Ultra-Performance Liquid Chromatographic and Densitometric Methods for Sensitive Determination of Xipamide and Triamterene in Pure and Pharmaceutical Dosage Forms

2021 ◽  
Author(s):  
N V Fares ◽  
Haitham A El Fiky ◽  
Amr M Badawey ◽  
Maha F Abd El Ghany
Keyword(s):  
Acetic Acid ◽  
Flow Rate ◽  
Mobile Phase ◽  
Dosage Forms ◽  
Hplc Method ◽  
Uv Detection ◽  
Pharmaceutical Dosage Forms ◽  
Selective Determination ◽  
Liquid Chromatographic

Abstract Background Validated UPLC method and TLC densitometric method were prescribed for determination of antihypertensive components. Objectives: To establish and validate rapid and accurate Ultra performance liquid chromatographic (UPLC) and TLC densitometric methods for determination of Xipamide and Triamterene in pure and dosage forms. Methods The first method; UPLC method, depended on using Agilent Zorbax Eclipse Plus C8 (50 mm × 2.1 mm, 1.8 μm), as the column, mobile phase composed of (acetonitrile-water) (70 + 30, v/v) adjusted by acetic acid to obtain (pH 3), 0.2 mL/min flow rate and UV detection at 231.4 nm. The second method was a thin layer chromatography (TLC) densitometric method, separation was achieved by using toluene-methanol-ethyl chloride-acetic acid (7 + 2 + 1 + 0.2, v/v/v) as the mobile phase, pre coated silica gel plates as the stationary phase and UV detection at 300.0 nm. Results The obtained results were validated and statistically compared with official and reported methods. The obtained results showed high accuracy and reproducible results with excellent mean recoveries for both drugs. Conclusions The UPLC method showed shorter retention time for both Xipamide (0.88 min) and Triamterene (0.63 min), lower detection limit less than 0.055 µg/mL for both drugs with high selectivity, decreased injection volume (1 µL) and lower flow rate other than any HPLC method. Both proposed methods were sensitive, selective, and effectively applied to pure and dosage forms (Epitens®). Highlights Unprecedented sensitive, rapid, and reproducible UPLC and TLC methods were developed for selective determination of mixture of Xipamide and Triamterene with LOD less than 0.076 µg/mL for both drugs.

scholarly journals RP-HPLC Determination of Raloxifene in Pharmaceuticl Tablets

2006 ◽  
Vol 3 (1) ◽  
pp. 60-64 ◽  
Author(s):  
P. Venkata Reddy ◽  
B. Sudha Rani ◽  
G. Srinu Babu ◽  
J. V. L. N. Seshagiri Rao
Keyword(s):  
Flow Rate ◽  
Retention Time ◽  
Mobile Phase ◽  
Dosage Forms ◽  
Hplc Method ◽  
Reverse Phase Hplc ◽  
Reverse Phase ◽  
Pharmaceutical Dosage Forms ◽  
Rp Hplc

A reverse phase HPLC method is developed for the determination of Raloxifene in pharmaceutical dosage forms. Chromatography was carried out on an inertsil C18 column using a mixture of acetonitrile and phosphate buffer (30:70 v/v) as the mobile phase at a flow rate of 1 mL/min. Detection was carried out at 290 nm .The retention time of the drug was 10.609 min. The method produced linear responses in the concentration range of 0.5-200 µg/mL of Raloxifene. The method was found to be applicable for determination of the drug in tablets.

scholarly journals Estimation of Ziprasidone Hydrochloride Monohydrate in Bulk and Capsules by Reverse Phase HPLC

2006 ◽  
Vol 3 (3) ◽  
pp. 169-172 ◽  
Author(s):  
B. Sudha Rani ◽  
P. Venkata Reddy
Keyword(s):  
Flow Rate ◽  
Phosphate Buffer ◽  
Mobile Phase ◽  
Dosage Forms ◽  
Hplc Method ◽  
Reverse Phase Hplc ◽  
Reverse Phase ◽  
Pharmaceutical Dosage Forms ◽  
Hydrochloride Monohydrate

