scholarly journals Simultaneous HPLC Determination of Chlordiazepoxide and Mebeverine HCl in the Presence of Their Degradation Products and Impurities

2015 ◽  
Vol 2015 ◽  
pp. 1-9
Author(s):  
Rania N. El-Shaheny ◽  
Fathalla F. Belal
Keyword(s):  
Simultaneous Determination ◽  
Degradation Product ◽  
Mobile Phase ◽  
Degradation Products ◽  
Potassium Dihydrogen Phosphate ◽  
Hplc Method ◽  
Dihydrogen Phosphate ◽  
Ir Studies ◽  
Validation Procedure

A simple, rapid, and sensitive RP-HPLC method was developed and validated for the simultaneous determination of chlordiazepoxide (CDO) and mebeverine HCl (MBV) in the presence of CDO impurity (2-amino-5-chlorobenzophenone, ACB) and MBV degradation product (veratric acid, VER). Separation was achieved within 9 min on a BDS Hypersil phenyl column (4.5 mm × 250 mm, 5 µm particle size) using a mobile phase consisting of acetonitrile: 0.1 M potassium dihydrogen phosphate: triethylamine (35 : 65 : 0.2, v/v/v) in an isocratic mode at a flow rate of 1 mL/min. The pH of the mobile phase was adjusted to 4.5 with orthophosphoric acid and UV detection was set at 260 nm. A complete validation procedure was conducted. The proposed method exhibited excellent linearity over the concentration ranges of 1.0–100.0, 10.0–200.0, 2.0–40.0, and 2.0–40.0 µg/mL for CDO, MBV, VER, and ACB, respectively. The proposed method was applied for the simultaneous determination of CDO and MBV in their coformulated tablets with mean percentage recoveries of 99.75 ± 0.62 and 98.61 ± 0.38, respectively. The results of the proposed method were favorably compared with those of a comparison HPLC method using Studentt-test and the variance ratioF-test. The chemical structure of MBV degradation product was ascertained by mass spectrometry and IR studies.

scholarly journals Simultaneous Determination of Matrine and Tinidazole in Compound Lotion by RH-HPLC Method

2013 ◽  
Vol 2013 ◽  
pp. 1-5 ◽  
Author(s):  
Zhikui Yin ◽  
Suying Ma ◽  
Jincai Wang ◽  
Xiaojun Shang
Keyword(s):  
Simultaneous Determination ◽  
Mobile Phase ◽  
Potassium Dihydrogen Phosphate ◽  
Hplc Method ◽  
Dihydrogen Phosphate ◽  
Uv Detector ◽  
Potassium Dihydrogen ◽  
Rp Hplc ◽  
Detector Method

A simple, sensitive, and accurate RP-HPLC coupled with UV detector method was developed and validated for simultaneous determination of matrine and tinidazole in compound lotion. The chromatographic separation of the two compounds was carried out with a SinoChoom ODS-BP C18column (5 μm, 4.6 mm × 200 mm) analytical column, using a mobile phase consisting of 0.025 mol/L potassium dihydrogen phosphate (containing triethylamine 0.05%, v/v) and acetonitrile (80 : 20, v/v) at a flow rate of 1.0 mL/min. The detection was monitored at 210 and 310 nm for matrine and tinidazole, respectively. Total run time was 12 min, and the column was maintained at 25°C. The excipients in the compound lotion did not interfere with the drug peaks. The calibration curves of matrine and tinidazole were fairly linear over the concentration ranges of 10.0–100.0 μg/mL (r=0.9954) and 20.0–200.0 μg/mL (r=0.9968), respectively. The RSD of both the intraday and interday variations was below 1.5% for matrine and tinidazole. The proposed HPLC method was validated according to International Conference on Harmonisation and proved to be suitable for the simultaneous determination of matrine and tinidazole in compound lotion.

scholarly journals Different Stability-Indicating Chromatographic Techniques for the Determination of Netobimin

2012 ◽  
Vol 2012 ◽  
pp. 1-8
Author(s):  
Nesrin K. Ramadan ◽  
Afaf O. Mohamed ◽  
Sara E. Shawky ◽  
Maissa Y. Salem
Keyword(s):  
Degradation Product ◽  
Mobile Phase ◽  
Potassium Dihydrogen Phosphate ◽  
Ammonium Hydroxide ◽  
Hplc Method ◽  
Dihydrogen Phosphate ◽  
Potassium Dihydrogen ◽  
Product Method ◽  
The Mean

