Stability-Indicating Spectrofluorometric Method for the Determination of Some Cephalosporin Drugs via Their Degradation Products

2015 ◽  
Vol 98 (2) ◽  
pp. 361-370 ◽  
Author(s):  
Nadia M Mostafa ◽  
Laila Abdel-Fattah ◽  
Soheir A Weshahy ◽  
Nagiba Y Hassan ◽  
Shereen A Boltia
Keyword(s):  
Degradation Products ◽  
Hplc Method ◽  
Excitation Wavelength ◽  
Pharmaceutical Dosage Forms ◽  
Stability Indicating ◽  
Acid Degradation ◽  
Accuracy And Precision ◽  
Spectrofluorometric Method ◽  
Good Agreement

Abstract A stability-indicating spectrofluorometric method was investigated for the determination of three cephalosporin drugs, namely, cefpodoxime proxetil (CPD), cefixime trihydrate (CFX), and cefepime hydrochloride (CPM), via their acid and alkali degradation products. The three drugs were determined via their acid degradation at 432, 422, and 435 nm using an excitation wavelength of 310, 330, and 307 nm for CPD, CFX, and CPM determination, respectively, and via their alkali degradation at 407, 411, and 405 nm using an excitation wavelength of 310, 305, and 297 nm for CPD, CFX, and CPM determination, respectively. Linearity was achieved in the ranges of 0.35–3.50,0.4–4.0, and 0.3–3.0 μg/mL for the acid degradation products of CPD, CFX, and CPM, respectively, and in ranges of 0.05–0.5, 0.1–1.0, and 0.08–0.80 μg/mL for the alkali degradation products of CPD, CFX, and CPM, respectively. The method was validated for various parameters according to International Conference on Harmonization guidelines. The method was successfullyapplied for the determination of these cephalosporindrugs in pharmaceutical dosage forms with good accuracy and precision. The results obtained by the proposed spectrofluorometric method were compared with good agreement to the official HPLC method.

Stability-Indicating Determination of Rebamipide in the Presence of its Acid Degradation Products

2014 ◽  
Vol 97 (1) ◽  
pp. 78-85 ◽  
Author(s):  
Samah S Abbas ◽  
Hala E Zaazaa ◽  
Hebat Allah M Essam ◽  
Mohammed G El-Bardicy
Keyword(s):  
Degradation Products ◽  
Complete Separation ◽  
Peak Amplitude ◽  
Pharmaceutical Dosage Forms ◽  
Stability Indicating ◽  
Acid Degradation ◽  
First Derivative ◽  
Rp Hplc ◽  
Absorbance Difference

Abstract Four sensitive and precise stability-indicating methods for the determination of rebamipide (REB) in the presence of its acid-degradation products and ina pharmaceutical formulation were developed and validated. Method A used the first derivative of the ratio spectra (1DD) spectrophotometric method by measuring the peak amplitude at 249.4 nm (maximum) and at 259 nm (minimum), and at the total peak amplitude (from 249.4 to 259 nm, 1DD249.4 + 259 nm) in the range of 2–14 μg/mL. This method yielded mean recoveries of 99.87 ± 0.83, 100.04 ± 0.75, and 100.28 ± 1.11%, respectively. Method B is a dual wavelength method, which allows the determination of REB in presence of its acid-degradation products by measuring the absorbance difference between 254 and 269 nm within a linearity range of 5–65 μg/mL; it showed a mean recovery of 99.84 ± 1.06. Method C is a TLC-densitometric procedure in which REB was separated from its degradation products using a developing solution of methanol–chloroform–ammonia (8.5 + 1.5 + 0.5, v/v/v). The quantitative evaluation of REB at 329 nm was linear over the concentration range of 0.50–4.5 μg/band, with a mean recovery of 99.49 ± 0.99% even in the presence of up to 90% degradation products. Method D is an RP-HPLC procedure. It provided the complete separation of REB from its degradation products on an XterraTM C18 column using phosphate buffer (pH 6, 0.01 M)–methanol (1 + 1, v/v) as the mobile phase (UV detection at 254 nm). Recovery was 99.28 ± 0.78% within the range of 10–190 μg/mL. The selectivity of the proposed methods was checked using laboratory-prepared mixtures. The proposed methods have been successfully applied to the analysis of REBin pharmaceutical dosage forms without interference from other dosage form excipients.

