Chaotropic agents in liquid chromatographic method development for the simultaneous analysis of levodopa, carbidopa, entacapone and their impurities
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 / ImpuritiesSource:
Journal of Pharmaceutical and Biomedical Analysis, 2013, 77, 9-15Publisher:
- 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
Collections
Institution/Community
PharmacyTY - 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 . .