Mobile phase pH and organic modifier in reversed-phase LC–ESI-MS bioanalytical methods: assessment of sensitivity, chromatography and correlation of retention time within silicologD predictions

Bioanalysis ◽  
2013 ◽  
Vol 5 (22) ◽  
pp. 2753-2770 ◽  
Author(s):  
Steve Silvester
Keyword(s):  
Retention Time ◽  
Mobile Phase ◽  
Bioanalytical Methods ◽  
Reversed Phase ◽  
Organic Modifier ◽  
Esi Ms ◽  
Reversed Phase Lc

scholarly journals Quantitation of Multiple Sphingolipid Classes Using Normal and Reversed-Phase LC–ESI–MS/MS: Comparative Profiling of Two Cell Lines

Lipids ◽  
2011 ◽  
Vol 47 (2) ◽  
pp. 209-226 ◽  
Author(s):  
M. Athar Masood ◽  
Raghavendra P. Rao ◽  
Jairaj K. Acharya ◽  
Josip Blonder ◽  
Timothy D. Veenstra
Keyword(s):  
Cell Lines ◽  
Reversed Phase ◽  
Esi Ms ◽  
Reversed Phase Lc

VALIDATED RP-HPLC METHOD FOR DETERMINATION OF ENZALUTAMIDE IN BULK DRUG AND PHARMACEUTICAL DOSAGE FORM

INDIAN DRUGS ◽  
2016 ◽  
Vol 53 (11) ◽  
pp. 46-50
Author(s):  
Z. G Khan ◽  
◽  
S. S. Patil ◽  
P. K. Deshmukh ◽  
P. O. Patil
Keyword(s):  
Retention Time ◽  
Mobile Phase ◽  
High Performance ◽  
Reversed Phase ◽  
Hplc Method ◽  
Uv Detector ◽  
Chromatography Method ◽  
Pharmaceutical Dosage Form ◽  
Bulk Drug

Novel, isocratic reversed phase high performance liquid chromatography method was developed and validated for the determination of enzalutamide (EZA) in bulk drug and pharmaceutical formulation. Efficient separation was achieved on PrincetonSPHER C18 100A, 5μ (250×4.6 mm) under the isocratic mode of elution using acetonitrile: water (80:20) % V/V as a mobile phase pumped in to the column at flow rate 1.0 mL/min. The effluent was monitored at 237.0 nm using UV detector. EZA was eluted in the given mobile phase at retention time (tR) of 3.2 minutes. The standard calibration curve was linear over the concentration range 10 - 60 μg/mL with correlation coefficient 0.997. The method was validated for accuracy, precision, sensitivity, robustness, ruggedness and all the resulting data treated statistically. The system suitability parameters like retention time, theoretical plates, tailing factor, capacity factor were found within the limit.

scholarly journals Preparation and Hydro-Lipophilic Properties of Methoxylated and Methylated 1-Hydroxynaphthalene-2-Carboxanilides

Proceedings ◽  
2018 ◽  
Vol 9 (1) ◽  
pp. 43 ◽  
Author(s):  
Iva Kapustikova ◽  
Tomas Gonec ◽  
Jiri Kos ◽  
Ewelina Spaczynska ◽  
Michal Oravec ◽  
...  
Keyword(s):  
Mobile Phase ◽  
High Performance ◽  
Chemical Structure ◽  
Reversed Phase ◽  
Log P ◽  
Organic Modifier ◽  
Chromatography Method ◽  
P Values ◽  
Liquid Chromatography Method ◽  
Substituted 1

A series of variously methoxylated and methylated N-aryl-1-hydroxynaphthalene-2-carboxanilides was prepared and characterized as potential anti-invasive agents. As it is known that lipophilicity significantly influences the biological activity of compounds, the hydro-lipophilic properties of these mono-, di- and tri-substituted 1-hydroxynaphthalene-2-carboxanilides are investigated in the study. All the discussed hydroxynaphthalene derivatives were analyzed using the reversed-phase, high-performance liquid chromatography method, to measure lipophilicity. The procedure was performed under isocratic conditions with methanol as an organic modifier in the mobile phase, using an end-capped, non-polar C18 stationary reversed-phase column. The present study discusses the correlations between the logarithm of the capacity factor k and log P/Clog P values, calculated in various ways, as well as the relationships between the lipophilicity and the chemical structure of the studied compounds.

