Determination of amitraz and 2,4‐dimethylaniline residues in honey by using LC with UV detection and MS/MS

Xu, Jinzhong; Jian-jun, Miao; Lin, Hong Ping; Ding, Tao; Zhao, Zhen-Yun; Wu, Bin; Shen, Chongyu; Jiang, Yuan

doi:10.1002/jssc.200900437

Cited by 23 publications

(11 citation statements)

References 55 publications

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“…However, amitraz is the one of the most difficult compounds to analyse because of its instability; moreover, it is easily degraded to metabolites such as 2,4-dimethylaniline (DMA), 2,4-dimethylformamidine (DMF) and N-2,4-dimethylphenyl-N-methylformamidine (DMPF) (Bernal et al 1997;Pierpoint et al 1997;Hepperle et al 2015). Therefore, amitraz extraction procedures should be carefully performed under basic conditions (Xu et al 2009;Tomasini et al 2012). Under restrictions in Japan, the MRL of amitraz is set as the sum of amitraz itself and 1.81 times the amount of DMPF (The Japan Food Chemical Research Foundation.…”

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confidence: 99%

Determination and surveillance of nine acaricides and one metabolite in honey by liquid chromatography-tandem mass spectrometry

Nakajima

Tsuruoka

Kanda

et al. 2015

Food Additives & Contaminants: Part A

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A simple and accurate analytical method for the determination of acaricides in honey was developed and validated in accordance with Japanese validation guidelines. Analytes - amitraz, N-2,4-dimethylphenyl-N-methylformamidine (DMPF), etoxazole, fenpyroximate, fipronil, hexythiazox, propargite, pyridaben and spirodiclofen - were extracted with ethyl acetate under basic conditions and subsequently cleaned up using an InertSep(®) MA-1 polymer-based anion-exchange column. The method was validated by fortified recovery tests at three different concentrations (1, 5 and 10 µg kg(-1)) performed with three samples daily on five different days. The method exhibited recoveries of 77-116% and precision (relative standard deviations - RSDs) of repeatability and within-laboratory reproducibility ranged from 2% to 22% and from 3% to 23%, respectively. The sample solution was successfully cleaned up to enable quantification using external solvent calibration curves. The limits of quantification (LOQs) were estimated to be 1 µg kg(-1) for all analytes. The method was applied to honey samples commercially available in Tokyo, Japan. Analysis of 250 honey samples indicated that amitraz was present in 127 samples, and that its residual concentration was less than 20 µg kg(-1). Propargite was detected in 23 samples at concentrations less than 1 µg kg(-1).

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confidence: 99%

Determination and surveillance of nine acaricides and one metabolite in honey by liquid chromatography-tandem mass spectrometry

Nakajima

Tsuruoka

Kanda

et al. 2015

Food Additives & Contaminants: Part A

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“…Specifically, amitraz stock standard was prepared by dissolving in acetonitrile because amitraz is more stable 5 in this solvent (Corta et al, 1999, Xu, et al, 2009). All the solutions were stored at -20º C in order to improve their stability (Tokmana, et.…”

