Rapid and selective determination of pitavastatin calcium in presence of its degradation products and co-formulated drug by first-derivative micelle-enhanced and synchronous fluorimetric methods

RSC Advances ◽  
2016 ◽  
Vol 6 (109) ◽  
pp. 107246-107255 ◽  
Author(s):  
Ahmed S. Fayed ◽  
Maha A. Hegazy ◽  
Enas E. Abbas ◽  
Nahla N. Salama
Keyword(s):  
Degradation Products ◽  
Hydrolytic Degradation ◽  
Native Fluorescence ◽  
Rapid Methods ◽  
Selective Determination ◽  
First Derivative ◽  
Synchronous Fluorimetry ◽  
Pitavastatin Calcium

New, selective and rapid methods are presented for determination of PIT in the presence of its hydrolytic degradation products and co-formulated drug, EZE. These methods are derivative micelle enhanced native fluorescence and synchronous fluorimetry.

scholarly journals Determination of Trimetazidine Dihydrochloride in the Presence of Its Acid-Induced Degradation Products

2004 ◽  
Vol 87 (4) ◽  
pp. 827-833 ◽  
Author(s):  
Lories I Bebawy ◽  
Mohammed F El Tarras ◽  
Samah A El Sabour
Keyword(s):  
Degradation Products ◽  
Standard Addition ◽  
Validity Of Results ◽  
Pharmaceutical Dosage Forms ◽  
First Derivative ◽  
The Third ◽  
Bulk Powder ◽  
Intact Drug ◽  
Trimetazidine Dihydrochloride

Abstract Three methods are presented for the determination of trimetazidine dihydrochloride in the presence of its acid-induced degradation products. The first method was based on measurement of first-derivative D1 value of trimetazidine dihydrochloride at 282 nm over a concentration range of 8.00–56.00 μg/mL with mean percentage accuracy of 99.80 ± 1.17. The second method was based on first derivative of the ratio spectra DD1 at 282 nm over the same concentration range with the percentage accuracy of 99.14 ± 0.68. The third method was based on separation of trimetazidine dihydrochloride from its acid-induced degradation products followed by densitometric measurement of the spots at 215 nm. The separation was performed on silica gel 60 F254 using methanol–ammonia (100 + 1.5, v/v) as mobile phase. This method was applicable for determination of the intact drug in the presence of its degradation products over a concentration range of 2.00–9.00 μg/spot with mean percentage accuracy of 99.86 ± 0.92. The proposed methods were successfully applied for the determination of trimetazidine dihydrochloride in bulk powder, laboratory-prepared mixtures containing different percentages of 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 the reported method.

scholarly journals Choline Salicylate Analysis: Chemical Stability and Degradation Product Identification

Molecules ◽  
2019 ◽  
Vol 25 (1) ◽  
pp. 51
Author(s):  
Katarzyna B. Wróblewska ◽  
Szymon Plewa ◽  
Paweł Dereziński ◽  
Izabela Muszalska-Kolos
Keyword(s):  
Hydrogen Peroxide ◽  
Hplc Analysis ◽  
Degradation Products ◽  
Hydrolytic Degradation ◽  
Acid Media ◽  
Product Identification ◽  
The Stability ◽  
Degradation Degree ◽  
Effect Of Light

Choline salicylate (CS) as a derivative of acetylsalicylic acid is commonly used in different drug forms. In medicine, it is applied topically to inflammation of the oral cavity mucosa and in laryngology. However, this substance in the form of an ionic liquid has not been investigated enough. There are no literature studies on stability tests constituting a stage of pre-formulation research. HPLC (Nucleosil C18, 4.6 × 150 mm, 5 μm; methanol-water-acetic acid 60:40:1, 230 nm or 270 nm) and UV (276 nm) methods for the determination of CS in 2% (g/mL) aqueous solutions were developed. Under stress conditions, CS susceptibility to hydrolytic degradation in aqueous medium, hydrochloric acid, sodium hydroxide, and hydrogen peroxide, and the effect of light on the stability of CS solutions were studied with HPLC analysis. The degradation degree of CS and the purity of the solutions were also tested. Choline salicylate has been qualified as practically stable in neutral and acid media, stable in an alkaline medium, very stable in an oxidizing environment, and photolabile in solution. The HPLC-MS/MS method was used to identify 2,3- and 2,5-dihydroxybenzoic acids as degradation products of CS under the tested conditions.