Two simple, accurate, and sensitive methods were developed for the determination of netobimin in the presence of its degradation product. Method (A) was an HPLC method, performed on C18 column using acetonitrile/methanol/0.01 M potassium dihydrogen phosphate (56 : 14 : 30 by volume) as a mobile phase with a flow rate of 0.5 mL/min. Detection was performed at 254 nm. Method (B) was a TLC method, using silica gel 60 F254plates; the optimized mobile phase was toluene/methanol/chloroform/ammonium hydroxide (5 : 4 : 6 : 0.1 by volume). The spots were scanned densitometrically at 346 nm. Linearity ranges were 1–10 μg/mL for method (A) and 0.5–5 μg/band for method (B), and the mean percentage recoveries were99.3±0.7% and99.7±0.7% for methods (A) and (B), respectively. The proposed methods were found to be specific for netobimin in the presence of up to 90% of its degradation product. Statistical comparison between the results obtained by these methods and the manufacturer method was done, and no significance difference was obtained.

scholarly journals Development and validation of a reversed-phase HPLC method for determination of assay content of Teriflunomide by the aid of BOMD simulations

2021 ◽  
pp. 281-294 ◽  
Author(s):  
Abolghasem Beheshti ◽  
Zahra Kamalzadeha ◽  
Monireh Haj-Maleka ◽  
Meghdad Payaba ◽  
Mohammad Amin Rezvanfar ◽  
...  
Keyword(s):  
Mobile Phase ◽  
Potassium Dihydrogen Phosphate ◽  
Active Pharmaceutical Ingredient ◽  
Reversed Phase ◽  
Hplc Method ◽  
Dihydrogen Phosphate ◽  
Td Dft ◽  
High Level ◽  
Development And Validation

Due to the new hopes for treatment of multiple sclerosis (MS) diseases by Teriflunomide (TFN), in this project, a cheap, robust, and fully validated method has been developed both for determination of assay content in API (active pharmaceutical ingredient), and for related impurities analysis (RIA). To operate the method, a common C18, end-capped (250 × 4.6) mm, 5µm liquid chromatography column, was applied. The mobile phase A was prepared by dissolving 2.74 g (20mM) of PDP (potassium dihydrogen phosphate) and 3.72 g (50mM) of PC (potassium chloride) in water (1000 mL). Then, pH was adjusted to 3.0 by adding OPA (ortho-phosphoric acid) 85%; while, the mobile phase B was acetonitrile (ACN) (100%). In order to confirm the experimental data about the λmax of TFN, we have used the Born-Oppenheimer molecular dynamics (BOMD) simulations, quantum mechanics (QM), and TD-DFT calculations. According to the results, the method showed a high level of suitability, specificity, linearity, accuracy, precision, repeatability, robustness, and reliable detection limit.

scholarly journals Stability-Indicating Validated HPLC Method for Simultaneous Determination of Oral Antidiabetic Drugs from Thiazolidinedione and Sulfonylurea Groups in Combined Dosage Forms

2010 ◽  
Vol 93 (4) ◽  
pp. 1086-1092 ◽  
Author(s):  
Anna Gumieniczek ◽  
Anna Berecka ◽  
ukasz Komsta
Keyword(s):  
Simultaneous Determination ◽  
Mobile Phase ◽  
Uv Light ◽  
Degradation Products ◽  
Dosage Forms ◽  
Hplc Method ◽  
Base Temperature ◽  
Stability Indicating ◽  
Acid And Base

Abstract For type 2 diabetes treatment, combinations of drugs from the thiazolidinedione and sulfonylurea groups are now available in the same tablet or capsule. Therefore, a stability-indicating and validated HPLC method was developed for simultaneous determination of pioglitazone, rosiglitazone, and glipizide in combined dosage forms. The examined drugs were subjected to different conditions such as acid and base, temperature, and UV light, and degradation of pioglitazone and glipizide was observed under thermal and acidic stress. However, selectivity of the presented method for pioglitazone, rosiglitazone, and glipizide assay against their degradation products was confirmed. It was also demonstrated to be robust, resisting small deliberate changes in pH of the buffer, flow rate, and percentage of acetonitrile in the mobile phase. The presented method utilizes a LiChrospher RP18 column (125 4.0 mm), acetonitrile in phosphate buffer at pH 4.3 (40 + 60, v/v) as the mobile phase, and UV detection at 225 nm for pioglitazone/glipizide or 245 nm for rosiglitazone/glipizide. The method was validated with respect to linearity, precision, and accuracy. Finally, the elaborated procedure was applied for the QC of pioglitazone/glipizide and rosiglitazone/glipizide mixtures.

scholarly journals Stability-Indicating Method for Determination of Oxyphenonium Bromide and Its Degradation Product by High-Performance Liquid Chromatography

2007 ◽  
Vol 90 (5) ◽  
pp. 1250-1257 ◽  
Author(s):  
Alaa EL-Gindy ◽  
Samy Emara ◽  
Heba Shaaban
Keyword(s):  
Degradation Product ◽  
High Performance ◽  
Potassium Dihydrogen Phosphate ◽  
Order Rate Constant ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Dihydrogen Phosphate ◽  
Stability Indicating Method ◽  
Oxyphenonium Bromide