Stability-Indicating TLC-Densitometric and HPLC Methods for the Simultaneous Determination of Piracetam and Vincamine in the Presence of Their Degradation Products

2016 ◽  
Vol 99 (6) ◽  
pp. 1490-1498 ◽  
Author(s):  
Amal B Ahmed ◽  
Maha M Abdelrahman ◽  
Nada S Abdelwahab ◽  
Fathy M Salama
Keyword(s):  
Simultaneous Determination ◽  
Degradation Products ◽  
Hplc Method ◽  
Pharmaceutical Formulation ◽  
Stability Indicating ◽  
Rp Hplc ◽  
Accuracy And Precision ◽  
Array Detection ◽  
Assay Methods

Abstract Newly established TLC-densitometric and RP-HPLC methods were developed and validated for the simultaneous determination of Piracetam (PIR) and Vincamine (VINC) in their pharmaceutical formulation and in the presence of PIR and VINC degradation products, PD and VD, respectively. The proposed TLC-densitometric method is based on the separation and quantitation of the studied components using a developing system that consists of chloroform–methanol–glacial acetic acid–triethylamine (8 + 2 + 0.1 + 0.1, v/v/v/v) on TLC silica gel 60 F254 plates, followed by densitometric scanning at 230 nm. On the other hand, the developed RP-HPLC method is based on the separation of the studied components using an isocratic elution of 0.05 M KH2PO4 (containing 0.1% triethylamine adjusted to pH 3 with orthophosphoric acid)–methanol (95 + 5, v/v) on a C8 column at a flow rate of 1 mL/min with diode-array detection at 230 nm. The developed methods were validated according to International Conference on Harmonization guidelines and demonstrated good accuracy and precision. Moreover, the developed TLC-densitometric and RP-HPLC methods are suitable as stability-indicating assay methods for the simultaneous determination of PD and VD either in bulk powder or pharmaceutical formulation. The results were statistically compared with those obtained by the reported RP-HPLC method using t- and F-tests.

scholarly journals STABILITY INDICATING RP-LC ASSAY METHOD FOR CARISOPRODOL

2017 ◽  
Vol 9 (6) ◽  
pp. 79
Author(s):  
M. Sangeetha ◽  
Tirumala . ◽  
Nagamallika .
Keyword(s):  
Degradation Products ◽  
Drug Product ◽  
Hplc Method ◽  
Assay Method ◽  
Pharmaceutical Dosage Forms ◽  
Stability Indicating ◽  
Photolytic Degradation ◽  
Ich Guidelines ◽  
The Mean

Objective: A reverse phase stability-indicating HPLC method was developed for the determination of Carisoprodol in pharmaceutical dosage forms. The chromatographic elution was achieved on C18, 250 mm × 4.6 mm, 5-μm particle size column.Methods: The mobile phase contains a mixture of water and acetonitrile in ratio of 60:40 v/v. The flow rate was 1.0 ml min-1 and was detected by Refractive index detector.Results: The method was proven to be linear over a range of 1 to 4 mg/ml with a mean correlation coefficient of 0.99998. The %mean recovery is in the range of 100.55% to 101.11% and %RSD was less than 1.0% between preparations. The % RSD for Assay results of initial sample preparation in different intervals of 0hr, 24 h, 30 h and 48 h was less than 1.0%. To establish stability-indicating capability of the method, drug product was subjected to the stress conditions of acid, base, oxidative, hydrolytic, thermal and photolytic degradation. The degradation products were well resolved from Carisoprodol.Conclusion: The developed method was validated as per international ICH guidelines with respect to specificity, linearity, accuracy, precision and robustness.

Stability-Indicating Methods for the Determination of Erdosteine in the Presence of its Acid Degradation Products

2014 ◽  
Vol 97 (1) ◽  
pp. 86-93 ◽  
Author(s):  
Nadia M Moustafa ◽  
Amr M Badawey ◽  
Nesrine T Lamie ◽  
Abd El-Aziz B Abd El-Aleem
Keyword(s):  
Mobile Phase ◽  
Degradation Products ◽  
Validity Of Results ◽  
Pharmaceutical Dosage Forms ◽  
Stability Indicating ◽  
Acid Degradation ◽  
First Derivative ◽  
Percentage Recovery ◽  
The Mean

