. the average coefficients of variation for the total n-alkanes did not exceed 2% under conditions of repeatability or 4% under conditions of reproducibility. the recovery for individual n-alkanes was above 94%; for their total content, it was 100.5%. in beeswax originating from apis mellifera, n-alkanes containing from 20 to 35 carbon atoms in their molecules were determined. the total content of these alkanes was between 9.08 g and 10.86 g/100 g (on average, 9.81 g/100 g). additionally, apart from the saturated hydrocarbons, unsaturated hydrocarbons and dienes were identified.

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Section: Introductionmentioning

confidence: 99%

Determination of Beeswax Hydrocarbons by Gas Chromatography with a Mass Detector (GC -MS ) Technique

Waś

Szczesna

Rybak-Chmielewska

2014

Journal of Apicultural Science

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“…paraffin) added to beeswax, than the methods based on the determination of physicochemical parameters (White & Kushmir, 1961;Tulloch & Hoffman, 1972;Tulloch, 1973;Serra Bonvehi, Cañas Lloria, & Gomez Pajuelo, 1989;Serra Bonvehi, 1990;Vit et al, 1992;Poncini, Poncini, & Prakash, 1993;Bernal et al, 2005;Serra Bonvehi & Ornantes Bermejo, 2012; or the gravimetric analysis method (DGF-M-V-6, 1957; PN-R-78890, 1996). The amount of paraffin detected also depends, to a great extent, on the kind of paraffin added to beeswax (Jimenez et al, 2009;Serra Bonvehi & Ornantes Bermejo, 2012). As it has been previously stated, the indicators of beeswax adulteration with hydrocarbons of an alien origin (e.g.…”

Section: Introductionmentioning

confidence: 84%

“…It is paraffin, though, that is the product most frequently used for beeswax adulteration. Due to having a similar composition and similar physico-chemical properties, the addition of paraffin to beeswax, especially when added in small amounts, is difficult to detect (Bogdanov, 2009;Jimenez et al, 2009;Serra Bonvehi & Ornantes Bermejo, 2012;Maia, Barros, & Nunes, 2013;Svečnjak et al, 2015). The chemical composition of paraffin has not yet been sufficiently analysed.…”

Section: Introductionmentioning

confidence: 99%

“…The paraffin properties and compositions may differ depending on the intended purpose of the Detection of paraffin in beeswax by GC-MŚ paraffin (Szpyrka, 1999). The chromatographic techniques applied for the evaluation of beeswax quality (Tulloch & Hoffman, 1972;Tulloch, 1973;Serra Bonvehi, 1988;Jimenez et al, 2003Jimenez et al, , 2004Jimenez et al, , 2006Jimenez et al, , 2007Jimenez et al, , 2009Serra Bonvehi & Ornantes Bermejo, 2012;Waś, Szczęsna, & Rybak-Chmielewska, 2014a are more efficient. These techniques allow for the detection of smaller amounts of adulterant (e.g.…”

Section: Introductionmentioning

confidence: 99%

“…The addition of paraffin results in an increase in the hydrocarbon content. At the same time, the addition of paraffin dilutes the beeswax and results in a lower content of: the esters of palmitic acid (palmitates), hydroxymonoesters, some fatty acids, and alcohols (Jimenez et al, 2006(Jimenez et al, , 2007(Jimenez et al, , 2009Serra Bonvehi & Ornantes Bermejo, 2012). In the current work, we continue our investigations into the detection of beeswax adulterated with paraffin (Waś, Szczęsna, & RybakChmielewska, 2015).…”

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Efficiency of GC-MS method in detection of beeswax adulterated with paraffin