Abstract A high-performance liquid chromatographic (HPLC) method was developed for determination of oxyphenonium bromide (OX) and its degradation product. The method was based on the HPLC separation of OX from its degradation product, using a cyanopropyl column at ambient temperature with mobile phase of acetonitrile25 mM potassium dihydrogen phosphate, pH 3.4 (50 + 50, v/v). UV detection at 222 nm was used for quantitation based on peak area. The method was applied to the determination of OX and its degradation product in tablets. The proposed method was also used to investigate the kinetics of the acidic and alkaline degradation of OX at different temperatures, and the apparent pseudo first-order rate constant, half-life, and activation energy were calculated. The pH-rate profile of the degradation of OX in Britton-Robinson buffer solutions within the pH range 212 was studied.

scholarly journals Validation of Simultaneous Volumetric and HPLC Methods for the Determination of Pridinol Mesylate in Raw Material

2013 ◽  
Vol 2013 ◽  
pp. 1-5
Author(s):  
Laura D. Simionato ◽  
Leonardo Ferello ◽  
Sebastián Stamer ◽  
Patricia D. Zubata ◽  
Adriana I. Segall
Keyword(s):  
Mobile Phase ◽  
Potassium Dihydrogen Phosphate ◽  
Hplc Method ◽  
Volumetric Method ◽  
Raw Material ◽  
Organic Layer ◽  
Dihydrogen Phosphate ◽  
Reverse Phase ◽  
Potassium Dihydrogen

Simple, sensitive, and economical simultaneous volumetric and HPLC methods for the determination of pridinol mesylate in raw material have been developed. The volumetric method is based on the reaction of pridinol with sodium lauryl sulphate in diluted sulphuric acid. Dimethyl yellow was used as indicator to detect the end point of the titration in aqueous/organic layer. The HPLC method for the determination of pridinol mesylate employs a reverse phase C18 column at ambient temperature with a mobile phase consisting of acetonitrile: 0.05 M potassium dihydrogen phosphate, pH adjusted to 5.0 (1 : 2, v/v). The flow rate was 0.8 mL/min. Quantitation was achieved with UV detection at 258 nm based on peak area. Both methods were found to be suitable for the quality control of pridinol mesylate in raw material.

scholarly journals A quantitative HPLC method for simultaneous determination of prodrug of voriconazole and voriconazole in beagle plasma, and its application to a toxicokinetic study

2021 ◽  
Author(s):  
Yufa Wen ◽  
Shuang Chen ◽  
Yanjuan Yuan ◽  
Qing Shao ◽  
Xuejun He ◽  
...  
Keyword(s):  
Simultaneous Determination ◽  
High Performance ◽  
Potassium Dihydrogen Phosphate ◽  
Internal Standard ◽  
Storage Conditions ◽  
Hplc Method ◽  
Dihydrogen Phosphate ◽  
Different Temperatures ◽  
Reproducible Method

AbstractA simple, rapid, efficient and reproducible method based on High Performance Liquid Chromatography (HPLC) for simultaneous determination of prodrug of voriconazole (POV) and voriconazole in beagle plasma has been established and validated. Omeprazole was utilized as the sole internal standard. Analytes and internal standards were extracted through protein precipitation and separated on a Venusil XBP C18 chromatography column (4.6 × 250 mm, 5 µm). The mobile phase was methanol and 20 mmol/L potassium dihydrogen phosphate. Chromatographic separation was achieved by using an isocratic elution procedure that used 65% methanol and a flow rate of 1 mL/min. The ultraviolet (UV) detection wavelength was 256 nm and the total running time was 15 min. This method showed good linear ranges of 100–75,000 ng/mL for voriconazole prodrug and 200–100,000 ng/mL for voriconazole respectively. The precision and accuracy were acceptable. Analytes in plasma samples are stable under different temperatures and storage conditions. The developed HPLC method has been successfully applied to the studies of toxicokinetics of POV after intravenous drip in beagle and provided important information for the further development and application.

