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Chaotropic agents in liquid chromatographic method development for the simultaneous analysis of levodopa, carbidopa, entacapone and their impurities

Authorized Users Only
2013
Authors
Vemić, Ana
Jančić-Stojanović, Biljana
Stamenković, Ivana
Malenović, Anđelija
Article (Published version)
Metadata
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Abstract
The simultaneous pharmaceutical analysis of multi-component drugs represents a challenge due to a large total number of analytes present in the sample. These analytes are not only the active pharmaceutical ingredients, but also the impurities that might follow the active substances. The aim of this study was to develop an efficient reversed-phase LC method for the simultaneous analysis of antiparkinsonian drugs levodopa, carbidopa and entacapone along with their six related impurities. For the achievement of desirable separation, different acids with anions possessing different properties according to Hofmeister classification (ortho-phosphoric, trifluoroacetic and perchloric acid) were tested. Finally, in order to draw the unbiased conclusions when optimizing the analytical method, for the final tuning of the gradient program, Box-Behnken experimental design and Derringer's desirability function were used. The experiments were performed on Zorbax Extend C18, 150 mm x 4.6 mm, 5 mu m pa...rticle size column with the UV detection at 280 nm and mobile phase flow rate of 1 mL/min. The optimal mobile phase consisted of methanol and 20 mM trifluoroacetic acid (pH 2.0 adjusted with NaOH), while their ratio is changed according to previously defined gradient program. The method was tested for selectivity, sensitivity, linearity, accuracy and precision, and proved to be suitable for routine qualitative and quantitative analysis of levodopa, carbidopa, entacapone and their impurities in their mixture.

Keywords:
Chaotropic agents / Experimental design / Gradient elution / Antiparkinsonian drugs / Impurities
Source:
Journal of Pharmaceutical and Biomedical Analysis, 2013, 77, 9-15
Publisher:
  • Elsevier Science BV, Amsterdam
Funding / projects:
  • Modelling of different chromatographic systems with chemometrical approach in pharmaceutical analysis (RS-172052)

DOI: 10.1016/j.jpba.2013.01.007

ISSN: 0731-7085

PubMed: 23354116

WoS: 000316306000002

Scopus: 2-s2.0-84873046225
[ Google Scholar ]
22
24
URI
https://farfar.pharmacy.bg.ac.rs/handle/123456789/1927
Collections
  • Radovi istraživača / Researchers’ publications
Institution/Community
Pharmacy
TY  - JOUR
AU  - Vemić, Ana
AU  - Jančić-Stojanović, Biljana
AU  - Stamenković, Ivana
AU  - Malenović, Anđelija
PY  - 2013
UR  - https://farfar.pharmacy.bg.ac.rs/handle/123456789/1927
AB  - The simultaneous pharmaceutical analysis of multi-component drugs represents a challenge due to a large total number of analytes present in the sample. These analytes are not only the active pharmaceutical ingredients, but also the impurities that might follow the active substances. The aim of this study was to develop an efficient reversed-phase LC method for the simultaneous analysis of antiparkinsonian drugs levodopa, carbidopa and entacapone along with their six related impurities. For the achievement of desirable separation, different acids with anions possessing different properties according to Hofmeister classification (ortho-phosphoric, trifluoroacetic and perchloric acid) were tested. Finally, in order to draw the unbiased conclusions when optimizing the analytical method, for the final tuning of the gradient program, Box-Behnken experimental design and Derringer's desirability function were used. The experiments were performed on Zorbax Extend C18, 150 mm x 4.6 mm, 5 mu m particle size column with the UV detection at 280 nm and mobile phase flow rate of 1 mL/min. The optimal mobile phase consisted of methanol and 20 mM trifluoroacetic acid (pH 2.0 adjusted with NaOH), while their ratio is changed according to previously defined gradient program. The method was tested for selectivity, sensitivity, linearity, accuracy and precision, and proved to be suitable for routine qualitative and quantitative analysis of levodopa, carbidopa, entacapone and their impurities in their mixture.
PB  - Elsevier Science BV, Amsterdam
T2  - Journal of Pharmaceutical and Biomedical Analysis
T1  - Chaotropic agents in liquid chromatographic method development for the simultaneous analysis of levodopa, carbidopa, entacapone and their impurities
VL  - 77
SP  - 9
EP  - 15
DO  - 10.1016/j.jpba.2013.01.007
ER  - 
@article{
author = "Vemić, Ana and Jančić-Stojanović, Biljana and Stamenković, Ivana and Malenović, Anđelija",
year = "2013",
abstract = "The simultaneous pharmaceutical analysis of multi-component drugs represents a challenge due to a large total number of analytes present in the sample. These analytes are not only the active pharmaceutical ingredients, but also the impurities that might follow the active substances. The aim of this study was to develop an efficient reversed-phase LC method for the simultaneous analysis of antiparkinsonian drugs levodopa, carbidopa and entacapone along with their six related impurities. For the achievement of desirable separation, different acids with anions possessing different properties according to Hofmeister classification (ortho-phosphoric, trifluoroacetic and perchloric acid) were tested. Finally, in order to draw the unbiased conclusions when optimizing the analytical method, for the final tuning of the gradient program, Box-Behnken experimental design and Derringer's desirability function were used. The experiments were performed on Zorbax Extend C18, 150 mm x 4.6 mm, 5 mu m particle size column with the UV detection at 280 nm and mobile phase flow rate of 1 mL/min. The optimal mobile phase consisted of methanol and 20 mM trifluoroacetic acid (pH 2.0 adjusted with NaOH), while their ratio is changed according to previously defined gradient program. The method was tested for selectivity, sensitivity, linearity, accuracy and precision, and proved to be suitable for routine qualitative and quantitative analysis of levodopa, carbidopa, entacapone and their impurities in their mixture.",
publisher = "Elsevier Science BV, Amsterdam",
journal = "Journal of Pharmaceutical and Biomedical Analysis",
title = "Chaotropic agents in liquid chromatographic method development for the simultaneous analysis of levodopa, carbidopa, entacapone and their impurities",
volume = "77",
pages = "9-15",
doi = "10.1016/j.jpba.2013.01.007"
}
Vemić, A., Jančić-Stojanović, B., Stamenković, I.,& Malenović, A.. (2013). Chaotropic agents in liquid chromatographic method development for the simultaneous analysis of levodopa, carbidopa, entacapone and their impurities. in Journal of Pharmaceutical and Biomedical Analysis
Elsevier Science BV, Amsterdam., 77, 9-15.
https://doi.org/10.1016/j.jpba.2013.01.007
Vemić A, Jančić-Stojanović B, Stamenković I, Malenović A. Chaotropic agents in liquid chromatographic method development for the simultaneous analysis of levodopa, carbidopa, entacapone and their impurities. in Journal of Pharmaceutical and Biomedical Analysis. 2013;77:9-15.
doi:10.1016/j.jpba.2013.01.007 .
Vemić, Ana, Jančić-Stojanović, Biljana, Stamenković, Ivana, Malenović, Anđelija, "Chaotropic agents in liquid chromatographic method development for the simultaneous analysis of levodopa, carbidopa, entacapone and their impurities" in Journal of Pharmaceutical and Biomedical Analysis, 77 (2013):9-15,
https://doi.org/10.1016/j.jpba.2013.01.007 . .

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