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Optimization of sample preparation and a quadrupole ICP-MS measurement protocol for the determination of elemental impurities in pharmaceutical substances in compliance with USP guidelines

Karen Van Hoecke UGent, Christian Catry and Frank Vanhaecke UGent (2012) JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY. 27(11). p.1909-1919
abstract
Both new guidelines concerning elemental impurity limit concentrations and novel analytical procedures for elemental analysis of pharmaceutical substances are being adopted by the United States Pharmacopeia (USP). This paper outlines the optimization of two sample preparation procedures for organic pharmaceutical excipient products, one relying on direct dissolution in an aqueous medium and another on microwave-assisted acid digestion. Optimization particularly involved the stabilization and reliable determination of Hg, Pd and Os. Analyte concentrations and spike recoveries were determined in two organic pharmaceutical excipients using a quadrupole ICP-MS instrument equipped with a collision–reaction cell. Aqueous dissolution was achieved with 0.009mMKBrO3 in 1% (v/v) HNO3 and 1% (v/v) HCl and microwave-assisted acid digestion was performed with aqua regia. Polyatomic interferences originally hampering the accurate determination of 51V, 52Cr, 53Cr, 55Mn, 56Fe and 75As were eliminated through introduction of He/H2 collision–reaction gas at a flow rate of 4.5–5.1 ml min-1 and applying a kinetic energy barrier of 3 V between the hexapole collision–reaction cell and the quadrupole analyzer. Limits of detection were more than a factor of ten lower than the proposed limit concentrations for parenteral administration and the impurity concentrations in the products tested never exceeded the limit concentrations defined by USP. Elemental spike recoveries ranged between 93.8 and 109.9% when standard addition was used for calibration, with relative standard deviations (RSDs) < 12.7%. It is expected that the proposed procedures can be directly implemented for routine impurity analysis of a broad spectrum of pharmaceutical substances.
Please use this url to cite or link to this publication:
author
organization
year
type
journalArticle (original)
publication status
published
subject
keyword
MERCURY, MASS-SPECTROMETRY, METALS
journal title
JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY
J. Anal. At. Spectrom.
volume
27
issue
11
pages
1909 - 1919
Web of Science type
Article
Web of Science id
000310479900010
JCR category
SPECTROSCOPY
JCR impact factor
3.155 (2012)
JCR rank
7/43 (2012)
JCR quartile
1 (2012)
ISSN
0267-9477
DOI
10.1039/C2JA30128H
language
English
UGent publication?
yes
classification
A1
copyright statement
I have transferred the copyright for this publication to the publisher
id
3005642
handle
http://hdl.handle.net/1854/LU-3005642
date created
2012-10-03 16:33:33
date last changed
2013-07-15 13:25:43
@article{3005642,
  abstract     = {Both new guidelines concerning elemental impurity limit concentrations and novel analytical procedures for elemental analysis of pharmaceutical substances are being adopted by the United States Pharmacopeia (USP). This paper outlines the optimization of two sample preparation procedures for organic pharmaceutical excipient products, one relying on direct dissolution in an aqueous medium and another on microwave-assisted acid digestion. Optimization particularly involved the stabilization and reliable determination of Hg, Pd and Os. Analyte concentrations and spike recoveries were determined in two organic pharmaceutical excipients using a quadrupole ICP-MS instrument equipped with a collision--reaction cell. Aqueous dissolution was achieved with 0.009mMKBrO3 in 1\% (v/v) HNO3 and 1\% (v/v) HCl and microwave-assisted acid digestion was performed with aqua regia. Polyatomic interferences originally hampering the accurate determination of 51V, 52Cr, 53Cr, 55Mn, 56Fe and 75As were eliminated through introduction of He/H2 collision--reaction gas at a flow rate of 4.5--5.1 ml min-1 and applying a kinetic energy barrier of 3 V between the hexapole collision--reaction cell and the quadrupole analyzer. Limits of detection were more than a factor of ten lower than the proposed limit concentrations for parenteral administration and the impurity concentrations in the products tested never exceeded the limit concentrations defined by USP. Elemental spike recoveries ranged between 93.8 and 109.9\% when standard addition was used for calibration, with relative standard deviations (RSDs) {\textlangle} 12.7\%. It is expected that the proposed procedures can be directly implemented for routine impurity analysis of a broad spectrum of pharmaceutical substances.},
  author       = {Van Hoecke, Karen and Catry, Christian and Vanhaecke, Frank},
  issn         = {0267-9477},
  journal      = {JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY},
  keyword      = {MERCURY,MASS-SPECTROMETRY,METALS},
  language     = {eng},
  number       = {11},
  pages        = {1909--1919},
  title        = {Optimization of sample preparation and a quadrupole ICP-MS measurement protocol for the determination of elemental impurities in pharmaceutical substances in compliance with USP guidelines},
  url          = {http://dx.doi.org/10.1039/C2JA30128H},
  volume       = {27},
  year         = {2012},
}

Chicago
Van Hoecke, Karen, Christian Catry, and Frank Vanhaecke. 2012. “Optimization of Sample Preparation and a Quadrupole ICP-MS Measurement Protocol for the Determination of Elemental Impurities in Pharmaceutical Substances in Compliance with USP Guidelines.” Journal of Analytical Atomic Spectrometry 27 (11): 1909–1919.
APA
Van Hoecke, K., Catry, C., & Vanhaecke, F. (2012). Optimization of sample preparation and a quadrupole ICP-MS measurement protocol for the determination of elemental impurities in pharmaceutical substances in compliance with USP guidelines. JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, 27(11), 1909–1919.
Vancouver
1.
Van Hoecke K, Catry C, Vanhaecke F. Optimization of sample preparation and a quadrupole ICP-MS measurement protocol for the determination of elemental impurities in pharmaceutical substances in compliance with USP guidelines. JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY. 2012;27(11):1909–19.
MLA
Van Hoecke, Karen, Christian Catry, and Frank Vanhaecke. “Optimization of Sample Preparation and a Quadrupole ICP-MS Measurement Protocol for the Determination of Elemental Impurities in Pharmaceutical Substances in Compliance with USP Guidelines.” JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY 27.11 (2012): 1909–1919. Print.