scholarly journals Development of Micellar HPLC-UV Method for Determination of Pharmaceuticals in Water Samples

2018 ◽  
Vol 2018 ◽  
pp. 1-12 ◽  
Author(s):  
Danielle Cristina da Silva ◽  
Cláudio Celestino Oliveira
Keyword(s):  
Liquid Chromatography ◽  
Mobile Phase ◽  
Solid Phase ◽  
Sodium Dodecyl ◽  
Micellar Liquid Chromatography ◽  
Phase Extraction ◽  
Mobile Phases ◽  
Concentration Factors ◽  
Better Than

Method for extraction and determination of amoxicillin, caffeine, ciprofloxacin, norfloxacin, tetracycline, diclofenac, ibuprofen, nimesulide, levonorgestrel, and 17α-ethynylestradiol exploiting micellar liquid chromatography with PDA detector and solid-phase extraction was proposed. The usage of toxic solvents was low; the chromatographic separation of the medicaments was performed using a C18 column and mobile phases A and B containing 15.0% (v/v) ethanol, 3.0% (m/v) sodium dodecyl sulfate (SDS), and 0.02 mol·L−1 phosphate at pHs 7.0 and 8.0, respectively. The method is simple, selective, and fast, and the analytes were separated in 23.0 min. For extraction, 1000 mL of sample containing 2.0% (v/v) ethanol and 0.002 mol·L−1 citric acid at pH 2.50 was loaded through a 1000 mg of C18 cartridge. The analytes were eluted using 3.0 mL of ethanol, which were evaporated and redissolved in 0.5 mL of mobile phase. Concentration factors better than 1200, except amoxicillin (224), were obtained. The analytical curves were linear (R2 better than 0.992); LOD and LOQ n=10 presented values in the range of 0.019–0.247 and 0.058–0.752 mg·L−1, respectively. Recoveries of 99% were obtained, and the results are in agreement with those obtained by the comparative methods.

scholarly journals Analysis of Some Biogenic Amines by Micellar Liquid Chromatography

2012 ◽  
Vol 2012 ◽  
pp. 1-8 ◽  
Author(s):  
Irena Malinowska ◽  
Katarzyna E. Stępnik
Keyword(s):  
Liquid Chromatography ◽  
Sodium Dodecyl Sulfate ◽  
Biogenic Amines ◽  
Physicochemical Parameters ◽  
Mobile Phase ◽  
Sodium Dodecyl ◽  
Micellar Liquid Chromatography ◽  
Ionic Surfactant ◽  
Mobile Phases ◽  
Dodecyl Sulfate

Micellar liquid chromatography (MLC) with the use of high performance liquid chromatography (HPLC) was used to determine some physicochemical parameters of six biogenic amines: adrenaline, dopamine, octopamine, histamine, 2-phenylethylamine, and tyramine. In this paper, an influence of surfactant’s concentration and pH of the micellar mobile phase on the retention of the tested substances was examined. To determine the influence of surfactant’s concentration on the retention of the tested amines, buffered solutions (at pH 7.4) of ionic surfactant—sodium dodecyl sulfate SDS (at different concentrations) with acetonitrile as an organic modifier (0.8/0.2 v/v) were used as the micellar mobile phases. To determine the influence of pH of the micellar mobile phase on the retention, mobile phases contained buffered solutions (at different pH values) of sodium dodecyl sulfate SDS (at 0.1 M) with acetonitrile (0.8/0.2 v/v). The inverse of value of retention factor () versus concentration of micelles () relationships were examined. Other physicochemical parameters of solutes such as an association constant analyte—micelle ()—and partition coefficient of analyte between stationary phase and water (hydrophobicity descriptor) () were determined by the use of Foley’s equation.

