scholarly journals Stability-indicating UHPLC and TLC-densitometric Methods for the Determination of Tiamulin Fumarate

2021 ◽  
pp. 8-21
Author(s):  
Shimaa E. Abdel Aziz ◽  
Nermin S. Ahmed ◽  
Sawsan A. Abdel Razeq
Keyword(s):  
Mobile Phase ◽  
Degradation Products ◽  
Oral Solution ◽  
Isocratic Elution ◽  
Thin Layer Chromatogram ◽  
Stability Indicating ◽  
Intact Drug ◽  
Tlc Plates ◽  
Rf Values

Two novel stability-indicating methods were developed for the determination of tiamulin fumarate. in the presence of its degradation products. The first was UHPLC-UV method. Efficient separation was achieved by isocratic elution with a mobile phase of 0.1% aqueous ortho-phosphoric acid (pH 3.5 ± 0.5) and methanol (20:80, v/v) with UV detection at 210 nm. Linearity was obtained in the range of 0.5-10.0 µg mL-1 with mean accuracy of 100.40 ± 0.71. The second method was a TLC-densitometric evaluation of a thin-layer chromatogram of the intact drug using a mobile phase of methanol: pentanol: ethyl acetate: 16.5% ammonia (5:4:2:4, by volume). The TLC-plates were scanned densitometrically at 220 nm where Rf values were 0.58, 0.48 and 0.74 for tiamulin F, its acidic and oxidative degradants, respectively. Moreover, the plates were sprayed with 16% sulfuric acid, heated at 105°C for 10 min. where a yellow-coloured band appeared corresponding to the intact drug was scanned densitometrically at 450 nm. While the bands of the two degradants were no longer observed anymore. Tiamulin F was determined in the range of 1.0-10.0 μg/band with mean accuracy of 100.27% ± 1.47 at 220 nm and 99.93% ± 1.38 at 450 nm. The proposed methods were successfully applied for the determination of drug in marketed oral solution. The obtained results were statistically analyzed and found to be in accordance with those obtained by a reported method.

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.

Stability-Indicating Methods for the Determination of Candesartan Cilexetil in Bulk Drug and Pharmaceutical Formulations

2013 ◽  
Vol 96 (3) ◽  
pp. 580-586 ◽  
Author(s):  
Yousry M Issa ◽  
Emad M Hussien ◽  
Magda M Ibrahim ◽  
Fatma M Abdel-Gawad ◽  
Saadia Barakat
Keyword(s):  
Mobile Phase ◽  
Candesartan Cilexetil ◽  
Degradation Products ◽  
Pharmaceutical Formulations ◽  
Stability Indicating ◽  
Bulk Powder ◽  
System Suitability ◽  
The Mean ◽  
Bulk Drug

Abstract Two stability-indicating methods were developed for the determination of candesartan cilexetil in the presence of its degradation products. The first method uses isocratic RP-HPLC with an Agilent C18 column. The mobile phase was phosphate buffer (pH = 2.8 ± 0.1)–acetonitrile (60 + 40, v/v). The flow rate was 2.0 mL/min, and the UV detection was at 254 nm. The second method depends on TLC-densitometric measurements of drug spots at 254 nm. The separation was carried out on silica gel 60 F254 plates using ethyl acetate–methanol–toluene– ammonia 33% (40 + 25 + 20 + 2, v/v/v/v) mobile phase. The methods were validated according to U.S. Pharmacopeia guidelines, and the acceptance criteria for accuracy, precision, linearity, specificity, robustness, LOD, LOQ, and system suitability were met in all cases. Linear ranges of the methods were 10.0–200.0 μg/mL and 1.0–9.0 μg/spot for HPLC and TLC, respectively. The proposed methods were successfully applied to the drug in bulk powder, in laboratory-prepared mixtures with its degradation products, and in commercially available tablets. The results were compared statistically at the 95% confidence level with each other. There were no significant differences between the mean recovery and precision of the two methods.

scholarly journals Validated Stability Indicating Chromatographic Methods for Quantification of Imidocarb Dipropionate; Application for the Determination of Its Residues in Bovine Meat and Milk Samples

2020 ◽  
Vol 103 (4) ◽  
pp. 980-988
Author(s):  
Ghada AbdElHamid Sedik ◽  
Doha Mohamed Naguib ◽  
Fahima Morsy ◽  
Hala Elsayed Zaazaa
Keyword(s):  
Degradation Products ◽  
Reversed Phase ◽  
Hplc Method ◽  
Stability Indicating ◽  
Milk Samples ◽  
Chromatographic Methods ◽  
Ich Guidelines ◽  
Imidocarb Dipropionate ◽  
Tlc Plates

