scholarly journals A new gas chromatographic method development and validation for the simultaneous determination of ibuprofen and caffeine in bulk and pharmaceutical dosage form

2020 ◽  
Vol 6 (1) ◽  
Author(s):  
Celine Zambakjian ◽  
Amir Alhaj Sakur
Keyword(s):  
Simultaneous Determination ◽  
Dosage Form ◽  
Chromatographic Method ◽  
Internal Standard ◽  
Pharmaceutical Dosage Form ◽  
Methyl Paraben ◽  
Ich Guidelines ◽  
System Suitability ◽  
Gas Chromatographic Method

Abstract Background Ibuprofen is a nonsteroidal anti-inflammatory drug (NSAID) that has analgesic, anti-inflammatory, and antipyretic properties. Caffeine is one of the most common adjuvant analgesic drugs which is combined with ibuprofen in commercially available formulations. Combining analgesics offers the possibility of increasing effectiveness without increasing dose and therefore risk. Prescribing ibuprofen and caffeine together is common in clinical practice. This is the first work reporting a new and validated gas chromatographic method for the simultaneous determination of ibuprofen and caffeine in bulk and pharmaceutical dosage form. The separation was performed on a TRB-17 column (30.00 m in length, 0.25-mm ID, and 0.25-μm df). Detection was carried out using a flame ionization detector (FID). Methyl paraben was used as an internal standard. The injection volume was 1 μL with 1:50 split ratio using nitrogen as a carrier gas at a flow rate of 1 mL/min. The oven temperature was programmed at 150 °C for 0.5 min, with a rise of 10 °C/min up to 250 °C. The injector temperature was 280 °C, and the detector temperature was 300 °C. The validation of the method including linearity, range, detection limit (DL), quantitation limit (QL), accuracy, precision, specificity, system suitability, and robustness was carried out utilizing International Conference on Harmonization (ICH) guidelines. Results The retention times of methyl paraben, ibuprofen, and caffeine were 1.687, 2.594, and 4.031 min, respectively. The method was linear in the range of 1000–7000 μg/mL for ibuprofen and 162.5–1137.5 μg/mL for caffeine with a correlation coefficient of 0.9999 for both drugs. The DL was found to be 131.68 μg/mL and 15.74 μg/mL for ibuprofen and caffeine, respectively, whereas QL was found to be 399.02 μg/mL for ibuprofen and 47.68 μg/mL for caffeine. The accuracy of the method was validated by mean percentage recovery, which was found to be in the acceptable range. The precision study results of the new method were less than the maximum allowable limit percentage of relative standard deviation %RSD ≤ 2.0. The specificity was evaluated by the standard edition method, and the results of the recovery data showed that excipients do not affect the accuracy of the proposed method. The results of system suitability and robustness tests were also within the acceptable limits. Conclusion The first reported method for simultaneous determination of ibuprofen and caffeine by gas chromatography in bulk and combined dosage form was carried out in this work. The developed method gave a good separation of the drugs and internal standard. The analytical performance of the method was statistically validated as per ICH guidelines, and satisfactory results were obtained. The proposed method can be easily adopted for the routine analysis of ibuprofen and caffeine.

Simultaneous determination of Sulphadoxine and Pyrimethamine by taking Tolterodine as an internal standard in Pharmaceutical dosage form by RP-HPLC

2021 ◽  
pp. 145-150
Author(s):  
Sushil D. Patil ◽  
Pravin B. Shelke ◽  
Priti Aher ◽  
Maswood Ahmed Hafizur Rahman
Keyword(s):  
Simultaneous Determination ◽  
Dosage Form ◽  
Internal Standard ◽  
Hplc Method ◽  
Control Analysis ◽  
Pharmaceutical Dosage Form ◽  
Quality Control Analysis ◽  
Rp Hplc ◽  
Sulphadoxine Pyrimethamine

