Ion-pairing high-performance liquid chromatography-ultraviolet （HPLC-UV） methods were developed to determine two commonly used chelating agents, ethylenediaminetetraacetic acid （EDTA） in Abilify （a small molecule...Ion-pairing high-performance liquid chromatography-ultraviolet （HPLC-UV） methods were developed to determine two commonly used chelating agents, ethylenediaminetetraacetic acid （EDTA） in Abilify （a small molecule drug with aripiprazole as the active pharmaceutical ingredient） oral solution and die- thylenetriaminepentaacetic acid （DTPA） in Yervoy （a monoclonal antibody drug with ipilimumab as the active pharmaceutical ingredient） intravenous formulation. Since the analytes, EDTA and DTPA, do not contain chromophores, transition metal ions （Cu2＋, Fe3＋） which generate highly stable metallocom- plexes with the chelating agents were added into the sample preparation to enhance UV detection. The use of metallocomplexes with ion-pairing chromatography provides the ability to achieve the desired sensitivity and selectivity in the development of the method. Specifically, the sample preparation in- volving metallocomplex formation allowed sensitive UV detection. Copper was utilized for the de- termination of EDTA and iron was utilized for the determination of DTPA. In the case of EDTA, a gradient mobile phase separated the components of the formulation from the analyte. In the method for DTPA, the active drug substance, ipilimumab, was eluted in the void. In addition, the optimization of the concentration of the ion-pairing reagent was discussed as a means of enhancing the retention of the aminopolycarboxylic acids （APCAs） including EDTA and DTPA and the specificity of the method. The analytical method development was designed based on the chromatographic properties of the analytes, the nature of the sample matrix and the intended purpose of the method. Validation data were presented for the two methods. Finally, both methods were successfully utilized in determining the fate of the chelates.展开更多
A specific, precise and accurate ion-pair HPLC-UV method has been developed and validated for simultaneous determination of phosphocreatine (PCr), and its metabolite creatine (Cr) as well as related ATP in plasma and ...A specific, precise and accurate ion-pair HPLC-UV method has been developed and validated for simultaneous determination of phosphocreatine (PCr), and its metabolite creatine (Cr) as well as related ATP in plasma and red blood cell (RBC) of rabbits. After addition of TMP as IS, the samples were deproteinized with 6% PCA. The analytes were separated on a Kromasil C18 column using a tertiary gradient mobile phase composed of buffer A (0.2% KH2PO4 + 0.08% tetrabutyl ammonium hydrogen sulphate, pH 3.0), buffer B (buffer A adjusted to pH 7.5 with 1 mol/L NaOH) and MeOH. Detection wavelengths were set at 210 nm for PCr and Cr and 260 nm for ATP and TMP. Some blank samples were initially run for baseline subtraction. The linear detection responses were obtained for PCr concentration over a range of 10 - 7500 mg/ml (plasma) and 5 - 2500 mg/ml (RBC) and for both Cr and ATP concentrations of 10 - 1500 mg/ml (plasma) and 5 - 750 mg/ml (RBC) (r > 0.99). The QC samples of 3 analytes showed intra-day and inter-day precisions (RSD) of - 107%. The method was successfully used to simultaneously determine plasma and RBC concentrations of the 3 analytes and to study pharmacokinetics after iv administration of PCr to rabbits.展开更多
The following article has been retracted due to the investigation of complaints received against it. The Editorial Board found that there are conflicts of interests between the authors and their organization. The scie...The following article has been retracted due to the investigation of complaints received against it. The Editorial Board found that there are conflicts of interests between the authors and their organization. The scientific community takes a very strong view on this matter, and the American Journal of Analytical Chemistry treats all unethical behavior seriously. This paper published in Vol. 5 No. 9 589-597, 2014 has been removed from this site. Title: Determination of Sibutramine and Its N-Desmethyl Metabolites in Human Plasma Using HPLC Coupled with Tandem Mass Author: Mohammad展开更多
A novel reserved\|phase ion\|pair liquid chromatographic method using hexadecyltrimethylammonium bromide（HTMAB） as an ion\|pair reagent for separating the complexes of metal and 8\|hydroxyquinoline\|5\|sulphonic aci...A novel reserved\|phase ion\|pair liquid chromatographic method using hexadecyltrimethylammonium bromide（HTMAB） as an ion\|pair reagent for separating the complexes of metal and 8\|hydroxyquinoline\|5\|sulphonic acid（HQS） coupled with on\|line fluorescence detection has been developed. The chromatographic behavior of metal\|HQS complexes in the proposed system was systematically investigated.When the C\-\{18\} column modified by HTMAB and the suitable mobile phase coupled with fluorescence detection（\%λ\%\-\{ex\}=388 nm; \%λ\%\-\{em\}=518 nm） were employed, the detection limit of cadmium is 7.72 ng/mL with an injection volume of 20 μL, and the linear range of calibration curve for cadmium is 50\800 ng/mL. It was successfully applied to determination of bio\|available cadmium in polluted soils of China. Moreover, the possible species of Cd\|HQS on the column has been investigated by log\|log plot analysis.展开更多
