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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

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

Acta Chromatographica

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2022

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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.

2

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

Fouad M. A., Elkady E. F.

Acta Chromatographica

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2014

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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

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

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

Acta Chromatographica

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2012

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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.

4

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

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

Acta Chromatographica

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2012

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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.

5

Development and validation of a stability-indicating HPTLC assay method for idebenone

Rathi A. A, Dhamecha D. L, Dehghan M. H. G, Saifee M, Wakte P. S, Shelke S. D., Dongre S. H

Acta Chromatographica

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2011

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Vol. 23, no. 2

281--294

EN

A simple, selective, precise, and stability-indicating high-performance thin layer chromatographic (HPTLC) method has been established and validated for the analysis of idebenone in bulk drug and formulations. The compounds were analyzed on aluminum-backed silica gel 60 F254 plates with petroleum ether-methanol (4:1, υ/υ) as mobile phase. Densitometric analysis of idebenone was performed at 282 nm. Regression analysis data for the calibration plots were indicative of good linear relationship between response and concentration over the range of 200–600 ng per spot. The correlation coefficient (r2) was 0.989 ± 0.002. The values of slope and intercept of the calibration plots were 2.386 ± 0.0435 and 577.733 ± 19.545, respectively. The method was validated for precision, accuracy, robustness, and ruggedness. The limits of detection and quantification were 14.642 and 44.369 ng, respectively. Idebenone was subjected to acid, base, peroxide, and sunlight degradation. In stability tests, the drug was susceptible to acid and basic hydrolysis, oxidation, and photodegradation.

6

The ICH guidance in practice: Stress degradation studies on irbesartan and development of a validated stability-indicating UPLC assay

Sahu K, Patel P, Karthikeyan C, Trivedi P

Acta Chromatographica

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2010

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Vol. 22, no. 2

189--205

EN

In this research work comprehensive stress testing of irbesartan was carried out according to ICH guideline Q1A (R2), and a stability-indicating reversed-phase ultra-performance liquid chromatographic (UPLC) assay was established. The drug was subjected to acid (0.1 M HCl), neutral, and alkaline (0.1 M NaOH) hydrolytic conditions at 80°C, and to oxidative decomposition at room temperature. Photolysis was carried out by exposing the drug to sunlight (60,000–70,000 lux) for two days. The solid drug was also subjected to 50°C for 60 days in a hot-air oven. Degradation of the drug was found to occur under alkaline, acidic, and neutral hydrolytic conditions. Separation of the drug and the degradation products was successfully achieved on a BEH (bridged ethylene hybrid) C 18 column with 40:60 aqueous glacial acetic acid (0.2%)-acetonitrile as mobile phase. The flow rate and detection wavelength were 0.1 mL min -1 and 229 nm, respectively. The method was validated and response was found to be linear in the drug concentration range 10–50 μg mL -1 The mean values (±RSD, %) of slope, intercept, and correlation coefficient were 32102 (± 0.0535), 1295 (± 3.02), and 0.9998 (± 0.0493), respectively. RSD in intra-day and inter-day precision studies was <1%. Recovery of the drug from a mixture of degradation products was between 99.26 and 100.01%. The method was specific to the drug, selective to degradation products, and robust. PDA purity test also confirmed the specificity of the method.

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Stability-indicating HP TLC method for determination of donepezil hydrochloride in bulk drug and pharmaceutical dosage form

Ali J., Ali M., Ahmad S., Bhavna M.

Chemia Analityczna

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2009

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Vol. 54, No. 6

1501-1516

EN

A sensitive, selective, precise and stability-indicating high-performance thin layer chroma-tographic (HPTLC) method for analysis of donepezil hydrochloride (DH) as bulk drug and in formulations was developed and validated. TLC aluminum plates pre-coated with 60 F-254 silica gel (20 x 10 cm) were used as the stationary phase. The solvent system consisted of butanol-water-glacial acetic acid (5:4:1, v/v/v). Densitometric analysis of DH was carried out in the absorbance mode at 260 nm. This system was found to give compact spots for DH (RF= 0.53 š 0.03 for six replicates). DH was subjected to acidic and alkaline hydrolysis, oxidation, dry and wet heat treatment, and photodegradation; under all these conditions the drug underwent degradation. Degradation products had significantly different RF values and thus were well separated from the pure drug. The method was validated with respect to linearity, precision, robustness, limit of detection (LOD), limit of quantification (LOQ), ruggedness and accuracy. Linearity was observed in the range 50—1000 ng per spot with a significantly high value of the correlation coefficient r2 = 0.9979; 95% confidence interval of r2 was 0.9908-0.9995. The mean S.E. value of the slope was 0.1316 with respect to the peak area. LOD and LOQ were 15.40 and 50.90 ng per spot, respectively. Statistical analysis proved that the method was repeatable and specific for the estimation of the studied drug. As the method could effectively separate the drug from its degradation products, it can be employed as a stability-indicating procedure.

PL

Opracowano i zwalidowano czułą, selektywną i precyzyjną, metody wysokosprawnej TLC do analizy chlorku donezepilu (DH) jako substancji chemicznej i w preparatach. Metoda umożliwia również ocenę trwałości leku. Zastosowano płytki na podłożu aluminiowym o wymiarach 20 * l O cm, pokryte żelem krzemionkowym 60 F-254. Jako eluent zastosowano butanol-wodę-lodowaty kwas octowy (5:4:1, v/v/v). DH wykrywano densytometrycznie przy 260 nm. W tych warunkach otrzymano zwarte plamki DH z RF= 0,53 š 0,03 dla sześciu powtórzeń. DH poddawano hydrolizie kwasowej i zasadowej, utlenianiu, ogrzewaniu na mokro i na sucho oraz naświetlaniu. We wszystkich tych przypadkach lek ulegał degradacji. Produkty degradacji miały wyraźnie różne wartości RFi były dobrze oddzielone od wyjściowego leku. Metodę walidowano uwzględniając liniowość, precyzje, odporność, wykrywalność, oznaczalność i dokładność. Liniowość obserwowano w zakresie 50—1000 ng w plamce, ze współczynnikiem korelacji r2 = 0,9979. Średnia wartość nachylenia wynosiła 0,1316 w odniesieniu do powierzchni piku. Wykrywalność i oznaczalność wynosiła odpowiednio 15,40 i 50,90 ng w plamce. Za pomocą analizy statystycznej wykazano, że metoda oznaczania badanego związku jest powtarzalna i specyficzna, umożliwia też oddzielanie leku od produktów jego degradacji, dzięki czemu może być zastosowana do badania trwałości leku.