scholarly journals Green Analytical Methods for the Separation of Seven Antihistamines: Application in Separation of Azelastine and Related Impurities in Nasal Solution

2019 ◽  
Vol 2019 ◽  
pp. 1-11
Author(s):  
Lucas Maciel da Costa ◽  
Heitor Oliveira de Almeida Leite ◽  
Nájla Mohamad Kassab ◽  
Anil Kumar Singh
Keyword(s):  
Gradient Method ◽  
Analytical Methods ◽  
Mobile Phase ◽  
Allergic Reactions ◽  
Organic Residue ◽  
Related Impurities ◽  
Chromatographic Methods ◽  
Highly Efficient ◽  
Water Ph ◽  
Fexofenadine Hcl

Antihistamines are widely used to alleviate the symptoms caused by allergic reactions. Most of these drugs have zwitteriónicas and/or amphoteric characteristics, which confer additional analytical challenges. This work aimed to develop a single eco-friendly and efficient chromatographic methods for analysis of seven antihistamines, namely, azelastine HCl, desloratadine, ebastine, fexofenadine HCl, ketotifen, loratadine, and olopatadine HCl. The separations were obtained using RP C-18 LUNA (150x4.6mm, 5 μm) column. The mobile phase consisted of acetonitrile and acidified water (pH 2.1) in the following proportion: 15:85, v/v for desloratadine, 25:75, v/v for ketotifen and olopatadine, 32:68, v/v for fexofenadine, 35:65, v/v for azelastine and loratadine, and 45:55, v/v for ebastine. All separations were obtained in less than 7.0 min. A prototype method was fully validated and applied in the assay of azelastine HCl in nasal solutions. The proposed methods for analysis of seven antihistamines are highly efficient, selective, and sensitive. Moreover, all methods can be considered excellent in terms of greenness, with total organic residue < 2.5 mL/analysis. An improved gradient method is also described for separation of azelastine HCl and its related impurities.

Identification, Characterization, and Quantification of Impurities of Safinamide Mesilate: Process-Related Impurities and Degradation Products

2017 ◽  
Vol 100 (4) ◽  
pp. 1029-1037 ◽  
Author(s):  
Liang Zou ◽  
Lili Sun ◽  
Hui Zhang ◽  
Wenkai Hui ◽  
Qiaogen Zou ◽  
...  
Keyword(s):  
Degradation Products ◽  
Hplc Method ◽  
Formation Mechanisms ◽  
Stability Indicating ◽  
Related Impurities ◽  
Related Substances ◽  
Water Ph ◽  
Bulk Drug ◽  
First Time

Abstract The characterization of process-related impurities and degradation products of safinamide mesilate (SAFM) in bulk drug and a stability-indicating HPLC method for the separation and quantification of all the impurities were investigated. Four process-related impurities (Imp-B, Imp-C, Imp-D, and Imp-E) were found in the SAFM bulk drug. Five degradation products (Imp-A, Imp-C, Imp-D, Imp-E, and Imp-F) were observed in SAFM under oxidative conditions. Imp-C, Imp-D, and Imp-E were also degradation products and process-related impurities. Remarkably, one new compound, identified as (S)-2-[4-(3-fluoro-benzyloxy) benzamido] propanamide (i.e., Imp-D), is being reported here as an impurity for the first time. Furthermore, the structures of the aforementioned impurities were characterized and confirmed via IR, NMR, and MS techniques, and the most probable formation mechanisms of all impurities proposed according to the synthesis route. Optimum separation was achieved on an Inertsil ODS-3 column (250 × 4.6 mm, 5 μm), using 0.1% formic acid in water (pH adjusted to 5.0) and acetonitrile as the mobile phase in gradient mode. The proposed method was found to be stability-indicating, precise, linear, accurate, sensitive, and robust for the quantitation of SAFM and its process-related substances, including its degradation products.

scholarly journals Robustness evaluation of the chromatographic determination of verapamil hydrochloride

2017 ◽  
Author(s):  
L. S. Logoyda
Keyword(s):  
Analytical Methods ◽  
Mobile Phase ◽  
Chromatographic Method ◽  
Final Analysis ◽  
Chromatographic Determination ◽  
Validation Process ◽  
Verapamil Hydrochloride ◽  
A Value ◽  
Analytical Parameter