Simultaneous Determination of Floctafenine and its Hydrolytic Degradation Product Floctafenic Acid Using Micellar Liquid Chromatography with Applications to Tablets and Human Plasma

2013 ◽  
Vol 96 (6) ◽  
pp. 1315-1324 ◽  
Author(s):  
Mohamed I Walash ◽  
Fathalla Belal ◽  
Nahed El-Enany ◽  
Manal Eid ◽  
Rania N El-Shaheny
Keyword(s):  
Liquid Chromatography ◽  
Human Plasma ◽  
Degradation Product ◽  
Mobile Phase ◽  
Sodium Dodecyl ◽  
Hydrolytic Degradation ◽  
Direct Determination ◽  
Micellar Liquid Chromatography ◽  
Main Metabolite

Abstract A stability-indicating micellar liquid chromatography (MLC) method was developed and validated for the assay of floctafenine (FLF) in the presence of its degradation product and main metabolite, floctafenic acid (FLA). The analysis was carried out on a CLC Shim-Pack octyl silane (C8) column (150 × 4.6 mm id, 5 μm particle size) using a micellar mobile phase consisting of 0.15 M sodium dodecyl sulfate, 10% n-propanol, and 0.3% triethylamine in 0.02 M orthophosphoric acid (pH = 3). The mobile phase was pumped at a flow rate of 1.0 mL/min with UV detection at 360 nm. The method showed good linearity for FLF and FLA over the concentration ranges of 0.5–25.0 and 0.4–10.0 μg/mL, with LODs of 0.16 and 0.12 μg/mL, respectively. The developed method was successfully applied to the determination of FLF in commercial dispersible tablets, with mean recovery of 98.87 ± 1.37%. Also, the proposed method was specific for the analysis of FLF in presence of the co-formulated drug thiocolchicoside in laboratory-prepared tablets, with mean recovery of 100.50 ± 1.07%. Statistical comparison of the results obtained by the proposed MLC method with those obtained by a comparison method showed good agreement. Moreover, the method was extended to study the degradation behavior of FLF under different International Conference on Harmonization recommended conditions such as alkaline, acidic, oxidative, thermal, and photolytic. The method was further applied for direct determination of FLA as the main metabolite of FLF in human plasma without prior extraction steps, with mean recovery of 110.50 ± 6.5%.

Determination of tizoxanide, the active metabolite of nitazoxanide, by micellar liquid chromatography using a monolithic column. Application to pharmacokinetic studies

2014 ◽  
Vol 6 (21) ◽  
pp. 8682-8689 ◽  
Author(s):  
Shereen Shalan ◽  
Jenny Jeehan Nasr ◽  
Fathalla Belal
Keyword(s):  
Liquid Chromatography ◽  
Active Metabolite ◽  
Mobile Phase ◽  
Monolithic Column ◽  
Sodium Dodecyl ◽  
Micellar Liquid Chromatography ◽  
Pharmacokinetic Studies ◽  
Chromatography Method ◽  
Liquid Chromatography Method

In this study, a micellar liquid chromatography method is proposed for determination of tizoxanide, the active metabolite of nitazoxanide, using a mobile phase consisting of 0.1 M sodium dodecyl sulphate, 8%n-propanol and 0.3% triethylamine in 0.02 M phosphoric acid.

scholarly journals Determination of Lipid Oxidation Level in Broiler Meat by Liquid Chromatography

2004 ◽  
Vol 87 (5) ◽  
pp. 1148-1152 ◽  
Author(s):  
Slavomír Marcinčák ◽  
Jozef Sokol ◽  
Pavel Bystrický ◽  
Peter Popelka ◽  
Peter Turek ◽  
...  
Keyword(s):  
Acetic Acid ◽  
Liquid Chromatography ◽  
Mobile Phase ◽  
Trichloroacetic Acid ◽  
Solid Phase ◽  
Extraction Methods ◽  
Reversed Phase ◽  
Phase Extraction ◽  
Broiler Meat

Abstract An assay was conducted for the determination of malondialdehyde (MDA) levels in broiler meat. The method involves extraction of tissues with trichloroacetic acid (TCA) and reaction of the TCA extract with 2,4-dinitrophenylhydrazine (DNPH). After separation of the MDA-DNPH complex using a solid-phase extraction C18 column, samples were eluted with 1 mL acetonitrile. Aliquots of 20 μL acetonitrile were analyzed by liquid chromatography on reversed-phase C18 column (3 μm) with UV detection. The products were eluted isocratically with the mobile phase containing acetonitrile–water–acetic acid (39 + 61 + 0.2, v/v/v). The retention time was for MDA-DNPH was 6.5 min, and the detection limit was 3.5 μg/kg. Two extraction methods (cold and hot) were also used in the study. The results showed that hot extraction increased results about 55.8% and recovery from samples spiked with 116.6 μg/kg was lower (74.6%) in comparison with cold extraction (94.7%).

Sign in / Sign up

Export Citation Format

Share Document