A reverse phase HPLC method is described for the determination of Ziprasidone HCl mono hydrate in bulk and pharmaceutical dosage forms. Chromatography was carried out on an ODS C18 column using a mixture of methanol and phosphate buffer (55:45v/v) as the mobile phase at a flow rate of 1mL/min. Detection was carried out at 314nm. The retension time of the drug was 4.522 min. The method produced linear responses in the concentration range of 0.5-30 μg /mL of Ziprasidone HCl mono hydrate.The method was found to be applicable for determination of the drug in capsules.

scholarly journals Selective Determination of Diazinon and Chlorpyrifos in the Presence of Their Degradation Products: Application to Environmental Samples

2018 ◽  
Vol 101 (4) ◽  
pp. 1191-1197 ◽  
Author(s):  
Mamdouh R Rezk ◽  
Abd El-Aziz B Abd El-Aleem ◽  
Shaban M Khalile ◽  
Omneya K El-Naggar
Keyword(s):  
Flow Rate ◽  
Environmental Samples ◽  
Mobile Phase ◽  
Degradation Products ◽  
Hplc Method ◽  
Stress Conditions ◽  
Uv Detection ◽  
Selective Determination ◽  
International Conference

Abstract An accurate, sensitive, and selective HPLC method was developed and validated for the determination of diazinon and chlorpyrifos. These pesticides were subjected to different stress conditions, such as acidic, alkaline, oxidative, thermal, and photolytic hydrolysis. The proposed method used a C18 Eclipse Plus column (100 × 4.6 mm, 3.5 µm) and a mobile phase consisting of acetonitrile–water (70 + 30, v/v) in an isocratic separation mode. The flow rate was 1.5 mL/min, with UV detection at 247 and 230 nm for diazinon and chlorpyrifos, respectively. The proposed method was linear over the range of 0.40–50.00 µg/mL for diazinon and 0.40–40.00 µg/mL for chlorpyrifos. The proposed method was validated per International Conference on Harmonization guidelines and subsequently applied for the successful determination of the studied pesticides in bulk form in their commercial samples in the presence of their degradation products. The developed method was used for the determination of the residues of these pesticides in lavender and rosemary leaves that were pretreated with the recommended doses of these pesticides.

scholarly journals Development and application of a validated HPLC method for the analysis of dissolution samples of mexiletine hydrochloride capsules

2010 ◽  
Vol 75 (7) ◽  
pp. 975-985 ◽  
Author(s):  
Dragan Milenovic ◽  
Zoran Todorovic
Keyword(s):  
Flow Rate ◽  
Mobile Phase ◽  
Hplc Method ◽  
Uv Detection ◽  
In Vitro Dissolution ◽  
Selective Method ◽  
Dissolution Studies ◽  
Detection And Quantification

The aim of this work was to develop and validate a simple, efficient, sensitive and selective method for the analysis of dissolution samples of mexiletine hydrochloride capsules by HPLC without the necessity of any time-consuming extraction, dilution or evaporation steps prior to drug assay. Separation was performed isocratically on a 5 ?m LiChrospher 60, RP-Select B column (250 x 4 mm ID) using the mobile phase buffer-acetonitrile (60:42, v/v) at a flow rate of 1.2 mL min-1 and UV detection at 262 nm. The elution occurred in less than 10 minutes. The assay was linear in the concentration range 50-300 ?g mL-1 (r2 = 0.9998). The validation characteristics included accuracy, precision, linearity, specificity, limits of detection and quantification, stability, and robustness. Validation acceptance criteria were met in all cases (the percent recoveries ranged between 100.01 and 101.68 %, RSD < 0.44 %). The method could be used for the determination of mexiletine hydrochloride and for monitoring its concentration in in vitro dissolution studies.

scholarly journals Validated RP-HPLC Method for the Determination of Ivabradine Hydrochloride in Pharmaceutical Formulation

2017 ◽  
Vol 9 (05) ◽  
Author(s):  
MD. Muzaffar -ur- Rehman1 ◽  
G. Nagamallika
Keyword(s):  
Mobile Phase ◽  
Dosage Forms ◽  
Hplc Method ◽  
Pharmaceutical Formulation ◽  
Intermediate Precision ◽  
Pharmaceutical Dosage Forms ◽  
Rp Hplc ◽  
Ich Guidelines ◽  
Bulk Drug