The aim of this study was the rubustness evaluation of the chromatographic determination of verapamil hydrochloride using Youden’s test.Methods: Youden’s test is a reliable method to evaluate the robustness of analytical methods, by means of an experiment design which involves seven analytical parameters combined in eight tests. In the present study, we assessed the robustness of a chromatographic method to quantify verapamil hydrochloride using Youden’s test. Hence, it was possible to determine the effect of each analytical parameter in the final analysis results. Youden’s test showed to be a simple and feasible procedure to evaluate the robustness of chromatographic methods.Results: Using the criteria of Youden’s test, the chromato­graphic method showed to be highly robust regarding the verapamil hydrochloride content, when variations in seven analytical parameters were introduced. The highest variation in the verapamil hydrochloride content was 0.26 %, when the concen­tration of triethylamine in the mobile phase was altered; a value considerably low and not significant in routine analyses.Conclusion: Youden’s test showed to be a reliable and useful tool for the robustness evaluation of the chromatographic method for verapamil hydrochloride quantitation. By means of this test, it was possible to evaluate the effect of seven analytical parameters in the final result of the analyses. Therefore, Youden’s test can be successfully applied for the ro­bustness evaluation in validation process of analytical methods by HPLC.

DEVELOPMENT AND VALIDATION OF STABILITY INDICATING RP-HPLC METHOD FOR THE SIMULTANEOUS DETERMINATION OF BERBERINE AND CURCUMIN IN AN AYURVEDIC FORMULATION

INDIAN DRUGS ◽  
2016 ◽  
Vol 53 (08) ◽  
pp. 48-52
Author(s):  
K. P Parekh ◽  
◽  
A. P. Jadhav
Keyword(s):  
Mobile Phase ◽  
Herbal Medicines ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Quality And Safety ◽  
Stability Indicating ◽  
Rp Hplc ◽  
Water Ph ◽  
Development And Validation

A simple, accurate, precise, robust stability indicating RP-HPLC method was developed and validated for simultaneous estimation of berberine and curcumin in an ayurvedic formulation. The two markers were resolved using a C-18 column using as the mobile phase methanol: water (pH 3 adjusted using acetic acid) in the ratio 75:25 V/V at a flow rate of 1mL/min. Retention times of berberine and curcumin were 2.58 ± 0.2 min and 8.5 ± 0.2 min, respectively at 358 nm. Linear response was observed in the concentration range of 2 – 8 ppm for berberine and 5 – 40 ppm for curcumin, with correlation coefficient (r2) of 0.994 and 0.998 for berberine and curcumin, respectively. The developed method was applied for quantitation of markers in marketed and in-house formulations of Gruhadhoomadi Churna. This method can also be used to evaluate formulations containing berberine and curcumin as markers, thus conforming to the need of ensuring quality and safety of herbal medicines.

High resolution and high throughput analytical methods for d-tagatose and process related impurities using capillary electrophoresis

2020 ◽  
Vol 609 ◽  
pp. 113981
Author(s):  
Sri Rama Krishna Surapureddi ◽  
Kunta Ravindhranath ◽  
Ghantasala S. Sameer Kumar ◽  
Prashanth Chiliveri ◽  
Sreedhar Reddy Sappidi
Keyword(s):  
Capillary Electrophoresis ◽  
High Resolution ◽  
High Throughput ◽  
Analytical Methods ◽  
Related Impurities

Stability-Indicating Chromatographic Methods for the Investigation of Ritodrine Hydrochloride Stability and Characterization of the Oxidative Degradation Product

2019 ◽  
Vol 57 (8) ◽  
pp. 730-737
Author(s):  
Noha Salem Rashed ◽  
Ola Mostafa Abdallah ◽  
Ahmed El-Olemy ◽  
Asmaa Ibrahim Hosam Eldin
Keyword(s):  
Degradation Product ◽  
Mobile Phase ◽  
Oxidative Degradation ◽  
Hplc Method ◽  
Pharmaceutical Dosage Form ◽  
Chromatographic Methods ◽  
Ritodrine Hydrochloride ◽  
Accuracy And Precision ◽  
Intact Drug

Abstract Two simple and sensitive chromatographic methods were developed and validated for quantitative determination of ritodrine hydrochloride in presence of its oxidative degradation product. The first method depends on densitomeric determination of thin-layer chromatograms of the intact drug in presence of its oxidative degradate. Excellent separation was achieved at 220 nm using a mobile phase of dichloromethane–methanol–glacial acetic acid (15 : 5 : 0.25, v/v/v). The second was an HPLC method, in which efficient separation was carried out on C18 column (150 × 4.6 × 5 μm) using a mobile phase consisting of water: acetonitrile (70,30, v/v) at a flow rate of 1 mL min−1 and UV detection at 220 nm. Beer’s law was obeyed in the range of 0.025–0.3 μg/spot and 5–40 μg mL−1 of the intact drug using the two methods, respectively. The proposed methods were validated according to International Conference on Harmonization guidelines and successfully applied for the determination of ritodrine hydrochloride in bulk powder, laboratory prepared mixtures and pharmaceutical dosage form with good accuracy and precision. The results obtained were compared with those of the reported method and were found to be in good agreement.