Abstract Background Imidocarb dipropionate (IMD) is an immunomodulator agent commonly used for treatment of anaplasmosis in cattle. Objective Thus, two sensitive, specific, and precise stability-indicating chromatographic methods have been developed, optimized, and validated for its determination in presence of its acid, alkaline, and oxidative stressed degradation products. Method The first method is based on separation of IMD and its forced induced degradation products on reversed phase cyano column using isocratic elution system consisted of sodium acetate buffer–methanol–acetonitrile (55: 30:15, v/v/v), pH 4.6 at a flow rate of 1.2 mL/min, and UV detection at 254 nm. The second method utilized TLC combined with densitometric determination of the separated bands at 254 nm. The separation was achieved using silica gel 60 F254 TLC plates with a mixture of ethyl acetate–methanol–ammonia–water (8.5:1:0.5:0.2, v/v/v/v) as a developing system. Results HPLC analysis was applied in range of 0.25–40 µg/mL with LOD of 0.073 µg/mL. While densitometric measurements showed linearity in the range of 0.1–1.8 µg/band with LOD of 0.02 µg/band. Conclusions The suggested methods were validated in compliance with the ICH guidelines and were successfully applied for determination of IMD in its commercial veterinary formulations with good recoveries. Furthermore, the proposed HPLC method was extended to the determination of IMD residues in bovine meat and milk samples Highlights Bovine meat, HPLC, Imidocarb dipropionate, Milk, TLC.

Stability-Indicating Determination of Tedizolid Phosphate in the Presence of its Active Form and Possible Degradants

2021 ◽  
Author(s):  
Eman M Moaaz ◽  
Ezzat M Abdel-Moety ◽  
Mamdouh R Rezk ◽  
Ahmed S Fayed
Keyword(s):  
Flow Rate ◽  
Phosphate Buffer ◽  
Mobile Phase ◽  
Degradation Products ◽  
Active Form ◽  
Pharmaceutical Formulations ◽  
Bacterial Strains ◽  
Stress Degradation ◽  
Tlc Plates

Abstract Tedizolid phosphate is an antibiotic prodrug that is metabolized into tedizolid which is used against various resistant bacterial strains. In this study, tedizolid phosphate was subjected to stress degradation conditions, namely, hydrolysis (neutral, acidic and alkaline), thermal, oxidative and photolytic ones. The prodrug was stable toward thermal and photolytic stress conditions, while it showed significant degradation upon applying oxidative and hydrolytic conditions. Two suggested chromatographic methods are described for separation and determination of tedizolid phosphate from the resulted degradation products. The first method is HPLC using Waters Xselect HSS C18 (250 × 4.6 mm, 5 μm) analytical column and mobile phase composed of phosphate buffer (50 mM, pH 6.5):acetonitrile (70:30, %v/v) pumped at flow rate of 1.0 mL/min with UV-detection at 300 nm. The second method is a TLC coupled with densitometric quantitation, precoated silica TLC-plates as a stationary phase and a mobile phase of methanol:butanol:ethyl acetate:ammonia (33%, w/v) (60:20:20:10,%v/v) were used. The chromatographed plates were scanned at 300 nm. The linearity was confirmed over concentration range of 1–100 μg/mL and 1–12 μg/band for HPLC and TLC-densitometric methods, respectively. Both methods were found to be suitable for determination of tedizolid phosphate in pure form and in its pharmaceutical formulations.

scholarly journals Stability Indicating HPLC Method for the Determination of Delamanid in Pharmaceutical Dosage Form

2021 ◽  
Vol 11 (1-s) ◽  
pp. 108-112
Author(s):  
Advaita B. Patel ◽  
Deepa R. Patel ◽  
Dhaval M. Patel ◽  
Mansi Babaria
Keyword(s):  
Analytical Method ◽  
Mobile Phase ◽  
Dosage Form ◽  
Degradation Products ◽  
Stress Test ◽  
Reversed Phase ◽  
Hplc Method ◽  
Pharmaceutical Dosage Form ◽  
Stability Indicating

