A simple, selective, and sensitive gas chromatography-mass spectrometry method for the analysis of five process-related impurities in atenolol bulk drug and capsule formulations

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Abstract

An extremely sensitive and simple gas chromatography with mass spectrometry method was developed and completely validated for the analysis of five process-related impurities, viz., 4-hydroxy-l-phenylglycine, 4-hydroxyphenylacetonitrile, 4-hydroxyphenylacetic acid, methyl-4-hydroxyphenylacetate, and 2-[4-((2RS)-2-hydroxy-3-[(1-methylethyl)amino]propoxy)phenyl]acetonitrile, in atenolol. The separation of impurities was accomplished on a BPX-5 column with dimensions of 50 m × 0.25 mm i.d. and 0.25 μm film thickness. The method validation was performed following International Conference on Harmonisation guidelines in which the method was capable to quantitate 4-hydroxy-l-phenylglycine, 4-hydroxyphenylacetonitrile, and 4-hydroxyphenylacetic acid at 0.3 ppm, and methyl-4-hydroxyphenylacetate and 2-[4-((2RS)-2-hydroxy-3-[(1-methylethyl)amino]propoxy)phenyl]acetonitrile at 0.35 ppm with respect to 10 mg/mL of atenolol. The method was linear over the concentration range of 0.3-10 ppm for 4-hydroxy-l-phenylglycine, 4-hydroxyphenylacetonitrile, and 4-hydroxyphenylacetic acid, and 0.35-10 ppm for methyl-4-hydroxyphenylacetate and 2-[4-((2RS)-2-hydroxy-3-[(1-methylethyl)amino]propoxy)phenyl]acetonitrile. The correlation coefficient in each case was found ≥0.998. The repeatability and recovery values were acceptable, and found between 89.38% and 105.60% for all five impurities under optimized operating conditions. The method developed here is simple, selective, and sensitive with apparently better resolution than the reported methods. Hence, the method is a straightforward and good quality control tool for the quantitation of selected impurities at trace concentrations in atenolol.

LanguageEnglish
JournalJournal of Separation Science
DOIs
StateAccepted/In press - 2017

Fingerprint

Atenolol
Gas chromatography
Capsules
Mass spectrometry
Impurities
Pharmaceutical Preparations
acetonitrile
4-hydroxyphenylacetic acid
4-hydroxyphenylacetate
Acetonitrile
Acids
Quality control
Film thickness
Recovery

Keywords

  • Beta-blockers
  • Genotoxicity
  • Mass spectrometry
  • Method validation

ASJC Scopus subject areas

  • Analytical Chemistry
  • Filtration and Separation

Cite this

@article{b8519461ff9442d3a239fd5d46489947,
title = "A simple, selective, and sensitive gas chromatography-mass spectrometry method for the analysis of five process-related impurities in atenolol bulk drug and capsule formulations",
abstract = "An extremely sensitive and simple gas chromatography with mass spectrometry method was developed and completely validated for the analysis of five process-related impurities, viz., 4-hydroxy-l-phenylglycine, 4-hydroxyphenylacetonitrile, 4-hydroxyphenylacetic acid, methyl-4-hydroxyphenylacetate, and 2-[4-((2RS)-2-hydroxy-3-[(1-methylethyl)amino]propoxy)phenyl]acetonitrile, in atenolol. The separation of impurities was accomplished on a BPX-5 column with dimensions of 50 m × 0.25 mm i.d. and 0.25 μm film thickness. The method validation was performed following International Conference on Harmonisation guidelines in which the method was capable to quantitate 4-hydroxy-l-phenylglycine, 4-hydroxyphenylacetonitrile, and 4-hydroxyphenylacetic acid at 0.3 ppm, and methyl-4-hydroxyphenylacetate and 2-[4-((2RS)-2-hydroxy-3-[(1-methylethyl)amino]propoxy)phenyl]acetonitrile at 0.35 ppm with respect to 10 mg/mL of atenolol. The method was linear over the concentration range of 0.3-10 ppm for 4-hydroxy-l-phenylglycine, 4-hydroxyphenylacetonitrile, and 4-hydroxyphenylacetic acid, and 0.35-10 ppm for methyl-4-hydroxyphenylacetate and 2-[4-((2RS)-2-hydroxy-3-[(1-methylethyl)amino]propoxy)phenyl]acetonitrile. The correlation coefficient in each case was found ≥0.998. The repeatability and recovery values were acceptable, and found between 89.38% and 105.60% for all five impurities under optimized operating conditions. The method developed here is simple, selective, and sensitive with apparently better resolution than the reported methods. Hence, the method is a straightforward and good quality control tool for the quantitation of selected impurities at trace concentrations in atenolol.",
keywords = "Beta-blockers, Genotoxicity, Mass spectrometry, Method validation",
author = "Reddy, {Ambavaram Vijaya Bhaskar} and Zulkifli Yusop and Jafariah Jaafar and {Bin Aris}, Azmi and {Abdul Majid}, Zaiton",
year = "2017",
doi = "10.1002/jssc.201700252",
journal = "Journal of Separation Science",
issn = "1615-9306",
publisher = "Wiley-VCH Verlag",