scholarly journals RP-LC method for simultaneous determination of sulfamethoxazole and trimethoprim content in veterinary drugs

2015 ◽  
Vol 40 (1) ◽  
pp. 32 ◽  
Author(s):  
Gabriela Padovani Tahan ◽  
Simone Caetani Machado ◽  
Evandro Conti Malaguti ◽  
Patrícia Penido Maia ◽  
Susanne Rath ◽  
...  
Keyword(s):  
Mobile Phase ◽  
High Performance ◽  
Simultaneous Analysis ◽  
Ultraviolet Detector ◽  
Veterinary Medicines ◽  
Alternative Approach ◽  
Relative Standard ◽  
Water Ph ◽  
Comparison Of The Results

This study describes the development of a method for simultaneous analysis of sulfamethoxazole (SMX) and trimethoprim (TMP) through the use of high-performance liquid chromatography/ultraviolet detector, with the application to veterinary medicines. Satisfactory chromatographic separation of SMX and TMP was isocratically with a C18 column (150 x 4.6 mm, 5 mm). A mobile phase consisting of water, pH 3.5, and methanol (60:40, v/v) was delivered at a flow rate of 1.0 mL min-1 for five minutes and then, increased to 1.8 mL min-1. Detection of the drugs was performed at 213 and 230 nm. Linearity was demonstrated in the range of 5 to 70 mg mL-1 for SMX and 1 to 30 mg mL-1 for TMP (r2 ≥ 0.99 for both compounds). The relative standard deviation was ≤ 5%, and the comparison of the results with the concentrations reported on the drug labels indicated that the quantification was accurate. The resultant stressed samples were analysed by the method. The proposed method shows great potential for simultaneous analysis of the drugs evaluated and represents a new alternative approach to quality control of veterinary medicines.

scholarly journals DEVELOPMENT AND VALIDATION OF METHAMPHETAMINE ANALYSIS IN SALIVA USING GAS CHROMATOGRAPHY-TANDEM MASS SPECTROMETRY

2018 ◽  
Vol 10 (1) ◽  
pp. 97
Author(s):  
Yahdiana Harahap ◽  
Muhammad Rezqi Hakim ◽  
Kuswardani Soedigdo
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Sample Preparation ◽  
Analytical Methods ◽  
Mobile Phase ◽  
Tandem Mass ◽  
Chromatography Tandem Mass Spectrometry ◽  
Validation Criteria ◽  
Inner Diameter ◽  
Development And Validation

Objective: The aim of this study was to develop and validate analytical methods for determining methamphetamine in saliva using gas chromatographytandemmass spectrometry (MS).Methods: The chromatography conditions were DB MS-5 capillary columns with a length of 30 m, inner diameter of 0.25 mm, mobile phase of Heliumgas 99.999%, flow rate of 0.8 mL/min, detection of MS at m/z values of 58.00 and 91.00, respectively, and ephedrine HCl as the internal standard.Results: The validation of analytical methods for methamphetamine satisfies the validation criteria by the EMEA Guidelines 2011. Bioanalyticalmethods obtained were linear in the concentration range from 15.0 to 300.0 ng/mL with r>0.9999. Sample preparation was done using liquid–liquidmicroextraction with cyclohexane, supernatant residue was dried and reconstituted with approximately 100 μL of methanol.Conclusion: The method was successfully applied to saliva samples of methamphetamine users with levels in the range of test.

Green Liquid Chromatographic Methods with Ultraviolet and Tandem Mass Spectrometry Detection: An Application to Ternary Mixture of Paracetamol, Pseudoephedrine, and Cetirizine in Capsules

2020 ◽  
Vol 103 (1) ◽  
pp. 148-155 ◽  
Author(s):  
Souha H Youssef ◽  
Dalia Mohamed ◽  
Maha A Hegazy ◽  
Amr Badawey
Keyword(s):  
Mobile Phase ◽  
Multiple Reaction Monitoring ◽  
Internal Standard ◽  
Hplc Method ◽  
Green Solvents ◽  
Chromatographic Methods ◽  
Combination Methods ◽  
Significant Difference ◽  
Acid Aqueous Solution ◽  
Liquid Chromatographic