Waś

Szczesna

Rybak-Chmielewska

2016

Journal of Apicultural Science

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A b s t r a c tThe efficiency of the gas chromatography -mass detector (GC-MS) technique for the detection of beeswax adulterated with paraffin, was evaluated. For this purpose, beeswax samples with paraffin additions (3, 5, 10, 30, 50%) were analysed. Since not enough is known about paraffin compositions, and since it is difficult to detect paraffin in beeswax, the aim of our research was also to compare the hydrocarbon composition of different types of paraffin. The analysis showed that the types of paraffin available on the market, differ qualitatively and quantitatively as far as their hydrocarbon compositions are concerned. In all kinds of paraffin, we found homologous series of n-alkanes that were much longer than those in beeswax. In beeswax, the amount of added paraffin that is possible to detect, differs and depends on the kind of paraffin used for adulteration. In this study, the minimum estimated percent that was detected using the GC-MS technique, was 3%. The adulteration is indicated by the presence of hydrocarbons containing over 35 carbon atoms in the molecule, and by the higher contents of n-alkanes (C 20 H 42 -C 35 H 72 ), in comparison to the concentration of these compounds determined in pure beeswax. We also presented the results of the quality control of commercial beeswax. Based on our results, it can be stated that beeswax adulteration is currently a problem. Keywords: adulteration, beeswax, detection, efficiency, GC-MS, paraffinResearch Institute of Horticulture, Apiculture Division in Puławy, Kazimierska 2, 24-100 Puławy, Poland INTRODUCTIONThe recent increased interest in the testing of beeswax composition and in the quality assessment of beeswax, is related to the numerous cases of beeswax adulteration. Substances such as ceresin, stearin, natural plant waxes (e.g. Candelilla wax, Carnauba wax), animal waxes and fats (e.g. lanolin, tallow), and mineral waxes (Montan, ozocerite) have been added to beeswax. It is paraffin, though, that is the product most frequently used for beeswax adulteration. Due to having a similar composition and similar physico-chemical properties, the addition of paraffin to beeswax, especially when added in small amounts, is difficult to detect (Bogdanov, 2009;Jimenez et al., 2009;Serra Bonvehi & Ornantes Bermejo, 2012;Maia, Barros, & Nunes, 2013;Svečnjak et al., 2015). The chemical composition of paraffin has not yet been sufficiently analysed. The information found in literature mostly concerned physicochemical properties (Bernal et al., 2005) or concerned the estimated data on the paraffin composition stated by the producers. From these data, it follows that the group of longstraight-chained saturated hydrocarbons (nalkanes) dominate in paraffin. The content of these hydrocarbons is estimated to be at different levels, and even at levels of up to 90%. Depending on the kind of paraffin (in particular the melting point of paraffin), and the purification level of the obtained product, the paraffin can also contain other hydrocarbons (e.g. branched, cyclic, unsa...

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Identification and Quantification of Single and Multi‐Adulteration of Beeswax by FTIR‐ATR Spectroscopy

Tanner

Lichtenberg-Kraag

2019

Euro J Lipid Sci & Tech

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Marketing of adulterated beeswax foundation has recently become a major economic problem for beekeepers. Paraffin contamination leads to collapse of combs, and stearic acid has a negative influence on the development of bee brood. The quality of beeswax for beekeeping has not been standardized in EU regulations. Recently, it was shown that attenuated total reflectance Fourier-transform infrared spectroscopy (FTIR-ATR) can be used to determine beeswax adulteration. Differences in the IR spectra of authentic beeswax can be identified and calculated through comparison with authentic beeswax. In this study, the method is further validated by employing a high number of samples of authentic beeswax from different origins. Low quantification and detection limits are achieved for paraffin, stearic acid, tallow, carnauba wax, and candelilla wax. Furthermore, the FTIR-ATR analytical conditions are verified by analyzing 358 samples of commercial and beekeeper-produced beeswax foundations. Multi-adulterated samples with as many as five different additives in beeswax mixtures are identified with the same accuracy as single substances. Additionally, the spectra of a further 14 different natural and synthetic waxes and hardened fats are analyzed and are compared with beeswax. Finally, a spectral library is established that can be used for further studies. Practical Applications: FTIR-ATR is a fast and cost-efficient tool in beeswax analysis for accurately monitoring a high sample volume. Analysis of 358 beeswax foundations showed an adulteration of 21.8% of the samples with paraffin, stearic acid, tallow, and combinations. Based on the results of this study, it is possible to detect beeswax adulteration of less than 3% of these adulterants and their combinations by FTIR-ATR spectroscopy. This method can be used for monitoring beeswax foundations to identify adulterated materials, exclude these materials from the recycling process, and produce high-quality beeswax, which is essential for bee health.

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Identification of adulterants added to beeswax: Estimation of detectable minimum percentages

Cited by 17 publications

References 15 publications

Determination of Beeswax Hydrocarbons by Gas Chromatography with a Mass Detector (GC -MS ) Technique

Determination of Beeswax Hydrocarbons by Gas Chromatography with a Mass Detector (GC -MS ) Technique

Efficiency of GC-MS method in detection of beeswax adulterated with paraffin

Identification and Quantification of Single and Multi‐Adulteration of Beeswax by FTIR‐ATR Spectroscopy

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