Delamanid is successfully used for treatment of MDR TB. A stability indicating analytical method has been developed and validated. In this study Delamanid was degraded under different stress test conditions as per International Conference on Harmonization. The degraded samples were used to develop a stability-indicating high performance liquid chromatographic (HPLC) method for the Delamanid. The Delamanid was well separated from degradation products using a reversed-phase Hypersil BDS C18 (250 mm × 4.6mm i.d., 5µm) column and a mobile phase comprising of 0.01M pH 2.70 Phosphate Buffer: Acetonitrile (pH 3.50) 70:30, pH of mobile phase was adjusted with Glacial acetic acid and other HPLC parameters were flow rate 1 mL/min, detection wavelength 254 nm and injection volume 10 µl. The method was validated for linearity, precision, accuracy, ruggedness and robustness. Results obtained after validation study indicating that the proposed single method allowed analysis of Delamanid in the presence of their degradation products formed under a variety of stress conditions. The developed procedure was also applicable to the determination of stability of the Delamanid in commercial pharmaceutical dosage form. Keywords:  Delamanid, stability indicating analytical method, HPLC

scholarly journals STABILITY-INDICATING METHODS FOR THE DERTERMINATION OF GEMIFLOXACIN IN PRESENCE OF ITS ACID DEGRADATION PRODUCT(S)

2015 ◽  
Vol 11 (6) ◽  
pp. 3698-3708
Author(s):  
Fatma Alamin ◽  
Ezzat Abdel Moety ◽  
Amr Badawey ◽  
Heba Hefne
Keyword(s):  
Degradation Products ◽  
Zero Crossing ◽  
Stability Indicating ◽  
Acid Degradation ◽  
First Derivative ◽  
Wide Range ◽  
Intact Drug ◽  
Minimal Data ◽  
The Difference

Brilliant, valid and simple five UV spectrophotometric stability indicating techniques are adopted for the determination of Gemifloxacin (GEM) in presence of its acid degradation products over a concentration range of 2-12 μg mL-1. The first method is an application of the first derivative (1D) spectrophotometry, that allows the determination of GEM without interference of its acid degradation products at zero crossing wavelength (254.6 nm). The second method depends on the first-derivative of the ratio spectra spectrophotometry (1DD) for determination of GEM in presence of its acid degradation products at a maximum of 273.0 nm and a minimum of 284.0 nm, While the third dual wavelength method offers a superior stability indicating procedures for the determination of GEM in the zero order spectra at the wavelength pair of 271.8 nm and 325.0 nm. The fourth method is the ratio difference one, with the advantages of minimal data processing and wide range of application. It is applied for the analysis of intact drug in presence of its acid degradation products by measuring the difference in the peak amplitude at the ratio spectra at 355.0 nm and 270.0 nm. The last method is based on the quantification of GEM through the bivariate calibration at 255.0 nm and 277.0 nm by adopting simple mathematic algorithm that provides simplicity and rapidity.

scholarly journals HPLC, TLC, and First-Derivative Spectrophotometry Stability-Indicating Methods for the Determination of Tropisetron in the Presence of Its Acid Degradates

2010 ◽  
Vol 93 (4) ◽  
pp. 1180-1191 ◽  
Author(s):  
Laila S Abdel-Fattah ◽  
Zeinab A El-Sherif ◽  
Khadiga M Kilani ◽  
Dalia A El-Haddad
Keyword(s):  
Degradation Product ◽  
Mobile Phase ◽  
Degradation Products ◽  
Derivative Spectrophotometry ◽  
Pharmaceutical Dosage Form ◽  
Zero Crossing ◽  
Stability Indicating ◽  
First Derivative ◽  
First Derivative Spectrophotometry

Abstract Three stability-indicating assay methods were developed for the determination of tropisetron in a pharmaceutical dosage form in the presence of its degradation products. The proposed techniques are HPLC, TLC, and first-derivative spectrophotometry (1D). Acid degradation was carried out, and the degradation products were separated by TLC and identified by IR, NMR, and MS techniques. The HPLC method was based on determination of tropisetron in the presence of its acid-induced degradation product on an RP Nucleosil C18 column using methanolwateracetonitriletrimethylamine (65 + 20 + 15 + 0.2, v/v/v/v) mobile phase and UV detection at 285 nm. The TLC method was based on the separation of tropisetron and its acid-induced degradation products, followed by densitometric measurement of the intact spot at 285 nm. The separation was carried out on silica gel 60 F254 aluminum sheets using methanolglacial acetic acid (22 + 3, v/v) mobile phase. The 1D method was based on the measurement of first-derivative amplitudes of tropisetron in H2O at the zero-crossing point of its acid-induced degradation product at 271.9 nm. Linearity, accuracy, and precision were found to be acceptable over concentration ranges of 40240 g/mL, 110 g/spot, and 636 g/mL for the HPLC, TLC, and 1D methods, respectively. The suggested methods were successfully applied for the determination of the drug in bulk powder, laboratory-prepared mixtures, and a commercial sample.

scholarly journals Stability-indicating RP-HPLC method for determination of beclomethasone dipropionate in nanocapsule suspensions