A simple, rapid, economic, sensitive and precise HPLC method has been developed for the simultaneous determination of Sulphadoxine and Pyrimethamine in pharmaceutical dosage form by taking Tolterodine as an internal standard. The method was carried out using Phenomenex C18 (4.6ID × 250mm; 5µm) column and mobile phase comprised of methanol and Phosphate Buffer in proportion of ratio 60:40 v/v. The flow rate was 1.0mL/min and detection was carried out at 276nm. The retention time of Sulphadoxine, Pyrimethamine and Tolterodine were found to be 2.967, 4.058 and 6.908 respectively. Linearity of Sulphadoxine and Pyrimethamine in the range of 2 to 12μg/mL and 4 to 24μg/mL respectively. The % recoveries of Sulphadoxine and Pyrimethamine were found to be in between 99.93% to 99. 96 % respectively. The proposed method is suitable for the routine quality control analysis for simultaneous determination of Sulphadoxine and Pyrimethamine was in bulk and pharmaceutical dosage form.

scholarly journals DETERMINATION OF CHROMATOGRAPHIC ASSAY AND VALIDATION OF OFLOXACIN IN BULK AND PHARMACEUTICAL DOSAGE FORM

2018 ◽  
Vol 11 ◽  
Author(s):  
Sumithra M
Keyword(s):  
Mobile Phase ◽  
Dosage Form ◽  
Chromatographic Method ◽  
Assay Method ◽  
Reverse Phase ◽  
Pharmaceutical Dosage Form ◽  
Ich Guidelines ◽  
Validation Parameters ◽  
The Mean

Objective: The objective of the study is simple, sensitive; eco-friendly reverse phase chromatographic method has been developed and validated for the quantitative determination of ofloxacin in bulk and marketed formulation. Method: The developed method was done using Hypersil silica C18 (250 mm × 4.6 mm, 5 μ particle size) as column and the mobile phase is containing water and methanol in the ratio of (10:90) vol/vol. The mobile phase pass at 1 ml/min flow rate and the eluted solution is measured at 270 nm using a PDA detector. Results: The assay method is linear from the concentration range of 5–30 μg/ml. The corelation coefficient is 0.9998. The mean percentage recovery for the developed method is found to be in the range of 98.4–100.6%. The developed method complies robustness studies. Conclusion: The validation of the developed method was done by as per the ICH guidelines. It obeys the linearity, accuracy, precision, and robustness studies. Validation parameters are within the limitations. The results of the developed process indicated the reverse phase chromatographic method is simple, accurate as well as precise, rapid and eco-friendly method for routine analysis of ofloxacin in bulk and its pharmaceutical dosage form.

VALIDATED HPTLC METHOD FOR SIMULTANEOUS DETERMINATION OF OLMESARTAN MEDOXIMIL AND METOPROLOL SUCCINATE IN TABLET DOSAGE FORM

INDIAN DRUGS ◽  
2012 ◽  
Vol 49 (10) ◽  
pp. 13-17
Author(s):  
V. V Kunjir ◽  
◽  
S. B. Jadhav ◽  
A. J Purkar ◽  
P. D. Chaudhari
Keyword(s):  
Simultaneous Determination ◽  
Mobile Phase ◽  
High Performance ◽  
Dosage Form ◽  
Chromatographic Method ◽  
Metoprolol Succinate ◽  
Ich Guidelines ◽  
Tablet Dosage ◽  
Hptlc Method

A high performance thin layer chromatographic method has been developed for the simultaneous determination of olmesartan medoximil and metoprolol succinate from tablet dosage form. The mobile phase consisting of water-methanol-ammonium sulphate (4.5:4.5:1.5 v/v/v) and wavelength of detection 233 nm was used. The developed method was validated as per ICH guidelines.

Therapeutic Monitoring of Anticonvulsant Drugs: Gas-Chromatographic Simultaneous Determination of Primidone, Phenylethylmalonamide, Carbamazepine, and Diphenylhydantoin

1975 ◽  
Vol 21 (11) ◽  
pp. 1658-1662 ◽  
Author(s):  
Charles J Least ◽  
George F Johnson ◽  
Harvey M Solomon
Keyword(s):  
Simultaneous Determination ◽  
Standard Method ◽  
Chromatographic Method ◽  
Limit Of Detection ◽  
Internal Standard ◽  
Normal Serum ◽  
Therapeutic Monitoring ◽  
The Mean ◽  
Gas Chromatographic Method

