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Stability-indicating RP-HPLC method for analysis of the antibiotic doripenem in pharmaceutical formulation—comparison to UV spectrophotometry and microbiological assay

100%

Mantovani L. , Sayago C. T. M. , Camargo V. B. , Silveira V. F. , Garcia C. V. , Schapoval E. E. S. , Mendez A. S. L.

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tom Vol. 24, no. 3

367--382

EN

A stability-indicating liquid chromatographic (LC) method with UV detection was developed for the determination of doripenem in the marketed formulation (Doribax® 500 mg, powder for injection). A forced degradation study was conducted according to available guidelines and main references. Thermal, oxidizing, acidic and basic stress conditions were assayed to show the stability-indicating power of the method. Chromatographic separation was achieved using an isocratic elution method in a reversed-phase system using a mobile phase prepared from phosphate buffer and acetonitrile. Extensive degradation was observed under thermal, oxidative and basic treatment, and the products formed were detected without interference in the analysis of doripenem. To verify the efficiency of chromatographic run, the system suitability was studied. The theoretical plates (N = 5498.3) and tailing factor (tf = 0.951) were constant during repeated injections. The retention time of doripenem was 7.35 min and the method was validated within the concentration range 5–50 μg mL-1 (r = 0.999). Adequate results were obtained that indicate repeatability (RSD % = 1.03–1.37), inter-day precision (RSD % = 0.51) and accuracy. In comparison to spectrophotometric and microbiological methods, statistical analysis showed no significant difference between the obtained results. The proposed method was successfully applied to doripenem quantification, showing it is applicable to determine the antibiotic in the presence of degradation products and also that is a reliable method for routine analysis.

2

Forced degradation study and validated stability-indicating RP-LC method for determination of nilotinib in bulk and capsules

88%

Fouad M. A. , Elkady E. F.

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2014

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tom Vol. 26, no. 4

637--647

EN

A simple, selective, and precise stability-indicating reversed-phase liquid chromatographic method was developed and validated for the determination of nilotinib. Nilotinib was subjected to acid and alkali hydrolysis, oxidation, thermal, and photo-degradation. The degradation products were well separated from the pure drug. The method was based on isocratic elution of nilotinib and its degradation products on reversed phase C18 column (100 mm × 4.6 mm, 3.5 μm) — Zorbax Eclipse Plus using a mobile phase consisting of 10 mM KH2PO4:acetonitrile (54.5:45.5%, v/v) at a flow rate of 1 mL min−1. Quantitation was achieved with UV detection at 265 nm. Linearity, accuracy and precision were found to be acceptable over the concentration range of 0.1–80 μg mL−1. The drug was found to be susceptible to acid and base hydrolysis but resistant to oxidation, dry heat degradation, and photodegradation. The proposed method was successfully applied to the determination of nilotinib in bulk and in its pharmaceutical preparation.

3

Sensitive and validated TLC densitometry method coupled with fluorescence detection for quantitative determination of the newly co-formulated drugs, celecoxib and amlodipine besylate in tablet dosage form

88%

Rizk M. , Toubar S. , Ramzy E. , Helmy M.

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tom Vol. 34, no. 2

150--161

EN

New, sensitive, rapid, cost-effective, and validated stability-indicating thin layer chromatographic (TLC) method coupled with fluorescence (FL) detection was developed for the quantitative analysis of celecoxib (CEL) and amlodipine besylate (AMLO) in their laboratory prepared binary mixture using the non-fluorescent TLC silica gel 60 plates. Ethyl acetate: diethylamine: 1-propanol (9:1:0.2, V/V) was used as a developing system. The retention factor (Rf) for each drug was 0.80 ± 0.03 and 0.44 ± 0.01 for CEL and AMLO, respectively. The plates were excited at 264 nm for the simultaneous FL measurement of CEL and AMLO, the calibration curves were linear over a concentration ranges of 30.0–300.0 ng/band and 15.0–150.0 ng/band with mean percentage recoveries of 99.80 ± 0.85 and 99.80 ± 0.77 For CEL and AMLO, respectively. The developed method was applied for the stability studies of the cited drugs in their laboratory prepared binary mixture and the forced degradation products were determined when present in presence of the pure drugs so the method can be considered as a stability-indicating one and it was validated as per ICH guidelines and proved to be accurate and precise.

4

Validated stability-indicating RP-HPLC UV method for simultaneous determination of metformin and repaglinide

75%

Joshi S. S. , Nahire R. R. , Shastri N. R. , Surendranath K. V. , Satish J.

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tom Vol. 24, no. 3

419--432

EN

A simple, rapid, precise, and accurate, stability-indicating reversed phase high performance liquid chromatographic method was developed and validated for simultaneous determination of metformin HCl and repaglinide. The chromatographic separation was achieved on YMC Pack AM ODS (5 μm, 250 mm length × 4.6 mm i.d.) column at a detector wavelength of 210 nm, using an isocratic mobile phase consisting of methanol and 10 mM potassium dihydrogen phosphate buffer (pH 2.5) in a ratio of 70:30 v/v at a flow rate of 1 mL min-1. The retention times for metformin and repaglinide were found to be 2.6 and 11.3 min, respectively. The drugs were exposed to thermal, photolytic, hydrolytic, and oxidative stress conditions, and the stressed samples were analyzed by the proposed method. Validation of the method was carried out as per International Conference on Harmonization (ICH) guidelines. Linearity was established for metformin and repaglinide in the range of 5–200 μg mL-1 and 1–200 μg m-1. L, respectively. The limits of detection were 0.3 μg mL-1 and 0.13 μg mL-1 for metformin and repaglinide, respectively. The method was found to be specific and stability-indicating as no interfering peaks of degradants and excipients were observed. The proposed method is hence suitable for application in quality-control laboratories for quantitative analysis of both the drugs individually and in combination, since it is simple and rapid with good accuracy and precision.