Fast gradient high performance liquid chromatography method with UV detection for simultaneous determination of seven angiotensin converting enzyme inhibitors together with hydrochlorothiazide in pharmaceutical dosage forms and spiked human plasma and urine

Talanta ◽  
2011 ◽  
Vol 85 (1) ◽  
pp. 123-129 ◽  
Author(s):  
Fawzi Elsebaei ◽  
Yan Zhu
Author(s):  
Liliya Logoyda ◽  
Yuliya Kondratova ◽  
Dmytro Korobko ◽  
Yuriy Soroka

Objective: The objective of this research was to develop more simple, sensitive, accurate, and less expensive analytical methods for the determination of captopril in medicines by Ultra-high-performance liquid chromatography.Materials and Methods: The chromatographic analysis of captopril performed on liquid chromatography Agilent 1290 Infinity II LC System.Results: A simple, rapid, sensitive, and specific method was developed for the determination of captopril by ultra-high-performance liquid chromatography in mono-medicines and pharmaceutical dosage forms in combination with hydrochlorothiazide without previous separation. Satisfactory resolution was achieved using Fused-Core® technology Ascentis Express C18 column (4.6×150 mm) and a mobile phase consisting of methanol and 0.1% solution of trifluoroacetic acid (40/60, v/v) at a flow rate 1.2 mL/minute and the wavelength detection was 220 nm. Ascentis Express columns, based on Fusеd-core pаrticle technоlogy, prоvide more than twice the speed and efficiency of traditiоnal cоlumns at half the backpressure of sub-2-μm columns. The retention time for captopril was 1.345 minute. The validation of this method was based on the ICH and USP guidelines.Conclusion: The results obtained in this research work clearly indicated that the assay was rapid, sensitive and successfully applied to the determination of both drugs in pharmaceutical dosage forms without interference from tablet excipients.


Author(s):  
Mannem Durga Babu ◽  
Kesana Surendrababu

Objective: The objective of the study was to develop and validate a novel, specific, precise, and simple reversed-phase high-performance liquid chromatography method for the estimation of guaifenesin present in methocarbamol API and its pharmaceutical dosage forms. Methods: The baseline separation for methocarbamol and guaifenesin was achieved by utilizing a Inertsil ODS C18 (250 mm × 4.6 mm) 5 μm column particle size and an isocratic elution method. The mobile phase contains a mixture of water and acetonitrile in the ratio of 70:30 v/v, respectively. The flow rate of the mobile phase was 1.0 mL/min with a column temperature of 25°C and detection wavelength at 272 nm. The method was validated for a limit of detection (LOD), limit of quantification (LOQ), linearity, accuracy, and reproducibility with the help of the exhibit and simulated samples. Results: The LOD for guaifenesin was 0.62 μg/mL. The LOQ for guaifenesin was 1.87 μg/mL. The correlation coefficient obtained for impurity was >0.99. The recovery was obtained for impurity was 106.56% at 50%, 95.20% at 100%, and 100.45% at 150%. In tablet analysis, we can found 0.26% (<0.5%). Conclusion: The developed method was validated as per the ICH guidelines with respect to specificity, precision, linearity, accuracy, LOD and quantification, ruggedness, robustness, and solution stability.


2019 ◽  
Vol 69 (3) ◽  
pp. 363-380 ◽  
Author(s):  
Tanja Rozman Peterka ◽  
Tina Trdan Lušin ◽  
Jure Bergles ◽  
Zoran Ham ◽  
Rok Grahek ◽  
...  

Abstract An ultra-high performance liquid chromatography method for simultaneous determination of tacrolimus impurities in pharmaceutical dosage forms has been developed. Appropriate chromatographic separation was achieved on a BEH C18 column using gradient elution with a total run time of 14 min. The method was applied to analyses of commercial samples and was validated in terms of linearity, precision, accuracy, sensitivity and specificity. It was found to be linear, precise and accurate in the range of 0.05 to 0.6 % of the impurities level in pharmaceutical dosage forms. Stability indicating power of the method was demonstrated by the results of forced degradation studies. The forced degradation study in solution revealed tacrolimus instability under stress alkaline, thermal, light and photolytic conditions and in the presence of a radical initiator or metal ions. The drug was stable at pH 3–5. Solid-state degradation studies conducted on amorphous tacrolimus demonstrated its sensitivity to light, elevated temperature, humidity and oxidation.


2019 ◽  
Vol 9 (4-s) ◽  
pp. 165-170
Author(s):  
Komal Gupta ◽  
Deepika Sharma ◽  
Pooja Chawla

Background: Racecadotril and Ofloxacin (RACIGYL- O) drug combination are used for the treatment of diarrhea. The drugs have been estimated individually in formulations but no method has been developed for simultaneous estimation of these two drugs as combination. Objective: To develop and validate a high performance liquid chromatography method for the simultaneous estimation of Racecadotril and Ofloxacin in tablet dosage form. Method: A WATERS C18 column (250 x 4.6mm, 5 μm) with mobile phase consisting of acetonitrile, methanol and water 40:40:20v/v (pH adjusted to 2.7 of water with ortho phosphoric acid). The flow rate was 1.0mL/min and effluents were monitored at 210nm. Results: The retention time of RAC and OFL was 4.666 min and 2.551 min respectively. The developed method was validated according to ICH guidelines with respect to specificity, linearity, accuracy, precision, robustness, Limit of Detection (LOD) and Limit of Quantification (LOQ). Conclusion: The method show good reproducibility and recovery with %RSD less than 2. So the proposed method was found to be simple, rapid, precise and accurate and useful for the determination of RAC and OFL in bulk and pharmaceutical dosage forms.   Keywords: RP-HPLC, Racecadotril, Ofloxacin, ICH guidelines.


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