文摘Ion-pairing high-performance liquid chromatography-ultraviolet （HPLC-UV） methods were developed to determine two commonly used chelating agents, ethylenediaminetetraacetic acid （EDTA） in Abilify （a small molecule drug with aripiprazole as the active pharmaceutical ingredient） oral solution and die- thylenetriaminepentaacetic acid （DTPA） in Yervoy （a monoclonal antibody drug with ipilimumab as the active pharmaceutical ingredient） intravenous formulation. Since the analytes, EDTA and DTPA, do not contain chromophores, transition metal ions （Cu2＋, Fe3＋） which generate highly stable metallocom- plexes with the chelating agents were added into the sample preparation to enhance UV detection. The use of metallocomplexes with ion-pairing chromatography provides the ability to achieve the desired sensitivity and selectivity in the development of the method. Specifically, the sample preparation in- volving metallocomplex formation allowed sensitive UV detection. Copper was utilized for the de- termination of EDTA and iron was utilized for the determination of DTPA. In the case of EDTA, a gradient mobile phase separated the components of the formulation from the analyte. In the method for DTPA, the active drug substance, ipilimumab, was eluted in the void. In addition, the optimization of the concentration of the ion-pairing reagent was discussed as a means of enhancing the retention of the aminopolycarboxylic acids （APCAs） including EDTA and DTPA and the specificity of the method. The analytical method development was designed based on the chromatographic properties of the analytes, the nature of the sample matrix and the intended purpose of the method. Validation data were presented for the two methods. Finally, both methods were successfully utilized in determining the fate of the chelates.
文摘A specific, precise and accurate ion-pair HPLC-UV method has been developed and validated for simultaneous determination of phosphocreatine (PCr), and its metabolite creatine (Cr) as well as related ATP in plasma and red blood cell (RBC) of rabbits. After addition of TMP as IS, the samples were deproteinized with 6% PCA. The analytes were separated on a Kromasil C18 column using a tertiary gradient mobile phase composed of buffer A (0.2% KH2PO4 + 0.08% tetrabutyl ammonium hydrogen sulphate, pH 3.0), buffer B (buffer A adjusted to pH 7.5 with 1 mol/L NaOH) and MeOH. Detection wavelengths were set at 210 nm for PCr and Cr and 260 nm for ATP and TMP. Some blank samples were initially run for baseline subtraction. The linear detection responses were obtained for PCr concentration over a range of 10 - 7500 mg/ml (plasma) and 5 - 2500 mg/ml (RBC) and for both Cr and ATP concentrations of 10 - 1500 mg/ml (plasma) and 5 - 750 mg/ml (RBC) (r > 0.99). The QC samples of 3 analytes showed intra-day and inter-day precisions (RSD) of - 107%. The method was successfully used to simultaneously determine plasma and RBC concentrations of the 3 analytes and to study pharmacokinetics after iv administration of PCr to rabbits.
文摘The following article has been retracted due to the investigation of complaints received against it. The Editorial Board found that there are conflicts of interests between the authors and their organization. The scientific community takes a very strong view on this matter, and the American Journal of Analytical Chemistry treats all unethical behavior seriously. This paper published in Vol. 5 No. 9 589-597, 2014 has been removed from this site. Title: Determination of Sibutramine and Its N-Desmethyl Metabolites in Human Plasma Using HPLC Coupled with Tandem Mass Author: Mohammad
文摘A novel reserved\|phase ion\|pair liquid chromatographic method using hexadecyltrimethylammonium bromide（HTMAB） as an ion\|pair reagent for separating the complexes of metal and 8\|hydroxyquinoline\|5\|sulphonic acid（HQS） coupled with on\|line fluorescence detection has been developed. The chromatographic behavior of metal\|HQS complexes in the proposed system was systematically investigated.When the C\-\{18\} column modified by HTMAB and the suitable mobile phase coupled with fluorescence detection（\%λ\%\-\{ex\}=388 nm; \%λ\%\-\{em\}=518 nm） were employed, the detection limit of cadmium is 7.72 ng/mL with an injection volume of 20 μL, and the linear range of calibration curve for cadmium is 50\800 ng/mL. It was successfully applied to determination of bio\|available cadmium in polluted soils of China. Moreover, the possible species of Cd\|HQS on the column has been investigated by log\|log plot analysis.
