Determination of Elemental Impurities in Acyclovir Ointment and Raw Materials Using Microwave Acid Digestion (MW-AD) and ICP-MS

Abstract

Inorganic elements present in pharmaceutical products were determined by inductively coupled plasma-mass spectrometer (ICP-MS), employing microwave acid digestion as a sample preparation method. , were determined in acyclovir ointment and its constituents. Elemental impurities in the pharmaceutical samples were determined using an inductively coupled plasma-universal cell technology-mass spectrometer (ICP-UCT-MS) operated in kinetic energy discrimination (KED) and standard mode. The accuracy of the method was assessed by means of addition and recovery experiments. Except for Cr, spiked recoveries of the elements added to the samples before microwave acid digestion (MW-AD) step were between 95.1 and 126%, and after MW-AD step ranged from 85.6 to 132%. Limits of detection (LOD) obtained by proposed method is in agreement to those required by the U.S. Pharmacopeia Convention (USP), showing that the ICP-MS technique is well suited for quantification of these elements. The LOD's (ng L -

Application of ICH Guidelines for the Assessment and Control of Elemental Impurities in Parecoxib Sodium by Graphite-Digestion and ICP-MS

“…Analysis of elemental impurities in drugs, foods, plants, and crude oil using microwave oven digestion combined with an inductively coupled plasma-mass spectrometer (ICP-MS) has been previously reported though [7][8][9][10][11], there are limited reports about elemental impurities in drugs analyzed by a none microwave oven digestion combined with ICP-MS due to the complex structures of analytes, like parecoxib sodium, in the form of salt (Figure 1). Microwave oven digestion is an e ective way but it is time-consuming and not safe.…”

Development of Green Methods for the Determination of Elemental Impurities in Commercial Pharmaceutical Tablets

“…In this regard, researchers have developed a variety of sample preparation methods coupled to sensitive detection techniques in order to improve detectability of elemental impurities. Plasma-based techniques, such as inductively coupled plasma optic emission spectrometry (ICP-OES) [10][11][12][13][14] and inductively coupled plasma mass spectrometry (ICP-MS) [11,13,[15][16][17][18][19][20][21], are frequently used with this purpose, due to their high sensitivity, multielemental capacity and wide linear range [5,22].…”

“…Several sample preparation methods have been developed aiming for elemental impurities determination in pharmaceutical ingredients, such as microwave-assisted wet digestion (MAWD) [10,12,13,18,19,27], microwave-induced combustion (MIC) [15], dissolution [16] and MAWD with single reaction chamber (MAWD-SRC) [20,28]. Out of these, MAWD is usually the method of choice, as modern microwave equipment enables precise control of temperature and pressure inside digestion vessels, as well as provide the direct heating of the samples [29].…”

“…It is important to mention as well that most published studies focus on the decomposition of active pharmaceutical ingredients (API). Only a few studies were found in the literature on the digestion of the commercial pharmaceutical drug, and even less when inorganic excipients are present in the formulation [10,12,18,28,44]. In this sense, the aim of this study is to develop sample preparation methods for oral drugs used in the treatment of type 2 diabetes and the further determination of class 1 and 2A elemental impurities.…”

Evaluation of the Elemental Impurities of the Drug Captopril Marketed Commercialized in Rio de Janeiro, Brazil

“…[10][11] These chapters emphasize the importance of assessing elemental impurities not only in active pharmaceutical ingredients and excipients, but also in final pharmaceutical products, aiming at the possibility of risk, considering the oral permissible daily exposures (PDEs). Examples of this include Gonzales (2017) 12 regarding acyclovir ointment samples and raw materials, Tavares (2013) 13 for radipharmaceuticals and Gang (2015) 14 for pharmaceutical excipients.…”