Effect of the aqueous component of the mobile phase on RP-TLC retention and its implication in the determination of lipophilicity for a series of structurally diverse drugs

2006 ◽  
Vol 19 (108) ◽  
pp. 151-156 ◽  
Author(s):  
Costas Giaginis ◽  
Demetris Dellis ◽  
Anna Tsantili-Kakoulidou
2019 ◽  
Vol 9 (o3) ◽  
Author(s):  
Imad Tarek Hanoon ◽  
Abed Mohammed Daheir AL-Joubory 2 ◽  
Marwa Mohamed Saied 3

A simple , specific, accurate and precise RP-HPLC method was developed for determination of Irbesartan (IRB) in pharmaceutical dosage forms in tablets products and sachet using symmetry (L 1 ) column at 30°C . The signal was detected at 225 nm. A mobile phase dissolve 0.5 g of buffer potassium phosphate in 100 ml distilled water and adjust pH 2.7 , methanol and acetonitrile at ratio (40 :30 :30 ) . and flow rate 1.2ml/min -1 at pH=7.2 a mobile phase The percent recovery was detected 101 % and the linearity of concentration was 10-50 µg.ml -1 and supported this method by using (FT.I.R.) spectrum method for organic spectrophotometer to prove the chemical structure of this drug and some physical properties . we are obtained the result is identical of other literature . The proposed method was applied successfully for determination of the IRB in tablets products.


2018 ◽  
Vol 8 (4) ◽  
pp. 42-47
Author(s):  
Tien Nguyen Huu ◽  
Tram Le Thi Bao ◽  
Ngoc Nguyen Thi Nhu ◽  
Thang Phan Phuoc ◽  
Khan Nguyen Viet

Background: Curcumin is a major ingredient in turmeric (Curcuma longa L., Zingiberaceae), which has important activities such as anti-tumor, anti-inflammatory, antioxidant, anti-ischemia, protection of gastric mucosa etc,. Curcumin can be considered as a biological marker of turmeric and turmeric products. Objectives: Developing an HPLC method for quantification of curcumin in turmeric powder and turmeric - honey ball pills; applying this method for products on the market. Materials and methods: turmeric powder and turmeric - honey ball pills collected in Thua Thien Hue province. After optimization process, the method was validated and applied to evaluate the content of curcumin. Results: The chromatography analysis was performed with: Zorbaz Eclipse XDB-C18 (150 × 4.6 nm; 5 µm); Mobile phase: acetonitril: 2% acetic acid (45:55), Flow rate was kept constant at 1.0 ml/min; Detector PDA (420 nm). The method was validated for the HPLC system compatibility, specificity, linearity range, precision and accuracy; the recovery greater than 98%. Conclusion: The developed HPLC method can determine curcumin in turmeric powder and turmeric - honey ball pills. Key words: Curcumin, turmeric powder, turmeric-honey ball pills, quantitative determination, HPLC


2019 ◽  
Vol 70 (6) ◽  
pp. 2015-2020
Author(s):  
Silvia Robu ◽  
Aurelia Romila ◽  
Olimpia Dumitriu Buzia ◽  
Adrian Florin Spac ◽  
Camelia Diaconu ◽  
...  

Numerous articles on Salvia officinalis L. have been published regarding the composition of their essential oil. The considerable variation found may be due to the quality of the plant material as well as to the methods used for analysis. A simple GC-MS method was developed and optimized in the QbD approach, for the determination of sage essential oils. The optimization of GC-MS analysis was performed using different mobile phase flows, injection volumes, split ratios and temperature programs. The optimized method proved to be simple and can be successfully applied for the determination of sage essential oils.


2018 ◽  
Vol 69 (3) ◽  
pp. 627-631 ◽  
Author(s):  
Viorica Ohriac (Popa) ◽  
Diana Cimpoesu ◽  
Adrian Florin Spac ◽  
Paul Nedelea ◽  
Voichita Lazureanu ◽  
...  

Pain is defined as a disagreeable sensory and emotional experience related to a tissue or potential lesion. Paracetamol (Acetaminophen) is the most used non-morphine analgesic. For the determination of paracetamol we developed and validated the high performance liquid chromatography (HPLC) analysis using a Dionex Ultimate 3000 liquid chromatograph equipped with a multidimensional detector. After determining the optimum conditions of analysis (80/20 water / acetonitrile mobile phase, flow rate 1.0 mL / min, detection wavelength 245 nm) we validated the method following the following parameters: linearity of response function, linearity of results, limit (LD = 0.66 mg / mL) and quantification limit (LQ = 2.00 mg / mL), and precision. The method of determining paracetamol by HPLC was applied to 30 samples of serum collected from patients who had pain and were treated with paracetamol.


2018 ◽  
Vol 69 (2) ◽  
pp. 297-299
Author(s):  
Adriana Nita ◽  
Delia Mirela Tit ◽  
Lucian Copolovici ◽  
Carmen Elena Melinte (Frunzulica) ◽  
Dana Maria Copolovici ◽  
...  