Validated Chromatographic and Spectrofluorimetric Methods for Analysis of Silodosin: A Comparative Study with Application of RP-HPLC in the Kinetic Investigation of Silodosin Degradation

2020 ◽  
Author(s):  
Shereen A Boltia ◽  
Mohammed Abdelkawy ◽  
Taghreed A Mohamed ◽  
Nahla N Mostafa
Keyword(s):  
Analytical Methods ◽  
High Performance ◽  
Degradation Products ◽  
Reversed Phase ◽  
Array Detector ◽  
Kinetic Investigation ◽  
First Derivative ◽  
Rp Hplc ◽  
Significant Difference

Abstract Background Stability indicating determination of pharmaceuticals is crucial, especially for drugs which have few published official analytical methods. Silodosin (SLD) is an FDA approved α1A-adrenoceptor blocker. Objective Efficient analytical methods were suggested, based on different instrumental techniques for quantification of SLD, besides conducting kinetic investigation of its degradation. Methods The first method is based on Reversed Phase High Performance Liquid Chromatography with Photodiode Array Detector (RP-HPLC-PDAD). Detection is done at wavelength 225 nm. The second method is focused on using High Performance Thin Layer Chromatography (HPTLC) and eluting the drug by solvent mixture followed by scanning at wavelength 270 nm. The third method depends on the First Derivative Synchronous Fluorescence Spectroscopy (1DSFS) for analysis of solutions of SLD and its acid and oxidative induced degradation products at Δλ = 90 nm, then determining the first derivative of the spectra and measuring peak amplitudes at 360 nm. Results Acceptable linearities were found in the concentration range of 0.50–90 μg/mL, 0.10–3.0 μg/band, and 0.05–0.50 µg/mL, for RP-HPLC-PDAD, HPTLC, and spectrofluorimetric methods, respectively. Conclusion Statistical analysis showed no significant difference between the suggested and the reported method. In monitoring the kinetics of SLD degradation, the order of reactions was determined and effects of degrading agent concentration and temperature on reaction rate were studied. Highlights Three analytical methods were developed for the determination of SLD based on RP-HPLC-PDAD, HPTLC, and 1DSFS in bulk and capsule dosage form. In addition, kinetic investigation of SLD degradation was performed using the developed RP-HPLC-PDAD 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.

scholarly journals Selective and Stability-Indicating Methods for the Simultaneous Determination of Mexiletine Hydrochloride and/or Its Related Substance: 2,6-Dimethylphenol

2008 ◽  
Vol 91 (4) ◽  
pp. 720-730
Author(s):  
Tarek S Belal ◽  
Rim S Haggag ◽  
Rasha A Shaalan
Keyword(s):  
Sodium Dodecyl ◽  
Coupling Reaction ◽  
Parent Drug ◽  
Related Substance ◽  
Selective Determination ◽  
Stability Indicating ◽  
Spectrophotometric Methods ◽  
First Derivative ◽  
The Stability

Abstract Four simple, rapid, sensitive, and selective analytical procedures were developed for determination of mexiletine hydrochloride (MX) and/or its related substance: 2,6-dimethylphenol (DMP). The latter is a synthetic impurity for which a maximum pharmacopeial limit is defined. The first method depends on derivative-ratio spectrophotometry, for which the first-derivative signals of the ratio spectra at 259 nm ( = 3 nm) are selected for the determination of MX. The second method is based on the spectrofluorometric measurement of MX in alkaline solution in the presence of 15 mM sodium dodecyl sulfate micellar medium at 292 nm (Ex 260 nm). The third method is based on liquid chromatographic (LC) separation of MX and DMP on an RP-C8 column with a mobile phase consisting of 50 mM Na2HPO4acetonitrile (60 + 40, adjusted to pH 2.4), and quantification of the analytes is achieved with UV detection at 212 nm based on peak area. The fourth method uses the coupling reaction of DMP with 2,6-dibromoquinone-4-chlorimide (DBQC) in borate buffer to form an intensely colored product that was spectrophotometrically measured using first-derivative amplitudes at 670 nm ( = 6nm) for the determination of DMP. Different variables affecting each method were carefully investigated and optimized. The reliability and analytical performance of the proposed methods, including linearity, range, precision, accuracy, and detection and quantitation limits, were statistically validated. The first 3 methods were successfully applied for the stability-indicating determination of MX in laboratory-prepared mixtures with DMP, as well as for the determination of MX in capsules. Also, the LC and the DBQC spectrophotometric methods permitted the selective determination of DMP in the presence of a large excess of the parent drug at or near the pharmacopeial limit (0.11).

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