Abstract We describe a sensitive and precise gas-chromatographic method in which benzylmalonate methylester monoamide is used as the internal standard for the simultaneous determination of primidone, phenylethylmalonamide, carbamazepine, and diphenylhydantoin. The trimethylsilyl derivatives of the anticonvulsants are well separated from each other and from normal serum constituents. The lower limit of detection for each drug is 0.5 mg/liter when 1 ml of serum is analyzed. Withinrun precision (CV), established by analysis of 10 replicates, was as follows: primidone (5.4 mg/liter), 2.6%; phenylethylmalonamide (5.5 mg/liter), 1.6%; diphenylhydantoin (6.6 mg/liter), 3.8%; and carbamazepine (10.4 mg/liter), 3.2%. Fifty specimens were analyzed for primidone and 35 for diphenylhydantoin by a standard gas-chromatographic method involving on-column methylation and by the procedure we have developed. The mean value observed for primidone with the on-column alkylation procedure was 9.3 mg/liter and with our procedure was 9.6 mg/liter. When values for our assay were regressed against values for the standard method, the slope of the least-squares line was 0.936, the intercept was 1.00 mg/liter, and r was 0.939. The mean values observed for diphenylhydantoin by on-column methylation and with our procedure were both 12.6 mg/liter. When values for our assay were regressed against the standard method, the slope of the leastsquares line was 0.944, the intercept was 0.3 mg/liter, and r was 0.988

Antipyrine metabolism in man: simultaneous determination of norantipyrine and 4-hydroxyantipyrine in urine by gas chromatography

1980 ◽  
Vol 58 (1) ◽  
pp. 17-21 ◽  
Author(s):  
T. Inaba ◽  
N. E. Fischer
Keyword(s):  
Gas Chromatography ◽  
Simultaneous Determination ◽  
Chromatographic Method ◽  
Internal Standard ◽  
Antipyrine Metabolism ◽  
Drug Oxidation ◽  
Gas Chromatographic Method

A gas chromatographic method was developed to determine metabolites of antipyrine, norantipyrine (NORA), and 4-hydroxyantipyrine in urine using p-methylated NORA as internal standard. This method requires no derivatization and has ample sensitivity to determine these metabolites in urine after ingestion of antipyrine, a compound widely used as a hepatic probe of drug oxidation.

A Green Liquid Chromatographic Method For The Simultaneous Determination of Chlorpheniramine Maleate, Pseudoephedrine Hydrochloride and Propyphenazone

2019 ◽  
Vol 15 (6) ◽  
pp. 635-641
Author(s):  
Nadia M. Mostafa ◽  
Ghada M. Elsayed ◽  
Nagiba Y. Hassan ◽  
Dina A. El Mously
Keyword(s):  
Simultaneous Determination ◽  
Mobile Phase ◽  
Dosage Form ◽  
Chromatographic Method ◽  
Green Analytical Chemistry ◽  
Chlorpheniramine Maleate ◽  
Accuracy And Precision ◽  
Liquid Chromatographic Method ◽  
Liquid Chromatographic

Background:The concept of green analytical chemistry prevails due to the growing environmental pollution.Objective:Our attempts are to develop simple and eco-friendly method which is non-harmful to the environment by producing minimal waste. In this context, a green liquid chromatographic method was applied for the simultaneous determination of chlorpheniramine maleate, pseudoephedrine hydrochloride and propyphenazone in their combined dosage form.Methods:Separation was carried out using X select HSS RP C18 analytical column (250 × 4.6 mm, 5μm) using methanol - 0.02 M phosphate buffer pH 3 - triethylamine (60:40: 0.1, by volume) as a mobile phase. The separated peaks were detected at 215 nm at a flow rate 1.0 mL/min.Results:Quantification was done over the concentration ranges of 1-25 µg/mL for chlorpheniramine maleate, 5-35 µg/mL for pseudoephedrine hydrochloride and 10-120 µg/mL for propyphenazone. The suggested method was validated with regard to linearity, accuracy and precision according to the International Conference on Harmonization guidelines with good results.Conclusion:It could be used as a safer alternative for routine analysis of the mentioned drugs in quality control laboratories.

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