The aim of this study was to develop and validate a rapid, accurate, and exact method for the quantitative determination of famotidine in pharmaceutical products. The HPLC analyses were performed by using a mobile phase containing methanol:1% acetic acid solution=30:7 (v/v), at a flow rate of 0.4 mL/min.The total time of the method was 10 min, and the retention time of famotidine was 4.16 min. The detection was evaluated at l=267 nm. The method has been validated by using different validation parameters. The linear response of the detector for famotidine peak area was observed at concentrations ranging from 0.1 to 0.0001 mg mL-1 , resulting in a correlation coefficient of 0.99998. The values of the detection limit and of the quantification limit are 0.00048 mg mL-1 and 0.00148 mg mL-1, respectively. The method proposed allowed accurate (with a relative error of less than 2%) and precise (RSD values less than 2.0%) determination of famotidine content in pharmaceutical products and can be used for its rapid quantitative analysis.


2020 ◽  
Vol 16 (7) ◽  
pp. 976-987
Author(s):  
Jakub Petřík ◽  
Jakub Heřt ◽  
Pavel Řezanka ◽  
Filip Vymyslický ◽  
Michal Douša

Background: The present study was focused on the development of HPLC method for purity testing of sofosbuvir by the Design of Experiments and determination of the activation energy of hydrolytic degradation reactions of sofosbuvir using HPLC based on the kinetics of sofosbuvir degradation. Methods: Following four factors for the Design of Experiments were selected, stationary phase, an organic modifier of the mobile phase, column temperature and pH of the mobile phase. These factors were examined in two or three level experimental design using Modde 11.0 (Umetrics) software. The chromatographic parameters like resolution, USP tailing and discrimination factor were calculated and analysed by partial least squares. The chromatography was performed based on Design of Experiments results with the mobile phase containing ammonium phosphate buffer pH 2.5 and methanol as an organic modifier. Separation was achieved using gradient elution on XBridge BEH C8 at 50 °C and a flow rate of 0.8 mL/min. UV detection was performed at 220 nm. The activation energy of hydrolytic degradation reactions of sofosbuvir was evaluated using two different calculation methods. The first method is based on the slope of dependence of natural logarithm of the rate constant on inverted thermodynamic temperature and the second approach is the isoconversional method. Results and Conclusion: Calculated activation energies were 77.9 ± 1.1 kJ/mol for the first method and 79.5 ± 3.2 kJ/mol for the isoconversional method. The results can be considered to be identical, therefore both calculation methods are suitable for the determination of the activation energy of degradation reactions.


2018 ◽  
Vol 15 (1) ◽  
pp. 32-38 ◽  
Author(s):  
Bürge Aşçı ◽  
Mesut Koç

Introduction:This paper presents the development and validation of a novel, fast, sensitive and accurate high performance liquid chromatography (HPLC) method for the simultaneous quantitative determination of dibucaine HCl, fluocortolone pivalate and fluocortolone caproate in pharmaceutical preparations.Experiment:Development of the chromatographic method was based on an experimental design approach. A five-level-three-factor central composite design requiring 20 experiments in this optimization study was performed in order to evaluate the effects of three independent variances including mobile phase ratio, flow rate and amount of acid in the mobile phase.Conclusion:The optimum composition for mobile phase was found as a methanol:water:acetic acid mixture at 71.6 : 26.4 : 2 (v/v/v) ratio and optimum separation was acquired by isocratic elution with a flow rate of 1.3 mL/min. The analytes were detected using a UV detector at 240 nm. The developed method was validated in terms of linearity, precision, accuracy, limit of detection/quantitation and solution stability and successfully applied to the determination of dibucaine HCl, fluocortolone pivalate and fluocortolone caproate in pharmaceutical topical formulations such as suppositories and ointments.


2019 ◽  
Vol 15 (6) ◽  
pp. 635-641
Author(s):  
Nadia M. Mostafa ◽  
Ghada M. Elsayed ◽  
Nagiba Y. Hassan ◽  
Dina A. El Mously

Background:The concept of green analytical chemistry prevails due to the growing environmental pollution.Objective:Our attempts are to develop simple and eco-friendly method which is non-harmful to the environment by producing minimal waste. In this context, a green liquid chromatographic method was applied for the simultaneous determination of chlorpheniramine maleate, pseudoephedrine hydrochloride and propyphenazone in their combined dosage form.Methods:Separation was carried out using X select HSS RP C18 analytical column (250 × 4.6 mm, 5μm) using methanol - 0.02 M phosphate buffer pH 3 - triethylamine (60:40: 0.1, by volume) as a mobile phase. The separated peaks were detected at 215 nm at a flow rate 1.0 mL/min.Results:Quantification was done over the concentration ranges of 1-25 µg/mL for chlorpheniramine maleate, 5-35 µg/mL for pseudoephedrine hydrochloride and 10-120 µg/mL for propyphenazone. The suggested method was validated with regard to linearity, accuracy and precision according to the International Conference on Harmonization guidelines with good results.Conclusion:It could be used as a safer alternative for routine analysis of the mentioned drugs in quality control laboratories.


1984 ◽  
Vol 49 (10) ◽  
pp. 2349-2354 ◽  
Author(s):  
František Vláčil ◽  
Karel Koňák

The selectivity coefficients of the nitrate and chloride ions and of anionic chloro complexes of Au(III), Rh(III), Pd(II), and Pt(IV) for ion exchange on Spheron DEAE in the chloride form are determined by the dynamic method. the complex anion species formed are identified and the ion exchange nature of the sorption of precious metals on this sorbent is confirmed based on the elution order of the precious metals as determined previously by the column chromatography on Spheron DEAE using hydrochloric acid as the mobile phase. The effect of the presence of perchlorate in the mobile phase during the liquid chromatography of precious metals and during the chromatographic determination of nitrate traces is explained.


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