Abstract Four accurate, sensitive, and reproducible stability-indicating methods for the determination of erdosteine in the presence of its acid degradation products are presented. The first method involves processing the spectra by using a first-derivative method at 229 nm in a concentration range of 10–70 μg/mL. The mean percentage recovery was 100.43 ± 0.977. The second method is based on ratio-spectra first derivative spectrophotometry at 227.4 and 255 nm over a concentration range of 10–70 μg/mL. The mean percentage recovery was 99.65 ± 1.122% and 100.02 ± 1.306% at 227.4 and 255 nm, respectively. The third method utilizes quantitative densitometric evaluation of the TLC of erdosteine in the presence of its acid degradation products, and uses methanol–chloroform–ammonia (7 + 3 + 0.01, v/v/v) asthe mobile phase. TLC chromatograms were scanned at235 nm. This method analyzes erdosteine in a concentration range of 2.4–5.6 μg/spot, with a mean percentage recovery of 100.03 ± 1.015%. The fourth method is HPLC for the simultaneousdetermination of erdosteine in the presence of its acid degradation products. The mobile phase consists of water–methanol (65 + 35, v/v). The standard curve of erdosteine showed good linearity overa concentration range of 10–80 μg/mL,with a mean percentage recovery of 99.90 ± 1.207%. These methods were successfully applied to the determination of erdosteine in bulk powder, laboratory-prepared mixtures containing different percentages of the degradation products, and pharmaceutical dosage forms. The validity of results was assessed by applying the standard addition technique. The results obtained agreed statistically with those obtained by a reported method, showing no significant differences with respect to accuracy and precision.

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.

scholarly journals Development and Validation of a Rapid RP-HPLC Method for the Estimation of Esmolol Hydrochloride in Bulk and Pharmaceutical Dosage Forms

2010 ◽  
Vol 7 (3) ◽  
pp. 807-812 ◽  
Author(s):  
Vanita Somasekhar ◽  
D. Gowri Sankar
Keyword(s):  
Limit Of Detection ◽  
Hplc Method ◽  
Detector Response ◽  
Reverse Phase Hplc ◽  
Limit Of Quantification ◽  
Pharmaceutical Dosage Forms ◽  
Rp Hplc ◽  
Accuracy And Precision ◽  
Development And Validation

A reverse phase HPLC method is described for the determination of esmolol hydrochloride in bulk and injections. Chromatography was carried on a C18column using a mixture of acetonitrile, 0.05 M sodium acetate buffer and glacial acetic acid (35:65:3 v/v/v) as the mobile phase at a flow rate of 1 mL/min with detection at 275 nm. The retention time of the drug was 4.76 min. The detector response was linear in the concentration of 1-50 μg/mL. The limit of detection and limit of quantification was 0.614 and 1.86 μg/mL respectively. The method was validated by determining its sensitivity, linearity, accuracy and precision. The proposed method is simple, economical, fast, accurate and precise and hence can be applied for routine quality control of esmolol hydrochloride in bulk and injections.

scholarly journals STABILITY INDICATING HPLC METHOD FOR DETERMINATION OF VILAZODONE HYDROCHLORIDE

2017 ◽  
Vol 9 (4) ◽  
pp. 123
Author(s):  
Birva A. Athavia ◽  
Zarna R. Dedania ◽  
Ronak R. Dedania ◽  
S. M. Vijayendra Swamy ◽  
Chetana B. Prajapati
Keyword(s):  
Limit Of Detection ◽  
Degradation Products ◽  
Hplc Method ◽  
Alkaline Condition ◽  
Forced Degradation ◽  
Molecular Formula ◽  
Stability Indicating ◽  
Dry Heat ◽  
Limit Of Quantitation

Objective: The aim and objective of this study was to develop and validate Stability Indicating HPLC method for determination of Vilazodone Hydrochloride.Methods: The method was carried out on a Phenomenex, C18 (250x4.6 mm, 5 µm) Column using a mixture of Acetonitrile: Water (50:50v/v), pH adjusted to 3.3 with Glacial Acetic Acid for separation. The flow rate was adjusted at 1 ml/min and Detection was carried out at 240 nm.Results: The retention time of vilazodone hydrochloride was found to be 2.3 min. The calibration curve was found to be linear in the range 25-75µg/ml with a correlation coefficient (R2=0.996). The limit of detection and limit of quantitation were found to be 4.78µg/ml and 14.48µg/ml respectively. The % recovery of vilazodone hydrochloride was found to be in the range of 98.21±0.08 % to 99.07±0.64%. The proposed method was successfully applied for the estimation of vilazodone hydrochloride in marketed tablet formulation.Vilazodone Hydrochloride was subjected to forced degradation under Acidic, Alkaline, Oxidation, Dry Heat and Photolytic degradation conditions. Vilazodone hydrochloride showed 3.12% degradation under acidic condition, 4.78% under alkaline condition, 7.8% under oxidation condition, 3.53% under dry heat condition and 4.9% under photolytic condition.Acid degradation impurity was identified and characterised by LC-MS/MS was found to be 1-(4-Penten-1-yl) piperazine having molecular weight 154.253 (m/z 155.08) and Molecular Formula C9H18N2.Conclusion: A simple, precise, rapid and accurate Stability Indicating HPLC method has been developed and validated for the determination of Vilazodone Hydrochloride in presence of its degradation products as per the ICH Guidelines. 

Sign in / Sign up

Export Citation Format

Share Document