A simple, rapid, precise, and accurate RP-HPLC method for the estimation of Ivabradine Hydrochloride an anti-anginal agent, both as a bulk drug and in pharmaceutical formulation was developed. The chromatographic separation was achieved on a Thermosil C18 150 × 4.5 mm, 5μm column by using a mobile phase containing a mixture of methanol and phosphate buffer pH 6.5 in the ratio of 65:35 % v/v at a flow rate of 1ml/min and at an ambient temperature. The detection was monitored at a wavelength of 265nm. A clear chromatographic peak was identified with the retention time of 4.36 min and tailing factor of 1.23. The developed method was validated according to ICH guidelines with respect to specificity, linearity, accuracy, precision and robustness. The method shows a good linear relationship with correlation co-efficient of more than 0.992 in the concentration range of 30μg-150μg. The method showed mean % Recovery of 100.4% and %RSD for repeatability and intermediate precision was less than 2%. The proposed method can be used successfully for the quantitative determination of Ivabradine HCL in pharmaceutical dosage forms.

scholarly journals Optimization of RP-HPLC method with UV detection for determination of ursodeoxycholic acid in pharmaceutical formulations

2020 ◽  
Vol 66 (1) ◽  
pp. 85-90
Author(s):  
Zhaklina Poposka Svirkova ◽  
Zorica Arsova-Sarafinovska ◽  
Aleksandra Grozdanova
Keyword(s):  
Ursodeoxycholic Acid ◽  
Flow Rate ◽  
Mobile Phase ◽  
Pharmaceutical Formulations ◽  
Gradient Elution ◽  
Hplc Method ◽  
Uv Detection ◽  
Rp Hplc ◽  
Ich Guidelines

Due to the low absorptivity of bile acids, the aim of this study was to develop and validate a simple and sensitive HPLC/UV method for quantification of ursodeoxycholic acid (UDCA) in pharmaceutical formulations. Effective separation was achieved on C18 end–capped column, with gradient elution of a mobile phase composed of 0.001 M phosphate buffer (pH 2.8±0.5) – acetonitrile mix, at flow rate 1.5 mL min-1, UV detection at 200 nm and injection volumes were 50 µL. The proposed HPLC method was fully validated according to the ICH guidelines and it was found to be simple, accurate, precise and robust. Key words: ursodeoxycholic acid, HPLC/UV, pharmaceutical formulations, validation

Liquid Chromatographic Determination of Acetic Acid in Foods

1984 ◽  
Vol 67 (5) ◽  
pp. 885-887
Author(s):  
Samy H Ashoor ◽  
Jim Welty
Keyword(s):  
Acetic Acid ◽  
Flow Rate ◽  
Mobile Phase ◽  
Chromatographic Determination ◽  
Uv Detector ◽  
Coefficients Of Variation ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract A liquid chromatographic (LC) method has been developed for the determination of acetic acid in vinegar and other foods. The LC system includes an Aminex HPX-87H column and a UV detector set at 210 nm. The mobile phase is 0.009N H2S04 at a flow rate of 0.7 mL/min. The method is simple and specific for acetic acid. Recoveries of acetic acid from a variety of products ranged from 93.3 to 102% with coefficients of variation from 2.4 to 4.6%.

scholarly journals Development and Validation of an HPLC Method for Determination of Ziprasidone and Its Impurities in Pharmaceutical Dosage Forms

2011 ◽  
Vol 94 (3) ◽  
pp. 713-722 ◽  
Author(s):  
Marija Pavlovic ◽  
Marija Malesevic ◽  
Katarina Nikolic ◽  
Danica Agbaba
Keyword(s):  
Mobile Phase ◽  
Raw Materials ◽  
Dosage Forms ◽  
Hplc Method ◽  
Array Detector ◽  
Least Squares Regression ◽  
Experimental Conditions ◽  
Pharmaceutical Dosage Forms ◽  
Development And Validation

