scholarly journals Development and Validation of RP-LC Method for the Determination of Cinnarizine/Piracetam and Cinnarizine/Heptaminol Acefyllinate in Presence of Cinnarizine Reported Degradation Products

2013 ◽  
Vol 8 ◽  
pp. ACI.S12478 ◽  
Author(s):  
Ola M. EL-Houssini ◽  
Nagwan H. Zawilla ◽  
Mohammad A. Mohammad
Keyword(s):  
Degradation Products ◽  
Pharmaceutical Formulations ◽  
Assay Method ◽  
Good Resolution ◽  
Reverse Phase ◽  
Intermediate Precision ◽  
Reverse Phase Liquid Chromatography ◽  
Phase Liquid ◽  
Development And Validation

Specific stability indicating reverse-phase liquid chromatography (RP-LC) assay method (SIAM) was developed for the determination of cinnarizine (Cinn)/piracetam (Pira) and cinnarizine (Cinn)/heptaminol acefyllinate (Hept) in the presence of the reported degradation products of Cinn. A C18 column and gradient mobile phase was applied for good resolution of all peaks. The detection was achieved at 210 nm and 254 nm for Cinn/Pira and Cinn/Hept, respectively. The responses were linear over concentration ranges of 20-200, 20-1000 and 25-1000 μgmL−1 for Cinn, Pira, and Hept respectively. The proposed method was validated for linearity, accuracy, repeatability, intermediate precision, and robustness via statistical analysis of the data. The method was shown to be precise, accurate, reproducible, sensitive, and selective for the analysis of Cinn/Pira and Cinn/Hept in laboratory prepared mixtures and in pharmaceutical formulations.

Separation and Analysis of Pilocarpine, Isopilocarpine, and Pilocarpic Acid by Reverse Phase Liquid Chromatography: Collaborative Study

1984 ◽  
Vol 67 (5) ◽  
pp. 924-926
Author(s):  
John L Van Ackeren ◽  
Richard M Venable ◽  
Irving W Wainer
Keyword(s):  
Degradation Products ◽  
Collaborative Study ◽  
Uv Spectrophotometry ◽  
Reverse Phase ◽  
Reverse Phase Liquid Chromatography ◽  
Coefficients Of Variation ◽  
Quantitative Results ◽  
Phase Liquid ◽  
Liquid Chromatographic

Abstract A method for separating and determining pilocarpine and 2 degradation products was developed and subjected to collaborative study. Pilocarpine, isopilocarpine, and pilocarpic acid were isolated on a reverse phase liquid chromatographic phenyl bonded column and detected by UV spectrophotometry at 220 nm. Nine collaborators received commercial samples labeled to contain 2,1, and 0.5% pilocarpine and a 2% practice sample. The collaborative results for pilocarpine were excellent; coefficients of variation ranged from 3.20 to 4.10%. The method was adopted official first action for determination of the active component, pilocarpine, in the presence of isopilocarpine and pilocarpic acid. Although quantitative results for the degradation products were not as good, the method is suitable as a limits test for these substances.

scholarly journals Simultaneous Determination of Acetaminophen, Pamabrom and Pyrilamine Maleate in Pharmaceutical Formulations Using Stability Indicating HPLC Assay Method

2017 ◽  
Vol 59 (2) ◽  
Author(s):  
Muhammad Ashfaq
Keyword(s):  
Simultaneous Determination ◽  
Mobile Phase ◽  
Degradation Products ◽  
Pharmaceutical Formulations ◽  
Assay Method ◽  
Good Resolution ◽  
Pharmaceutical Dosage Forms ◽  
Stability Indicating ◽  
Water Ph

A simple, specific and accurate stability indicating RPHPLC method was developed for the determination of acetaminophen, pamabrom and pyrilamine maleate simultaneously in pharmaceutical dosage forms. Successful separation of all the components was enacted within 10 min using C18 column with mobile phase of methanol and acidified water (pH 1.8) in the ratio of (27: 73 v/v respectively). Flow rate of the mobile phase was 1.5 mL/min with detection at 300 nm. The method was validated in accordance with ICH guidelines. Response was a linear function of concentration over the range of 50- 150 􀈝g/mL for acetaminophen, 2.5-7.5 􀈝g/ mL for pamabrom and 1.5-4.5 􀈝g/mL for pyrilamine maleate. The method resulted in excellent separation of all the analytes along with their stress induced degradation products with acceptable peak tailing and good resolution. It is therefore can be applied successfully for simultaneous determination of acetaminophen, pamabrom and pyrilamine maleate in pharmaceutical formulations and their stability studies.