2015 ◽  
Vol 51 (4) ◽  
pp. 803-810 ◽  
Author(s):  
Janaíne Micheli Chassot ◽  
Luana Mota Ferreira ◽  
Felipe Pereira Gomes ◽  
Letícia Cruz ◽  
Leandro Tasso
Keyword(s):  
Mobile Phase ◽  
Beclomethasone Dipropionate ◽  
Degradation Products ◽  
Degradation Kinetics ◽  
Hplc Method ◽  
Stability Indicating ◽  
Rp Hplc ◽  
Relative Standard ◽  
Bulk Drug

abstract A simple stability-indicating RP-HPLC/UV method was validated for determination of beclomethasone dipropionate (BD) in nanocapsule suspensions. Chromatographic conditions consisted of a RP C18column (250 mm x 4.60 mm, 5 µm, 110 Å), using methanol and water (85:15 v/v) as mobile phase at 1.0 mL/min with UV detection at 254 nm. The calibration curve was found to be linear in the concentration range of 5.0-25.0 µg/mL with a correlation coefficient > 0.999. Precision was demonstrated by a relative standard deviation lower than 2.0%. Accuracy was assessed by the recovery test of BD from nanocapsules (98.03% to 100.35%). Specificity showed no interference from the components of nanocapsules or from the degradation products derived from acid, basic and photolytic conditions. In conclusion, the method is suitable to be applied to assay BD in bulk drug and in nanocapsules, and it can be employed to study stability and degradation kinetics.

scholarly journals Development and Validation of a Novel Stability-Indicating RP-HPLC Method for Simultaneous Determination of Tezacaftor and Ivacaftor in Fixed Dose Combination

2020 ◽  
Vol 58 (4) ◽  
pp. 346-354
Author(s):  
Narendra Singh ◽  
Parveen Bansal ◽  
Mukesh Maithani ◽  
Yashpal Chauhan
Keyword(s):  
Mobile Phase ◽  
Degradation Products ◽  
Pharmaceutical Preparations ◽  
Reversed Phase ◽  
Fixed Dose ◽  
Simultaneous Estimation ◽  
Dihydrogen Phosphate ◽  
Stability Indicating ◽  
Rp Hplc

Abstract A simple and precise novel stability-indicating method for the simultaneous estimation of tezacaftor and ivacaftor in combined tablet dosage form was developed and validated using reversed-phase high-performance liquid chromatography (RP-HPLC). The method is being reported for the first time and includes an estimation of degradation products produced post-stress conditions without any extraction or derivatization. The chromatographic separation of the drugs was achieved with a Symmetry Shield RP18 Column (100 Å, 5 μm, 4.6 mm × 250 mm) using a mixture of buffer, methanol and acetonitrile (42:27:31 v/v/v) as mobile phase. The buffer used in mobile phase contained 35 mM potassium dihydrogen phosphate, and its pH was adjusted to 7.0 ± 0.02 with 20% orthophosphoric acid. The instrument was set at flow rate of 1.2 mL min−1 at ambient temperature and the wavelength of UV-visible detector at 275 nm. The developed method could be suitable for the quantitative determination of these drugs in pharmaceutical preparations and also for quality control in bulk manufacturing. Stress testing was performed to prove the specificity. No interference was observed from its stress degradation products. The statistical analysis was done by using F-test and t-test at 95% confidence level.

scholarly journals Development and validation of the stability-indicating LC-UV method for the determination of cefoselis sulphate

2012 ◽  
Vol 10 (1) ◽  
pp. 121-126 ◽  
Author(s):  
Przemysław Zalewski ◽  
Judyta Cielecka-Piontek ◽  
Anna Jelińska
Keyword(s):  
Mobile Phase ◽  
Degradation Products ◽  
Kinetic Studies ◽  
Hplc Method ◽  
Assay Method ◽  
Forced Degradation ◽  
Stability Indicating ◽  
The Stability ◽  
Development And Validation

AbstractThe stability-indicating LC assay method was developed and validated for quantitative determination of cefoselis sulphate in the presence of degradation products formed during the forced degradation studies. An isocratic, RP-HPLC method was developed with C-18 (250 × 4.6 mm, 5 µm) column and 12 mM ammonium acetate-acetonitrile (95:5 V/V) as a mobile phase. The flow rate of the mobile phase was 1.0 mL min−1. Detection wavelength was 260 nm and temperature was 30°C. Cefoselis similarly to other cephalosporins was subjected to stress conditions of degradation in aqueous solutions including hydrolysis, oxidation, photolysis and thermal degradation. The developed method was validated with regard to linearity, accuracy, precision, selectivity and robustness. The method was applied successfully for identification and determination of cefoselis sulphate in pharmaceuticals and during kinetic studies.

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