Abstract Ziprasidone is known as a novel “atypical” or “second-generation” antipsychotic drug. A sensitive and reproducible method was developed and validated for determination of ziprasidone and its major impurities, which are significantly different in polarity. The separation is performed on a Waters Spherisorb® octadecylsilyl 1 column (5.0 μm particle size, 250 × 4.6 mm id) using a gradient with mobile phase A [buffer–acetonitrile (80 + 20, v/v)] and mobile phase B [buffer–acetonitrile (10 + 90, v/v)] at a working temperature of 25°C. The buffer was 0.05 M KH2PO4 solution with an addition of 10 mL triethylamine/L solution, adjusted to pH 2.5 with orthophosphoric acid. The flow rate was 1.5 mL/min, and the eluate was monitored at 250 nm using a diode array detector. Optimization of the experimental conditions was performed using partial least squares regression, for which four factors were selected for optimization: buffer concentration, buffer pH, triethylamine concentration, and temperature. The proposed validated method is convenient and reliable for the assay and purity control in both raw materials and dosage forms.

scholarly journals Isocratic RP-HPLC Method for Simultaneous Separation and Estimation of Zofenopril and Hydrochlorthiazide in Pharmaceutical Dosage Forms

2012 ◽  
Vol 9 (2) ◽  
pp. 999-1006 ◽  
Author(s):  
G. S. Devika ◽  
M. Sudhakar ◽  
J. Venkateshwara Rao
Keyword(s):  
Mobile Phase ◽  
High Performance ◽  
Sodium Hydroxide Solution ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Pharmaceutical Dosage Forms ◽  
Rp Hplc ◽  
Simultaneous Separation ◽  
Liquid Chromatographic

A simple, rapid, sensitive and accurate isocratic reverse phase high performance liquid chromatographic (RP-HPLC) method has been developed and subsequently validated for the simultaneous determination of Zofenopril and Hydrochlorthiazide in combined dosage form. Chromatographic separation of the two drugs was performed on a Purospher BDS C18 column (250 mm × 4.6 mm id, 5 μm particle size). The mobile phase comprising of acetonitrile methanol: 0.02M NaH22PO4buffer (40:20:40) was delivered at a flow rate of 1.0mL/min. The pH of the mobile phase is adjusted to 7.2 with Sodium hydroxide solution. Detection was performed at 245 nm.The separation was completed within 10 min and the retention time of hydrochlorthiazide is 4.62 and Zofenopril is 6.86 min respectively. Calibration curves were linear with R2between 0.99-1.0 over a concentration range of 100-600 μg/ml for Zofenopril calcium and 50-300 μg/ml for hydrochlorthiazide..The developed method was successfully applied to determi

scholarly journals Simultaneous Identification and Quantification of Anthraquinones, Polydatin, and Resveratrol in Polygonum multiflorum, Various Polygonum Species, and Dietary Supplements by Liquid Chromatography and Microscopic Study of Polygonum Species

2007 ◽  
Vol 90 (6) ◽  
pp. 1532-1538 ◽  
Author(s):  
Bharathi Avula ◽  
Vaishali C Joshi ◽  
Yan-Hong Wang ◽  
Ikhlas A Khan
Keyword(s):  
Acetic Acid ◽  
Mobile Phase ◽  
High Performance ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Polygonum Multiflorum ◽  
Relative Standard ◽  
Simultaneous Identification ◽  
Liquid Chromatographic

Abstract A high-performance liquid chromatographic (HPLC) method with ultraviolet absorption detection was developed to determine the presence of anthraquinones, polydatin, and resveratrol in Polygonum multiflorum Thunb. as well as other medicinal Polygonum species, viz., P. cuspidatum, P. oriental, P. aviculare, and P. vulgare, as well as commercial products that claim to contain P. multiflorum. The best results were obtained with a Phenomenex Gemini C18 column using gradient mobile phase composed of water (0.1 acetic acid) and acetonitrile (0.1 acetic acid). Elution was at a flow rate of 1.0 mL/min. The detection wavelength was 280 nm for anthraquinones and 320 nm for polydatin and resveratrol. The main anthraquinones identified were emodin and physcion. The HPLC pattern of P. multiflorum was also compared with 5 other species of Polygonum. The method was validated for precision, repeatability, and accuracy. The relative standard deviation was between 0.9 and 1.6. The method was sensitive, quick, and accurate for determination of anthraquinones, polydatin, and resveratrol in 6 different species of Polygonum and can be used for quality control of P. multiflorum. The commercial samples and the 6 Polygonum species were compared microscopically, and a detailed description is provided for P. multiflorum.

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