Development of validated method for the determination of exemestane by using RP-HPLC

2018 ◽  
Vol 9 (1) ◽  
pp. 185
Author(s):  
Siva Sai Kiran B ◽  
Raja S
Keyword(s):  
Detection Limit ◽  
Retention Time ◽  
Mobile Phase ◽  
Reversed Phase ◽  
Chromatographic Peak ◽  
Rp Hplc ◽  
Ich Guidelines ◽  
Hplc Grade Water ◽  
Isocratic Mode

A novel RP-HPLC validated method for determination of Exemestane is developed. The chromatographic separation was done on Phenomenex Luna reversed phase C18 (150 mm x 4.6 mm, 5 μm) column in isocratic mode, using Acetonitrile: HPLC grade water (50:50, v/v) as mobile phase at 254 nm wavelength. Exemestane chromatographic peak is eluted with retention time 4.656 min. The linearity range was 5-30 μg/ml with correlation coefficient 0.999. The method was validated as per ICH Guidelines. The quantification and detection limit for estimation of Exemestane was found to be 0.365 and 1.926 μg/ml respectively. Recovery of Exemestane was found in the range of 98.0-102.0%. Keywords: RP-HPLC; Exemestane; Validation; Estimation

Separation of metal-cyanide complexes by reversed-phase ion-interaction high-performance liquid chromatography

1994 ◽  
Vol 72 (2) ◽  
pp. 269-273 ◽  
Author(s):  
Louis Giroux ◽  
Dwight J. Barkley
Keyword(s):  
Ionic Strength ◽  
Mobile Phase ◽  
High Performance ◽  
Reversed Phase ◽  
Organic Modifier ◽  
Experimental Conditions ◽  
Metal Cyanide ◽  
Cyanide Complexes ◽  
Cyano Complexes ◽  
Phase Differences

Reversed-phase ion-interaction chromatography has been used to study the separation of Cu(I), Ag(I), Ni(II), Au(I), Co(III), Fe(III), and Fe(II) cyano complexes on silica and carbon-based reversed-phases with UV detection at 215 nm. Separation of the metal-cyanide complexes was affected by a number of experimental factors including the nature and concentration of the organic modifier, nature and concentration of the ion-pairing reagent, pH, and ionic strength of the mobile phase. Differences between the elution order of metallo-cyanides observed in the present work and in other investigations under similar experimental conditions are explained by a difference in the ionic strength of the mobile phase. Finally, this technique is used to analyze metal-cyanide complexes in a gold mill solution.

Development and Validation of a Reversed-Phase HPLC Method for Determination of Alkaloids from Papaver somniferum L. (Papaveraceae)

2012 ◽  
Vol 95 (2) ◽  
pp. 399-405 ◽  
Author(s):  
Jelena Acevska ◽  
Aneta Dimitrovska ◽  
Gjoshe Stefkov ◽  
Katerina Brezovska ◽  
Marija Karapandzova ◽  
...  
Keyword(s):  
Mobile Phase ◽  
Ph Value ◽  
Reversed Phase ◽  
Hplc Method ◽  
Papaver Somniferum ◽  
Chromatographic Behavior ◽  
Organic Modifier ◽  
Column Temperature ◽  
Development And Validation

Abstract An HPLC method for the separation of six target alkaloids from Papaver somniferum L. (morphine, codeine, oripavine, thebaine, papaverine, and noscapine) was developed, optimized, and validated. The chromatographic behavior of these alkaloids was investigated using a reversed-phase chromatography at acidic and alkaline pH. The effects of ion-pairing agents, pH value of the mobile phase, concentration of the buffer components, mobile phase organic modifier, and column temperature were studied. Regardless of the large differences in their pKa values, all alkaloids were separated within a close retention window, and good peak shape was achieved for each of the six alkaloids. The proposed method has adequate selectivity, linearity, accuracy, precision, and reproducibility and is applicable for poppy straw.

