Development of high-performance liquid chromatographic determination of salicylaldehyde isonicotinoyl hydrazone in rabbit plasma and application of this method to an in vivo study
An analytical methodology appropriate for the determination of the novel drug candidate salicylaldehyde isonicotinoyl hydrazone (SIH) in rabbit plasma has been developed and validated. Desirable chromatographic separation was achieved on a C18 column employing a mixture of phosphate buffer (0.01 M N...
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Published in | Journal of separation science Vol. 28; no. 12; pp. 1300 - 1306 |
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Main Authors | , , , , , , |
Format | Journal Article |
Language | English |
Published |
Weinheim
WILEY-VCH Verlag
01.08.2005
WILEY‐VCH Verlag Wiley |
Subjects | |
Online Access | Get full text |
ISSN | 1615-9306 1615-9314 |
DOI | 10.1002/jssc.200500077 |
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Abstract | An analytical methodology appropriate for the determination of the novel drug candidate salicylaldehyde isonicotinoyl hydrazone (SIH) in rabbit plasma has been developed and validated. Desirable chromatographic separation was achieved on a C18 column employing a mixture of phosphate buffer (0.01 M NaH2PO4·2 H2O with 2 mM EDTA, pH 6.0) and methanol (53:47; v/v) as the mobile phase. In order to develop a suitable sample preparation procedure, different methods have been tested (solid‐phase extraction, liquid‐liquid extraction, and protein precipitation). Protein precipitation using 0.1 M HClO4 and acetonitrile allowed the highest recoveries of the analyte to be reproducibly attained. The analytical methodology developed in this study was validated with respect to linearity (0.26–30.0 μg/mL), accuracy, precision, selectivity, recovery, and stability. A concentration of 0.26 μg/mL was determined as the LLOQ. The chromatographic method was applied to a preliminary plasma pharmacokinetic study. This study has provided the first information about the concentrations of SIH in plasma of a living subject. These results could have a significant impact on further progress in the development of this promising compound. |
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AbstractList | An analytical methodology appropriate for the determination of the novel drug candidate salicylaldehyde isonicotinoyl hydrazone (SIH) in rabbit plasma has been developed and validated. Desirable chromatographic separation was achieved on a C18 column employing a mixture of phosphate buffer (0.01 M NaH2PO4·2 H2O with 2 mM EDTA, pH 6.0) and methanol (53:47; v/v) as the mobile phase. In order to develop a suitable sample preparation procedure, different methods have been tested (solid‐phase extraction, liquid‐liquid extraction, and protein precipitation). Protein precipitation using 0.1 M HClO4 and acetonitrile allowed the highest recoveries of the analyte to be reproducibly attained. The analytical methodology developed in this study was validated with respect to linearity (0.26–30.0 μg/mL), accuracy, precision, selectivity, recovery, and stability. A concentration of 0.26 μg/mL was determined as the LLOQ. The chromatographic method was applied to a preliminary plasma pharmacokinetic study. This study has provided the first information about the concentrations of SIH in plasma of a living subject. These results could have a significant impact on further progress in the development of this promising compound. An analytical methodology appropriate for the determination of the novel drug candidate salicylaldehyde isonicotinoyl hydrazone (SIH) in rabbit plasma has been developed and validated. Desirable chromatographic separation was achieved on a C18 column employing a mixture of phosphate buffer (0.01 M NaH2PO4 x 2 H2O with 2 mM EDTA, pH 6.0) and methanol (53:47; v/v) as the mobile phase. In order to develop a suitable sample preparation procedure, different methods have been tested (solid-phase extraction, liquid-liquid extraction, and protein precipitation). Protein precipitation using 0.1 M HClO4 and acetonitrile allowed the highest recoveries of the analyte to be reproducibly attained. The analytical methodology developed in this study was validated with respect to linearity (0.26-30.0 microg/mL), accuracy, precision, selectivity, recovery, and stability. A concentration of 0.26 microg/mL was determined as the LLOQ. The chromatographic method was applied to a preliminary plasma pharmacokinetic study. This study has provided the first information about the concentrations of SIH in plasma of a living subject. These results could have a significant impact on further progress in the development of this promising compound.An analytical methodology appropriate for the determination of the novel drug candidate salicylaldehyde isonicotinoyl hydrazone (SIH) in rabbit plasma has been developed and validated. Desirable chromatographic separation was achieved on a C18 column employing a mixture of phosphate buffer (0.01 M NaH2PO4 x 2 H2O with 2 mM EDTA, pH 6.0) and methanol (53:47; v/v) as the mobile phase. In order to develop a suitable sample preparation procedure, different methods have been tested (solid-phase extraction, liquid-liquid extraction, and protein precipitation). Protein precipitation using 0.1 M HClO4 and acetonitrile allowed the highest recoveries of the analyte to be reproducibly attained. The analytical methodology developed in this study was validated with respect to linearity (0.26-30.0 microg/mL), accuracy, precision, selectivity, recovery, and stability. A concentration of 0.26 microg/mL was determined as the LLOQ. The chromatographic method was applied to a preliminary plasma pharmacokinetic study. This study has provided the first information about the concentrations of SIH in plasma of a living subject. These results could have a significant impact on further progress in the development of this promising compound. An analytical methodology appropriate for the determination of the novel drug candidate salicylaldehyde