title: Feasibility of ultra-trace determination of bromine and iodine in honey by ICP-MS using high sample mass in microwave-induced combustion.
abstract: This work demonstrates the feasibility of ultra-trace determination of halogens in biological samples by inductively coupled plasma mass spectrometry (ICP-MS) after decomposition by microwave-induced combustion (MIC). The conventional MIC method was improved to allow the combustion of samples with mass higher than that used in previous works in order to achieve better limits of detection (LODs). The applicability of the proposed method for ultra-trace determination of bromine and iodine in organic samples was demonstrated here using honey. It was possible to decompose up to 1000 mg of honey using microcrystalline cellulose as a combustion aid and polyethylene film for sample wrapping. After combustion, analytes were absorbed using 50 mmol L(-1) NH4OH and recoveries for Br and I were between 99 and 104 %, and relative standard deviations were lower than 5 %. Microwave-assisted alkaline dissolution (MA-AD) was also evaluated for honey sample preparation using NH4OH or tetramethylammonium hydroxide solutions. However, the LODs for the MA-AD method were unsuitable because the high carbon content in digests required a dilution step prior to the analysis by ICP-MS. The LODs obtained by MIC were improved from 1143 to 34 ng g(-1) for Br and from 571 to 6.0 ng g(-1) for I, when compared to the MA-AD method. Furthermore, it was possible to decompose up to eight samples simultaneously in 30 min (including the cooling step) with very low reagent consumption and consequently lower generation of effluents, making MIC method well suited for routine ultra-trace determination of Br and I in honey. Graphical Abstract A high mass of honey was efficiently digested by MIC for subsequent Br and I determination by ICP-MS.
authors: Centro de Ciências Químicas, Farmacêuticas e de Alimentos, Universidade Federal de Pelotas, 96010-610, Pelotas, RS, Brazil.
authors: Vanize C
authors: VC
authors: Costa
authors: Departamento de Química, Universidade Federal de Santa Maria, 97105-900, Santa Maria, RS, Brazil.
authors: Rochele S
authors: RS
authors: Picoloto
authors: Centro de Ciências Químicas, Farmacêuticas e de Alimentos, Universidade Federal de Pelotas, 96010-610, Pelotas, RS, Brazil.
authors: Carla A
authors: CA
authors: Hartwig
authors: Departamento de Química, Universidade Federal de Santa Maria, 97105-900, Santa Maria, RS, Brazil.
authors: Paola A
authors: PA
authors: Mello
authors: Departamento de Química, Universidade Federal de Santa Maria, 97105-900, Santa Maria, RS, Brazil.
authors: Erico M M
authors: EM
authors: Flores
authors: Centro de Ciências Químicas, Farmacêuticas e de Alimentos, Universidade Federal de Pelotas, 96010-610, Pelotas, RS, Brazil. marciamesko@yahoo.com.br.
authors: Marcia F
authors: MF
authors: Mesko
mesh_terms: D001966:Bromine / Q000032:analysis*; D002482:Cellulose / Q000737:chemistry; D004867:Equipment Design; D005240:Feasibility Studies; D006722:Honey / Q000032:analysis*; D006358:Hot Temperature; D007455:Iodine / Q000032:analysis*; D057230:Limit of Detection; D013058:Mass Spectrometry / Q000379:methods*; D008872:Microwaves
chemical_list: D002482:Cellulose; D007455:Iodine; C109691:microcrystalline cellulose; D001966:Bromine
keywords: Bromine determination; Honey analysis; ICP-MS; Iodine determination; Microwave-induced combustion; Sample preparation