Stability Indicating Liquid Chromatographic Method for the Determination of Fenofibrate and its Application to Kinetic Studies

2013 ◽  
Vol 5 (4) ◽  
pp. 1866-1874
Author(s):  
K. Srinivasa Rao ◽  
Keshar N K ◽  
N Jena ◽  
M.E.B Rao ◽  
A K Patnaik
Keyword(s):  
Degradation Products ◽  
Kinetic Studies ◽  
Pharmaceutical Formulations ◽  
Assay Method ◽  
Pharmaceutical Dosage Form ◽  
Stability Indicating ◽  
Zero Order Kinetics ◽  
Relative Standard ◽  
Liquid Chromatographic

A stability-indicating LC assay method was developed for the quantitative determination of fenofibrate (FFB) in pharmaceutical dosage form in the presence of its degradation products and kinetic determinations were evaluated in acidic, alkaline and peroxide degradation conditions. Chromatographic separation was achieved by use of Zorbax C18 column (250 × 4.0 mm, 5 μm). The mobile phase was established by mixing phosphate buffer (pH adjusted 3 with phosphoric acid) and acetonitrile (30:70 v/v). FFB degraded in acidic, alkaline and hydrogen peroxide conditions, while it was more stable in thermal and photolytic conditions. The described method was linear over a range of 1.0-500 μg/ml for determination of FFB (r= 0.9999). The precision was demonstrated by relative standard deviation (RSD) of intra-day (RSD= 0.56– 0.91) and inter-day studies (RSD= 1.47). The mean recovery was found to be 100.01%. The acid and alkaline degradations of FFB in 1M HCl and 1M NaOH solutions showed an apparent zero-order kinetics with rate constants 0.0736 and 0.0698  min−1 respectively and the peroxide degradation with 5% H2O2 demonstrated an apparent first-order kinetics with rate constant k = 0.0202 per min. The t1/2, t90   values are also determined for all the kinetic studies. The developed method was found to be simple, specific, robust, linear, precise, and accurate for the determination of FFB in pharmaceutical formulations.  

Determination of queuosine derivatives by reverse-phase liquid chromatography for the hypomodification study of Q-bearing tRNAs from various mammal liver cells

2004 ◽  
Vol 801 (2) ◽  
pp. 237-247 ◽  
Author(s):  
Annie Costa ◽  
Jean-Paul Paı̈s de Barros ◽  
Gérard Keith ◽  
Wlodzimierz Baranowski ◽  
Jean Desgrès
Keyword(s):  
Liquid Chromatography ◽  
Liver Cells ◽  
Reverse Phase ◽  
Reverse Phase Liquid Chromatography ◽  
Phase Liquid

Determination of Diacetyl in Butter as 2,3-Diaminonaphthalene Derivative, Using a Fluorometric Procedure or Reverse Phase Liquid Chromatography with Fluorescence Detection

1988 ◽  
Vol 71 (3) ◽  
pp. 462-465
Author(s):  
Pietro Damiani ◽  
Giovanni Burini
Keyword(s):  
Liquid Chromatography ◽  
Fluorescence Detection ◽  
The Other ◽  
Reverse Phase ◽  
Reverse Phase Liquid Chromatography ◽  
Fluorescence Characteristics ◽  
Chromatographic Procedure ◽  
Phase Liquid ◽  
Liquid Chromatographic

Abstract Two procedures, one fluorometric and the other reverse phase liquid chromatographic, for determination of a derivative of diacetyl are described. Exploratory work on diacetyl standard solutions to establish the best conditions for the derivatization with 2,3-diaminonaphthalene (DAN) to yield 2,3-dimethylbenzo[g]-quinoxaline (DMBQ) is discussed, as well as the fluorescence characteristics of the DMBQ derivative. Diacetyl was determined in 10 commercial butter samples by the proposed procedures and by other known methods (determination of o-phenylenediamine and 3,3-diaminobenzidinederivatives). Recoveries from butter samples spiked with known amounts of diacetyl ranged from 96.9 to 101.8% (with CVs ranging from 0.3 to 2.1%) for the fluorometric procedure and from 96.9 to 102.7% (with CVs ranging from 0.5 to 2.4%) for the chromatographic procedure. These results agree well with those obtained with o-phenylenediamine and 3,3-diaminobenzidine methods on the same butter samples. The proposed methods have the advantages of improved detectability and specificity.

Determination of Aspirin and Salicylic Acid by Reverse-Phase Liquid Chromatography

1987 ◽  
Vol 70 (6) ◽  
pp. 964-966
Author(s):  
Dorothy R Heidemann ◽  
Edward S Schulenberg ◽  
William H Smith
Keyword(s):  
Salicylic Acid ◽  
Dosage Forms ◽  
Solid Dosage Forms ◽  
Reverse Phase ◽  
Solid Dosage ◽  
Reverse Phase Liquid Chromatography ◽  
Sample Extraction ◽  
Phase Liquid ◽  
Phase Column

Abstract Buffered solid dosage forms containing aspirin, magnesium hydroxide, and aluminum hydroxide are blended with acidic ethanol to extract the aspirin and salicylic acid rapidly. The resulting preparation is then immediately injected onto a 4.6 mm x 3 cm 5 (im reverse-phase column. Aspirin and free salicylic acid are determined simultaneously. The run time is <2 min. The total time from the initiation of sample extraction to completion of the separation is <5 min.

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