EurekaMag.com logo
+ Site Statistics
References:
53,869,633
Abstracts:
29,686,251
+ Search Articles
+ Subscribe to Site Feeds
EurekaMag Most Shared ContentMost Shared
EurekaMag PDF Full Text ContentPDF Full Text
+ PDF Full Text
Request PDF Full TextRequest PDF Full Text
+ Follow Us
Follow on FacebookFollow on Facebook
Follow on TwitterFollow on Twitter
Follow on LinkedInFollow on LinkedIn

+ Translate

Study and determination of elemental impurities by ICP-MS in active pharmaceutical ingredients using single reaction chamber digestion in compliance with USP requirements



Study and determination of elemental impurities by ICP-MS in active pharmaceutical ingredients using single reaction chamber digestion in compliance with USP requirements



Talanta 136: 161-169



In this work a method for active pharmaceutical ingredients (APIs) digestion using the single reaction chamber (SRC-UltraWave™) system was proposed following the new recommendations of United States Pharmacopeia (USP). Levodope (LEVO), primaquine diphosphate (PRIM), propranolol hydrochloride (PROP) and sulfamethoxazole (SULF) were used to evaluate the digestion efficiency of the proposed method. A comparison of digestion efficiency was performed by measuring the carbon content and residual acidity in digests obtained using SRC and in digests obtained using conventional microwave-assisted digestion system (Multiwave(TM)). Three digestion solutions (concentrated HNO3, aqua regia or inverse aqua regia) were evaluated for digestion of APIs. The determination of Cd, Ir, Mn, Mo, Ni, Os, Pb, Pd, Pt, Rh, Ru was performed using inductively coupled plasma mass spectrometry (ICP-MS) in standard mode. Dynamic reaction cell (DRC) mode was used for the determination of (51)V, (52)Cr, (53)Cr, (63)Cu and (65)Cu in order to solve polyatomic ion interferences. Arsenic and Hg were determined using chemical vapor generation coupled to ICP-MS (FI-CVG-ICP-MS). Masses of 500mg of APIs were efficiently digested in a SRC-UltraWave™ system using only HNO3 and allowing a carbon content lower than 250mg L(-1) in final digests. Inverse aqua regia was suitable for digestion of sample masses up to 250mg allowing the determination of Ir, Pd, Pt, Rh and Ru. By using HNO3 or inverse aqua regia, suitable recoveries were obtained (between 91 and 109%) for all analytes (exception for Os). Limits of quantification were in agreement with USP requirements and they ranged from 0.001 to 0.015µg g(-1) for all elemental impurities (exception for Os). The proposed method was suitable for elemental impurities determination in APIs and it can be used in routine analysis for quality control in pharmaceutical industries.

(PDF emailed within 0-6 h: $19.90)

Accession: 058920371

Download citation: RISBibTeXText

PMID: 25702998

DOI: 10.1016/j.talanta.2014.12.023



Related references

Application of LA-ICP-MS as a rapid tool for analysis of elemental impurities in active pharmaceutical ingredients. Journal of Pharmaceutical and Biomedical Analysis 91: 119-122, 2014

Microwave-assisted wet digestion with H2O2 at high temperature and pressure using single reaction chamber for elemental determination in milk powder by ICP-OES and ICP-MS. Talanta 156-157: 232-238, 2016

Impurities in Drug Products and Active Pharmaceutical Ingredients. Critical Reviews in Analytical Chemistry (): 1-7, 2016

Development and validation of a stability-indicating reverse phase ultra performance liquid chromatographic method for the estimation of nebivolol impurities in active pharmaceutical ingredients and pharmaceutical formulation. Se Pu 33(10): 1051-1058, 2016

Control and analysis of hydrazine, hydrazides and hydrazones--genotoxic impurities in active pharmaceutical ingredients (APIs) and drug products. Journal of Pharmaceutical and Biomedical Analysis 54(5): 900-910, 2011

Determination of elemental impurities in pharmaceutical products and related matrices by ICP-based methods: a review. Analytical and Bioanalytical Chemistry 408(17): 4547-4566, 2016

Highly efficient, selective, sensitive and stability indicating RP-HPLC-UV method for the quantitative determination of potential impurities and characterization of four novel impurities in eslicarbazepine acetate active pharmaceutical ingredient by LC/ESI-IT/MS/MS. Journal of Pharmaceutical and Biomedical Analysis 61: 165-175, 2012

Control and analysis of alkyl and benzyl halides and other related reactive organohalides as potential genotoxic impurities in active pharmaceutical ingredients (APIs). Journal of Pharmaceutical and Biomedical Analysis 48(3): 497-507, 2008

The application of structure-based assessment to support safety and chemistry diligence to manage genotoxic impurities in active pharmaceutical ingredients during drug development. Regulatory Toxicology and Pharmacology 44(3): 282-293, 2006

Stability indicating LC method for rapid determination of related substances of O-desmethyl venlafaxine in active pharmaceutical ingredients and pharmaceutical formulations. Journal of Chromatographic Science 52(10): 1247-1254, 2015

The modern approaches to the determination of the content of elemental impurities in the pharmaceutical substances with the use of inductively-coupled plasma mass-spectrometry. Sudebno-Meditsinskaia Ekspertiza 58(6): 31-33, 2016

Recent trends in product development and regulatory issues on impurities in active pharmaceutical ingredient (API) and drug products. Part 1: Predicting degradation related impurities and impurity considerations for pharmaceutical dosage forms. Aaps Pharmscitech 15(1): 198-212, 2014

Low level determinations of methyl methanesulfonate and ethyl methanesulfonate impurities in Lopinavir and Ritonavir Active pharmaceutical ingredients by LC/MS/MS using electrospray ionization. Journal of Pharmaceutical and Biomedical Analysis 55(2): 379-384, 2011

Microwave-assisted digestion using nitric acid for heavy metals and sulfated ash testing in active pharmaceutical ingredients. Die Pharmazie 71(4): 177-180, 2016

Determination of pK(a) values of active pharmaceutical ingredients. TrAC Trends in Analytical Chemistry 26(11): 1043-1061, 2007