scholarly journals Identification of Flavonoids from the Leaves Extract of Mangrove (Rhizophora apiculata)

2019 ◽  
Vol 5 ◽  
pp. 1
Author(s):  
Asma Nisar ◽  
Awang Bono ◽  
Hina Ahmad ◽  
Ambreen Lateef ◽  
Maham Mushtaq ◽  
...  
Keyword(s):  
Ascorbic Acid ◽  
High Performance Liquid Chromatography ◽  
Gallic Acid ◽  
Retention Time ◽  
Mobile Phase ◽  
High Performance ◽  
Reversed Phase ◽  
Hplc Method ◽  
Rhizophora Apiculata ◽  
Medicinal Properties

A fast and specific reversed-phase high-performance liquid chromatography (HPLC) method was used for the immediate identification of flavonoids (gallic acid, rutin, quercetin, ascorbic acid, and kaempferol) in the leaves extract of Mangrove (Rhizophora apiculata). The R. apiculata has lots of valuable medicinal properties including antiallergic, anti-inflammatory, antimicrobial, antiviral, antioxidant, vascular antitumor activity, and enzyme inhibition; however, the activity of antioxidant is perhaps the greatest studied property attributed to flavonoids. Magnetic stirrer was used for the pretreatment process of sample with methanol by using a temperature of 50°C for 40 min, followed by separation on column size 250 mm x 4.6 mm (5 μm) Hypersil Gold C18 (Thermo Electron Corporation) with water–methanol–acetonitrile (45:40:15 v/v/v) containing acetic acid 1.0% as a mobile phase. Moreover, 254-nm wavelength was used to detect the extract. The standard retention times (Rt) of gallic acid, rutin, ascorbic acid, quercetin, and kaempferol were found to be 2.610, 2.875, 3.150, 5.789, and 8.983, respectively. The existence of gallic acid, rutin, ascorbic acid, kaempferol, and quercetin in Mangrove leaves extract was found matching according to the standard retention time. In Mangrove leaves, gallic acid was found to have the retention time at 2.538, rutin at 2.873, quercetin at 5.796, and kaempferol at 8.976. However, the ascorbic acid was not identified. The amount of rutin, gallic acid, quercetin, and kaempferol was calculated by using the assay formula. In Mangrove leaves, the amount of gallic acid, rutin, quercetin, and kaempferol is 3.024, 5.485, 5.144, and 8.361%, respectively.

Chromatography of Mo(VI) and W(VI) chelates with 2,3-dihydroxynaphthalene

1990 ◽  
Vol 55 (2) ◽  
pp. 372-378
Author(s):  
Milan Vrchlabský ◽  
Naděžda Pollaková ◽  
Aleš Hrdlička
Keyword(s):  
Phosphate Buffer ◽  
Mobile Phase ◽  
Detection Limits ◽  
Reversed Phase ◽  
Ion Pair ◽  
Organic Modifier ◽  
Ion Pair Chromatography ◽  
Counter Ions ◽  
Glass Column ◽  
Tenfold Excess

Mo(VI) and W(VI) were separated in the form of their anionic chelates with 2,3-dihydroxynaphthalene (DHN) by reversed phase ion-pair chromatography. The effect of the organic modifier content and concentration of tetrabutylammonium cations (TBA) in the mobile phase and the effect of concentration of DHN in the injected sample on the separation were studied. The best results were attained by using a mobile phase containing DHN (0.5 mmol dm-3), TBA counter-ions (10 mmol dm-3) and phosphate buffer (50 mmol dm-3) in a medium of 30% (v/v) methanol and 30% (v/v) acetonitrile at pH 7 and by injecting Mo(VI) and W(VI) samples containing DHN in a tenfold excess. On a CGC glass column 150 . 3.3 mm i.d. packed with Separon SGX C18 (5μm), the solutes were separated at resolutions of Rij = 1.0 (DHN-Mo) and 1.6 (Mo-W). The detection limits at 240 nm were 0.5 and 0.2 nmol for Mo(VI) and W(VI), respectively.

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