Validated Stability-Indicating RP-HPLC Method for Simultaneous Determination of Clorsulon and Ivermectin Employing Plackett-Burman Experimental Design for Robustness Testing

2016 ◽  
Vol 99 (2) ◽  
pp. 571-578 ◽  
Author(s):  
Ahmed S Saad ◽  
Nahla S Ismail ◽  
Marwa Soliman ◽  
Hala E Zaazaa
Keyword(s):  
Experimental Design ◽  
Simultaneous Determination ◽  
Degradation Products ◽  
Hplc Method ◽  
Forced Degradation ◽  
Dihydrogen Phosphate ◽  
Sodium Dihydrogen Phosphate ◽  
Pharmaceutical Dosage Form ◽  
Stability Indicating

Abstract A sensitive and highly selective stability-indicating gradient HPLC method was developed and validated for simultaneous determination of clorsulon (CLO) and ivermectin (IVM) in the presence of their degradation products. The drugs were subjected to different stress conditions, including acid and alkaline hydrolysis, oxidative, thermal, and photolytic forced degradation. The robustness of the proposed method was assessed using the Plackett-Burman experimental design, the factors affecting system performance were defined, and nonsignificant intervals for the significant factors were determined. The separation was carried out on a ZORBAX SB phenyl analytical column (250 × 4.6 mm id, 5 μm particle size), with gradient elution utilizing 10 mM sodium dihydrogen phosphate and acetonitrile as mobile phase. UV detection was performed for CLO and IVM at 254 nm over a concentration range of 4–140 and 5–50 μg/mL, respectively, with mean percentage recoveries of 99.90 ± 1.30 and 98.59 ± 1.16%, respectively. The proposed method was successfully applied to a pharmaceutical dosage form containing the investigated drugs. The results were statistically compared with the official HPLC methods, and no significant differences were found.

ESTIMATION OF TINIDAZOLE IN ALBINO RAT PLASMA BY USING RP-HPLC

INDIAN DRUGS ◽  
2017 ◽  
Vol 54 (06) ◽  
pp. 48-52
Author(s):  
M. Debnath ◽  
◽  
Y. Indira Muzib ◽  
S. Ashutosh Kumar
Keyword(s):  
Mobile Phase ◽  
Potassium Dihydrogen Phosphate ◽  
High Specificity ◽  
Rat Plasma ◽  
Hplc Method ◽  
Precipitation Method ◽  
Dihydrogen Phosphate ◽  
Albino Rat ◽  
Rp Hplc

A new RP-HPLC method for the quantitative determination of tinidazole in albino rat plasma was developed and validated as per US-FDA guidelines. The drug was spiked in the albino rat plasma and extracted with mobile phase by precipitation method. The extracted analyte was injected into Hypersil ODS C 18 (4.6 x 150 mm; 5 μm) or equivalent, maintained at 25°C temperature and effluent monitored at 310 nm. The mobile phase consisted of potassium dihydrogen phosphate [pH 3.0]: acetonitrile [HPLC Grade] (40:60 v/v). The flow rate was maintained at 1.0 mL/min. The developed method shows high specificity for tinidazole. The calibration curve for tinidazole was linear from 1.0 to 40.0 ng/0.5mL plasma (r 2 = 1). The inter-day and intra-day precision was found to be within limits. The average % recovery for the drug tinidazole was found to be 99.53 - 100.21 % and the reproducibility was found to be satisfactory. The proposed method was adequate, sensitivity, reproducibility, and specificity for the determination of tinidazole in albino rat plasma.

scholarly journals Stability-Indicating HPLC Method for the Simultaneous Determination of HIV Tablet Containing Emtricitabine, Tenofovir Disoproxil Fumarate, and Rilpivirine Hydrochloride in Pharmaceutical Dosage Forms

2014 ◽  
Vol 2014 ◽  
pp. 1-9 ◽  
Author(s):  
S. Venkatesan ◽  
N. Kannappan ◽  
Sai Sandeep Mannemala
Keyword(s):  
Tenofovir Disoproxil Fumarate ◽  
Degradation Products ◽  
Drug Product ◽  
Potassium Dihydrogen Phosphate ◽  
Hplc Method ◽  
Dihydrogen Phosphate ◽  
Combination Drug ◽  
Pharmaceutical Dosage Forms ◽  
Stability Indicating

A simple, accurate, rapid, and stability-indicating RP-HPLC method for a combination of tenofovir disoproxil fumarate, emtricitabine, and rilpivirine has been developed and subsequently validated in commercial tablets. The proposed HPLC method utilizes Phenomenex Gemini C18 column (150 mm × 4.6 mm i.d., 5 µm) and mobile phase consisting of MeCN, potassium dihydrogen phosphate buffer (20 mM, pH 3.3), and triethylamine 58.72 : 41.23 : 0.05 (v/v) at a flow rate of 1.7 mL/min. Quantitation was achieved with UV detection at 270 nm. The method was validated in terms of accuracy, precision, linearity, limits of detection, limits of quantitation, and robustness. This optimized method has been successively applied to pharmaceutical formulation and no interference from the tablet excipients was found. TDF, EMT, and RPV and their combination drug product were subjected to acid, base, neutral hydrolysis, oxidation, dry heat, and photolytic stress conditions and the stressed samples were analyzed by the proposed method. As the proposed LC method could effectively separate the drugs from its degradation products, it can be employed as stability-indicating method for the determination of instability of these drugs in bulk and commercial tablets.

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