Section: Standards and Reagentsmentioning

confidence: 99%

Mixture-risk-assessment of pesticide residues in retail polyfloral honey

2016

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The presence of even tiny quantities of pesticide residues in honey, a traditional healthy product, is a matter of concern for producers, packers and consumers. This paper aims to quantify pesticides in retail brands of polyfloral honey, and to calculate the mixture risk assessment of honey for consumers according to the results obtained from the analyzed samples. A LC-MS/MS multi-residue method was developed and validated for 13 compounds: 11 pesticides (chlorfenvinphos, coumaphos, tau-fluvalinate, amitraz, which are very common in veterinary treatments, and imidacloprid, acetamiprid, simazine, cyproconazole, tebuconazole, chlorpiryphos-methyl, chlorpiryphos, widely used in agricultural practices), and 2 metabolites of amitraz (2,. Results showed that the samples contained pesticide residues at different concentrations; however, the MRL in honey for each of the 11 pesticides was never exceeded. The most common were amitraz (from 1 to 50 µg/kg) present in 100% of the samples, and coumaphos (up to 14 µg/kg) in 63%. The hazard index (HI) for adults was less than 0.002 in all cases, a long way from 1, the value established as the limit of acceptability.Therefore, commercial honey does not represent any significant risk to health. However, considering that residue levels should be present "as low as reasonably achievable" it is deemed necessary to make an effort to reduce their presence by appropriate agricultural and, above all, beekeeping practices due to acaridae treatments.Keywords: Honey; pesticides; Mixture-risk-assessment; MRL; hazard index 2 IntroductionHoney is a highly valued natural product due to its nutritional properties and appreciated therapeutic applications. However, recently, food alerts caused by the detection of antibiotics, pesticides or heavy metals in honey have jeopardized its healthy image (JuanBorrás et al., 2015). Pesticide residues in honey come from environmental pollution and veterinary practices (Totti et al., 2006;Calatayud-Vernich et al., 2016 , 2016). However, this is the first attempt to apply this approach to retail honey.Therefore, the objective of this paper was to quantify the presence of different pesticides (usually found in the routine control analyses of honey samples) in polyfloral labeled brands, and to estimate the mixture risk assessment of the honey for consumers (due to exposure to pesticides) based on the results obtained from the analyzed samples. As a first step, the analytical procedure was validated in order to guarantee the quality of the results obtained. Material and Methods Honey samplesThis study was carried out with supermarket own-brands and well-known brand honey, which represent almost all of the retail sales in the Spanish market. A total of 22 honey samples, labelled as polyfloral were purchased across Spain from different retail outlets.Samples were purchased with as recent a packing date as possible, based on the label information, and were kept frozen until analysis to minimize losses of target compounds.A mixture of 5 polyfloral honeys w...

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“…Water-soluble products are mainly identified in the honey, while fat-soluble products have a higher affinity for the beeswax. Most of the synthetic acaricides are lipophilic and therefore accumulate in beeswax,whereasresiduesinhoneyarerelativelylow (Karazafiris et al 2008;Xu et al 2009;Valdovinos-Flores et al 2016). These chemicals can also resist the waxmeltingtemperature;therefore,someofthemcan accumulate for years as it is a common beekeeping practice to recycle wax almost continuously in the form of the foundations on which bees construct a complete comb (Ravoet et al 2015).…”

Section: Introductionmentioning

confidence: 99%

Coumaphos residues in honey, bee brood, and beeswax after Varroa treatment

et al. 2017

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Residues of acaricide coumaphos were assessed in honey, bee brood, and beeswax during a 2-year field experiment. Honey, bee brood, and beeswax samples were collected before and after routine use of coumaphos in the treatment of bee colonies against varroosis in two consecutive years. Determination of coumaphos in honey and bee brood was based on RP-HPLC with UV detection after a liquid-liquid extraction with hexane or ethyl acetate. Coumaphos in beeswax was identified and quantified by GC/MS. Results indicate the undetectable presence of coumaphos in honey. In bee brood, coumaphos was observed after the treatment. In beeswax, the accumulation of coumaphos was determined not only in hives where it was used but also in hives nearby in which coumaphos was not used. Results indicate the accumulation of coumaphos in bee brood and beeswax. Due to the coumaphos accumulation this drug should be used only in strongly affected bee colonies.

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Determination of amitraz and 2,4‐dimethylaniline residues in honey by using LC with UV detection and MS/MS

Cited by 23 publications

References 55 publications

Determination and surveillance of nine acaricides and one metabolite in honey by liquid chromatography-tandem mass spectrometry

Determination and surveillance of nine acaricides and one metabolite in honey by liquid chromatography-tandem mass spectrometry

Mixture-risk-assessment of pesticide residues in retail polyfloral honey

Coumaphos residues in honey, bee brood, and beeswax after Varroa treatment

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