Peak fronting in reversed-phase high-performance liquid chromatography: a study of the chromatographic behavior of oxycodone hydrochloride

1999 ◽  
Vol 19 (5) ◽  
pp. 669-678 ◽  
Author(s):  
Kevin Broglé ◽  
Raphael M. Ornaf ◽  
David Wu ◽  
Philip J. Palermo
2014 ◽  
Vol 52 (1-2) ◽  
pp. 71-76
Author(s):  
O. Rotkaja ◽  
J. Golushko ◽  
P. Mekss

Abstract Protein molecules present more complex analytical challenges than conventional low molecular weight pharmaceutical compounds, and thus need powerful analytical approaches for the entire pharmaceutical development and quality control process. We used high-performance liquid chromatography to investigate the reversed-phase chromatographic behavior of eleven proteins (albumin, carbonic anhydrase, cytohrome c, L-glutamic dehydrogenase, enolase, α-lactoglobulin, Lysozyme, myoglobin and ribonuclease. By using a water/organic solvent/trifluoroacetic acid system the influence of experimental parameters was examined, and chromatographic results from two C4- chain-length supports were found to be comparable. The model enables prediction of initial conditions from two experimental data points for different types of reversed-phase columns with water-acetonitrile-TFA, water-methanol-TFA, and water-2-propanol-TFA mobile phases


2017 ◽  
pp. 44-48
Author(s):  
Larisa Sotnikova ◽  
Larisa Sotnikova ◽  
Polina Goryunova ◽  
Polina Goryunova ◽  
Sergey Sozinov ◽  
...  

The present paper illustrates the results of the study on chromatographic behavior and optimization of some parameters of the method of quantitative determination of bornyl acetate and isobornyl acetate diastereomers under the conditions of reversed-phase high- performance liquid chromatography. Chromatography was performed with HPLC platform Agilent 1200 with diode-matrix detector and a column Agilent Zorbax XDB, Extend-C18. Detection of the studied analytes was performed at a wavelength of 210 nm. Determinationof the concentration of bornyl acetate isomers was carried out in mixture with other components of the Abiessibirica essential oil in chromatographic systems with mobile phases of acetonitrile-water or isopropyl alcohol-water. The range of analyte concentrations in a sample was varied from 2 to 430 mg/ml for bornyl acetate and from 2 to 950 mg/ml for isobornyl acetate. It is stated that in a chromatographic system with a mobile phase, based on acetonitrile, the peaks of the studied components have an asymmetric shape, and the retention times of analytes increase with the decrease of their concentrations in a sample. In a chromatographic system with isopropyl alcohol the asymmetry of the bornyl acetate peak disappears, the width decreases and the retention time stabilizes. For isobornyl acetate a peak width also decreases, its asymmetry is preserved, but at the same time, the asymmetry coefficient takes on permitted values (less than 2). Calibration charts for the mentioned compounds in the used eluents are linear throughout the studiedconcentration range with correlation coefficients of R2>0.998. Thus, the conducted researches allow to recommend the reversed-phaseHPLC variant for the separate quantitative determination of bornyl acetate and isobornyl acetate in the pine oil samples.


2021 ◽  
pp. 147-158
Author(s):  
Strahinja Kovacevic ◽  
Milica Karadzic-Banjac ◽  
Jasmina Anojcic ◽  
Lidija Jevric ◽  
Sanja Podunavac-Kuzmanovic ◽  
...  

Homoandrostane derivatives, as compounds with significant bioactivity, were studied in terms of their chromatographic behavior in reversed-phase ultra-high performance liquid chromatography (RP-UHPLC). In the present study, five androstane derivatives from the series of homoandrostanes were analyzed, including: 3?-hydroxy-17-oxa-17a-homoandrost-5-en-16-one, 3?,5?-dihydroxy-17- oxa-17a-homoandrostane-6,16-dione, 17-oxa-5?,6?-epoxy-17a-homoandrostane-3,16-dione, 5?-hydroxy- 17-oxa-17a-homoandrostane-6,16-dione-3?-yl acetate and 3?-hydroxy-17-oxa-5?,6?-epoxy-Dhomoandrostan- 16-one. The compounds were analyzed by applying methanol-water mobile phases with different volume fractions of methanol, as a polar protic solvent, and logk0 parameters of each compound were determined. The outstanding correlations between in silico logP descriptors and logk0 parameters were obtained, as well as between in silico logD descriptors and logk0 parameters. The logk0 parameters are very well correlated with polar surface area (PSA) descriptor as well. The studied compounds and lipophilicity descriptors (including the chromatographic lipophilicity parameters - logk0) were clustered applying hierarchical cluster analysis (HCA) in the form of clustered heat map known as double dendrogram. Furthermore, the sum of ranking differences (SRD) method was used for the ranking of the lipophilicity measures of the analyzed homoandrostane derivatives so the most suitable lipophilicity measures of this series of compounds can be selected.


Author(s):  
Raju Chandra ◽  
Manisha Pant ◽  
Harchan Singh ◽  
Deepak Kumar ◽  
Ashwani Sanghi

A reliable and reproducible reversed-phase high performance liquid chromatography (RP-HPLC) was developed for the quantitative determination of Remipril drug content from marketed bulk tablets. The active ingredient of Remipril separation achieved with C18 column using the methanol water mobile phase in the ratio of 40:60 (v/v). The active ingredient of the drug content quantify with UV detector at 215 nm. The retention time of Remipril is 5.63 min. A good linearity relation (R2=0.999) was obtained between drug concentration and average peak areas. The limit of detection and limit of quantification of the instrument were calculated 0.03 and 0.09 µg/mL, respectively. The accuracy of the method validation was determined 102.72% by recoveries method.


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