Abstract Background: Effective chromatographic methods were developed for the determination of a multicomponent capsule prescribed for treating the common cold. Greening approaches were adopted as opposed to conventional methods. Objectives: Two novel, green chromatographic methods were established to quantitatively analyze the combination. Methods: First, an HPLC/UV method utilizing green solvents (water and ethanol) and acetic acid to adjust pH at 5 was accomplished. The stationary phase was a ZorbaxSB-C18 column (150 × 4.6 mm, 5 μm), and peaks were detected at 215 nm. The second method is a highly sensitive ultra-performance LC (UPLC)-MS/MS method in which the greening approach was established through the reduction of the analysis time (2 min), decreased solvent consumption (flow rate 300 μL/min), and the utilization of a small volume of samples (injection volume 2 μL). The mixture was separated using a UPLC-BEH C18 column (50 × 2.1 mm, 1.7 μm) with an isocratic elution using methanol–0.1% formic acid aqueous solution (60+40, v/v) as mobile phase and utilizing diphenhydramine as an internal standard. Positive-ion electrospray ionization and multiple reaction monitoring were applied for detection. Results: Recovery percentages for paracetamol, pseudoephedrine, and cetirizine were 101.70 ± 0.969, 100.18 ± 1.563, and 99.67 ± 1.429 for the HPLC method and 99.18 ± 1.172, 100.03 ± 0.883, and 99.82 ± 0.912 for the UPLC-MS/MS method, respectively. Conclusions: The proposed methods efficiently analyzed paracetamol, pseudoephedrine, and cetirizine in Allercet Cold® capsules. Validation of the proposed methods was in accordance with the International Conference on Harmonization recommendations, and statistical comparison with the reported method displayed no significant difference regarding accuracy and precision. Highlights: Paracetamol, pseudoephedrine, and cetirizine were successfully quantified using two chromatographic methods. The HPLC method developed is considered green, using water and ethanol as a mobile phase. The UPLC-MS/MS method was rapid and determined the three drugs with accuracy at nanogram levels.

scholarly journals Chemometrically assissted optimization and validation of RP-HPLC method for the analysis of itraconazole and its impurities

2013 ◽  
Vol 63 (2) ◽  
pp. 159-173 ◽  
Author(s):  
Irena Kasagić ◽  
Anđelija Malenović ◽  
Marko Jovanović ◽  
Tijana Rakić ◽  
Biljana Jančić Stojanović ◽  
...  
Keyword(s):  
Mobile Phase ◽  
Hplc Method ◽  
Fractional Factorial ◽  
Pharmaceutical Dosage Forms ◽  
Column Temperature ◽  
Rp Hplc ◽  
Temperature Separation ◽  
Validation Parameters ◽  
Water Ph ◽  
Chromatographic Parameters

This paper presents the chemometrically assisted optimization and validation of the RP-HPLC method intended for the quantitative analysis of itraconazole and its impurities in pharmaceutical dosage forms. To reach the desired chromatographic resolution with a limited number of experiments in a minimum amount of time, Box- -Behnken design was used to simultaneously optimize some important chromatographic parameters, such as the acetonitrile content in the mobile phase, pH of the aqueous phase and the column temperature. Separation between itraconazole and impurity F was identified as critical and selected as a response during the optimization. The set optimal mobile phase composition was acetonitrile/ water pH 2.5 adjusted with o-phosphoric acid (50:50, V/V). Separations were performed on a Zorbax Eclipse XDB-C18, 4.6 × 150 mm, 5 μm particle size column with the flow rate 1 mL min-1, column temperature set at 30 °C and UV detection at 256 nm. The established method was then subjected to method validation and the required validation parameters were tested. For the robustness evaluation, fractional factorial 24-1 design was utilized and factors that might significantly affect the system performance were defined. As other validation parameters were also found to be suitable, the possibility to apply the proposed method for the determination of itraconazole, its impurities B and F in any laboratory under different circumstances has been proven.

Gradient Elution Separation of Main Ingredients from Polygoni Multiflori Extract by HPLC

2013 ◽  
Vol 864-867 ◽  
pp. 503-507
Author(s):  
Tao Wang
Keyword(s):  
Gradient Method ◽  
Mobile Phase ◽  
Separation Efficiency ◽  
Gradient Elution ◽  
Polygonum Multiflorum ◽  
Uv Detector ◽  
Experimental Conditions ◽  
Column Temperature ◽  
Stilbene Glucoside

In this experiment, the main compounds of stilbene glucoside and anthraquinones from polygonum multiflorum extract were separated by HPLC gradient elution. SinoChrom ODS-BP C18 is selected as chromatographic column. The optimal experimental conditions under 254nm wavelength UV detector include the column temperature: 26°C, mobile phase: methanol/water, and flow rate: 1.0ml/mol. The gradient method can be optimized by changing the steepness and shape of gradient elution. Through optimizing gradient method, the separation efficiency is improved within a certain range of gradient elution strength. This article provides important reference for quality control and content determination of fleece-flower root.

Sign in / Sign up

Export Citation Format

Share Document