Microwave-assisted digestion using nitric acid for heavy metals and sulfated ash testing in active pharmaceutical ingredients

0472554 - MBÚ 2017 RIV DE eng J - Journal Article
Pluháček, Tomáš - Hanzal, J. - Hendrych, J. - Milde, D.
Microwave-assisted digestion using nitric acid for heavy metals and sulfated ash testing in active pharmaceutical ingredients.
Pharmazie. Roč. 71, č. 4 (2016), s. 177-180. ISSN 0031-7144. E-ISSN 0031-7144
Institutional support: RVO:61388971
Keywords : PLASMA-MASS SPECTROMETRY * ICP-MS * ELEMENTAL IMPURITIES
Subject RIV: EE - Microbiology, Virology
Impact factor: 1.126, year: 2016

The monitoring of inorganic impurities in active pharmaceutical ingredients plays a crucial role in the quality control of the pharmaceutical production. The heavy metals and residue on ignition/sulfated ash methods employing microwave-assisted digestion with concentrated nitric acid have been demonstrated as alternatives to inappropriate compendial methods recommended in United States Pharmacopoeia (USP) and European Pharmacopoeia (Ph. Eur.). The recoveries using the heavy metals method ranged between 89 % and 122 % for nearly all USP and Ph. Eur. restricted elements as well as the recoveries of sodium sulfate spikes were around 100 % in all tested matrices. The proposed microwave-assisted digestion method allowed simultaneous decomposition of 15 different active pharmaceutical ingredients with sample weigh up to 1 g. The heavy metals and sulfated ash procedures were successfully applied to the determination of heavy metals and residue on ignition/sulfated ash content in mycophenolate mofetil, nicergoline and silymarin.
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Permanent Link: http://hdl.handle.net/11104/0269838