}

TY - JOUR

T1 - A simple, selective, and sensitive gas chromatography-mass spectrometry method for the analysis of five process-related impurities in atenolol bulk drug and capsule formulations

AU - Reddy,Ambavaram Vijaya Bhaskar

AU - Yusop,Zulkifli

AU - Jaafar,Jafariah

AU - Bin Aris,Azmi

AU - Abdul Majid,Zaiton

PY - 2017

Y1 - 2017

N2 - An extremely sensitive and simple gas chromatography with mass spectrometry method was developed and completely validated for the analysis of five process-related impurities, viz., 4-hydroxy-l-phenylglycine, 4-hydroxyphenylacetonitrile, 4-hydroxyphenylacetic acid, methyl-4-hydroxyphenylacetate, and 2-[4-((2RS)-2-hydroxy-3-[(1-methylethyl)amino]propoxy)phenyl]acetonitrile, in atenolol. The separation of impurities was accomplished on a BPX-5 column with dimensions of 50 m × 0.25 mm i.d. and 0.25 μm film thickness. The method validation was performed following International Conference on Harmonisation guidelines in which the method was capable to quantitate 4-hydroxy-l-phenylglycine, 4-hydroxyphenylacetonitrile, and 4-hydroxyphenylacetic acid at 0.3 ppm, and methyl-4-hydroxyphenylacetate and 2-[4-((2RS)-2-hydroxy-3-[(1-methylethyl)amino]propoxy)phenyl]acetonitrile at 0.35 ppm with respect to 10 mg/mL of atenolol. The method was linear over the concentration range of 0.3-10 ppm for 4-hydroxy-l-phenylglycine, 4-hydroxyphenylacetonitrile, and 4-hydroxyphenylacetic acid, and 0.35-10 ppm for methyl-4-hydroxyphenylacetate and 2-[4-((2RS)-2-hydroxy-3-[(1-methylethyl)amino]propoxy)phenyl]acetonitrile. The correlation coefficient in each case was found ≥0.998. The repeatability and recovery values were acceptable, and found between 89.38% and 105.60% for all five impurities under optimized operating conditions. The method developed here is simple, selective, and sensitive with apparently better resolution than the reported methods. Hence, the method is a straightforward and good quality control tool for the quantitation of selected impurities at trace concentrations in atenolol.

AB - An extremely sensitive and simple gas chromatography with mass spectrometry method was developed and completely validated for the analysis of five process-related impurities, viz., 4-hydroxy-l-phenylglycine, 4-hydroxyphenylacetonitrile, 4-hydroxyphenylacetic acid, methyl-4-hydroxyphenylacetate, and 2-[4-((2RS)-2-hydroxy-3-[(1-methylethyl)amino]propoxy)phenyl]acetonitrile, in atenolol. The separation of impurities was accomplished on a BPX-5 column with dimensions of 50 m × 0.25 mm i.d. and 0.25 μm film thickness. The method validation was performed following International Conference on Harmonisation guidelines in which the method was capable to quantitate 4-hydroxy-l-phenylglycine, 4-hydroxyphenylacetonitrile, and 4-hydroxyphenylacetic acid at 0.3 ppm, and methyl-4-hydroxyphenylacetate and 2-[4-((2RS)-2-hydroxy-3-[(1-methylethyl)amino]propoxy)phenyl]acetonitrile at 0.35 ppm with respect to 10 mg/mL of atenolol. The method was linear over the concentration range of 0.3-10 ppm for 4-hydroxy-l-phenylglycine, 4-hydroxyphenylacetonitrile, and 4-hydroxyphenylacetic acid, and 0.35-10 ppm for methyl-4-hydroxyphenylacetate and 2-[4-((2RS)-2-hydroxy-3-[(1-methylethyl)amino]propoxy)phenyl]acetonitrile. The correlation coefficient in each case was found ≥0.998. The repeatability and recovery values were acceptable, and found between 89.38% and 105.60% for all five impurities under optimized operating conditions. The method developed here is simple, selective, and sensitive with apparently better resolution than the reported methods. Hence, the method is a straightforward and good quality control tool for the quantitation of selected impurities at trace concentrations in atenolol.

KW - Beta-blockers

KW - Genotoxicity

KW - Mass spectrometry

KW - Method validation

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DO - 10.1002/jssc.201700252

M3 - Article

JO - Journal of Separation Science

T2 - Journal of Separation Science

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SN - 1615-9306

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