isonicotinoyl hydrazone (SIH) in rabbit plasma has been developed and validated. Desirable chromatographic separation was achieved on a C 18 column employing a mixture of phosphate buffer (0.01 M NaH 2 PO 4 ·2 H 2 O with 2 mM EDTA, pH 6.0) and methanol (53:47; v/v ) as the mobile phase. In order to develop a suitable sample preparation procedure, different methods have been tested (solid‐phase extraction, liquid‐liquid extraction, and protein precipitation). Protein precipitation using 0.1 M HClO 4 and acetonitrile allowed the highest recoveries of the analyte to be reproducibly attained. The analytical methodology developed in this study was validated with respect to linearity (0.26–30.0 μg/mL), accuracy, precision, selectivity, recovery, and stability. A concentration of 0.26 μg/mL was determined as the LLOQ. The chromatographic method was applied to a preliminary plasma pharmacokinetic study. This study has provided the first information about the concentrations of SIH in plasma of a living subject. These results could have a significant impact on further progress in the development of this promising compound. An analytical methodology appropriate for the determination of the novel drug candidate salicylaldehyde isonicotinoyl hydrazone (SIH) in rabbit plasma has been developed and validated. Desirable chromatographic separation was achieved on a C18 column employing a mixture of phosphate buffer (0.01 M NaH2PO4 x 2 H2O with 2 mM EDTA, pH 6.0) and methanol (53:47; v/v) as the mobile phase. In order to develop a suitable sample preparation procedure, different methods have been tested (solid-phase extraction, liquid-liquid extraction, and protein precipitation). Protein precipitation using 0.1 M HClO4 and acetonitrile allowed the highest recoveries of the analyte to be reproducibly attained. The analytical methodology developed in this study was validated with respect to linearity (0.26-30.0 microg/mL), accuracy, precision, selectivity, recovery, and stability. A concentration of 0.26 microg/mL was determined as the LLOQ. The chromatographic method was applied to a preliminary plasma pharmacokinetic study. This study has provided the first information about the concentrations of SIH in plasma of a living subject. These results could have a significant impact on further progress in the development of this promising compound. |
Author | Popelová, Olga Geršl, Vladimír Poňka, Přemysl Kovaříková, Petra Klimeš, Jiří Štěrba, Martin Mokrý, Milan |
Author_xml | – sequence: 1 givenname: Petra surname: KOVARIKOVA fullname: KOVARIKOVA, Petra organization: Department of Pharmaceutical Chemistry and Drug Control, Faculty of Pharmacy in Hradec Králové, Charles University in Prague, Hradec Králové, Czech Republic – sequence: 2 givenname: Jiri surname: KLIMES fullname: KLIMES, Jiri organization: Department of Pharmaceutical Chemistry and Drug Control, Faculty of Pharmacy in Hradec Králové, Charles University in Prague, Hradec Králové, Czech Republic – sequence: 3 givenname: Martin surname: STERBA fullname: STERBA, Martin organization: Department of Pharmacology, Faculty of Medicine in Hradec Králové, Hradec Králové, Czech Republic – sequence: 4 givenname: Olga surname: POPELOVA fullname: POPELOVA, Olga organization: Department of Pharmacology, Faculty of Medicine in Hradec Králové, Hradec Králové, Czech Republic – sequence: 5 givenname: Milan surname: MOKRY fullname: MOKRY, Milan organization: Department of Pharmaceutical Chemistry and Drug Control, Faculty of Pharmacy in Hradec Králové, Charles University in Prague, Hradec Králové, Czech Republic – sequence: 6 givenname: Vladimir surname: GERSL fullname: GERSL, Vladimir organization: Department of Pharmacology, Faculty of Medicine in Hradec Králové, Hradec Králové, Czech Republic – sequence: 7 givenname: Premysl surname: PONKA fullname: PONKA, Premysl organization: LadyDavis Institute for Medical Research, McGill University, Montreal, Canada |
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Cites_doi | 10.1007/s00432-003-0498-7 10.1182/asheducation-2001.1.47 10.1016/S0020-1693(00)80471-5 10.1159/000203952 10.1196/annals.1306.026 10.1002/jssc.200401878 10.1016/0014-5793(79)80111-8 10.7326/0003-4819-120-6-199403150-00008 10.1016/S0304-4165(02)00478-6 10.2174/0929867033457638 |
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Keywords | Organic hydrazide Solid phase extraction Biological fluid Chemical analysis Intravenous administration HPLC chromatography Rabbit Solvent extraction Blood Chemical enrichment Blood plasma Pyridine derivatives Sample preparation Siderophore Hydrazone Ionophore HPLC Quantitative analysis Trace analysis Validation Chemical precipitation Liquid liquid extraction Benzene derivatives Iron-chelator Lagomorpha In vivo Vertebrata Mammalia SIH Salicylaldehyde isonicotinoyl hydrazone Animal Chelating agent Phenols Iron Ions Pharmacokinetics |
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Snippet | An analytical methodology appropriate for the determination of the novel drug candidate salicylaldehyde isonicotinoyl hydrazone (SIH) in rabbit plasma has been... |
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SubjectTerms | Aldehydes - blood Analytical chemistry Animals Blood Chemical Analysis - methods Blood Chemical Analysis - standards Blood Chemical Analysis - statistics & numerical data Chemistry Chromatographic methods and physical methods associated with chromatography Chromatography, High Pressure Liquid - methods Chromatography, High Pressure Liquid - standards Chromatography, High Pressure Liquid - statistics & numerical data Drug Stability Exact sciences and technology HPLC Hydrazones - blood Iron Chelating Agents - analysis Iron-chelator Male Other chromatographic methods Pharmacokinetics Quality Control Rabbits Salicylaldehyde isonicotinoyl hydrazone SIH |
Title | Development of high-performance liquid chromatographic determination of salicylaldehyde isonicotinoyl hydrazone in rabbit plasma and application of this method to an in vivo study |
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