Bromine and iodine determination in active pharmaceutical ingredients by ICP-MS

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[1] [1,Muller, Aline L. H.
[2] 1,Mello, Paola A.
[3] Mesko, Marcia F.
[4] Duarte, Fabio A.
[5] 1,Dressler, Valderi L.
[6] 1,Muller, Edson I.
[7] 1,Flores, Erico M. M.
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Flores, E.M.M. (ericommf@gmail.com) | 1889年 / Royal Society of Chemistry卷 / 27期
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A method based on microwave-induced combustion (MIC) was applied for digestion of active pharmaceutical ingredients (APIs) and subsequent determination of bromine and iodine by inductively coupled plasma mass spectrometry (ICP-MS). Ten APIs including amoxicillin; atenolol; clavulanic acid; clonazepan; diltiazem; haloperidol; imipramine; nimesulide; propranolol and sodium diclofenac were decomposed by MIC. Combustion of 500 mg of each API was possible in less than 30 s using 20 bars of oxygen as initial pressure. A single and diluted solution (50 mmol L-1 (NH4) 2CO3) was used for the absorption of both analytes and a reflux step of 5 min was applied to improve analyte recoveries. Final digests were suitable to Br and I determination by ICP-MS. Accuracy was evaluated using certified reference materials and agreement better than 95 and 97% for Br and I was obtained; respectively. Results were also compared with those obtained by ion chromatography (IC). The carbon content in digests obtained after decomposition was lower than 500 mg L-1 avoiding interferences in the determination step for both techniques. With the use of MIC; up to eight samples could be processed simultaneously and only diluted solutions are required; minimizing reagent consumption and waste generation. The limits of detection for Br and I by ICP-MS were 0.02 and 0.001 μg g-1; respectively; that were considered suitable for the determination of these elements in the investigated active pharmaceutical ingredients. © 2012 The Royal Society of Chemistry;
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