Wyniki wyszukiwania - BazTech

1

Stability-indicating RP-HPLC assay for simultaneous determination of chlorpheniramine maleate and prednisolone in veterinary injection

Ali Amir, Farooq Umar, Ahmed Mahmood, Athar Muhammad Makshoof, Salman M., Arif Saira, Nadeem Kashif, Naz Hassan

Acta Chromatographica

|

2020

|

Vol. 32, no. 2

122--127

EN

The present work described a simple, rapid, sensitive, accurate, and precise method for simultaneous determination of chlorpheniramine maleate (CHRM) and prednisolone acetate (PRED) in injection samples by high-performance liquid chromatography (HPLC) coupled with UV–Vis detection. Chromatographic separation was accomplished, employing isocratic mode and a mobile phase comprised of acetonitrile and a phosphate buffer (50:50, v/v, 30 °C), adjusted to pH 3.0. The flow rate used was 1.0 mL/min on a Thermo Hypersil ODS C18 column (5 μm, 4.6 × 250 mm), and the injection volume of sample was 20 μL. Analysis of CHRM and PRED was performed at a wavelength of 254 nm. The runtime for analysis was 12.5 min, and the retention times of CHRM and PRED were found to be 2.81 and 5.07 min, respectively. The calibration graph showed linearity over the concentration range 10–70 μg/mL for CHRM and 20–140 μg/mL for PRED with a coefficient of determination (R2) ≥0.9986. Repeatability and reproducibility (expressed as % RSD) were lower than 1.72 and 1.47%, respectively. The proposed HPLC method was demonstrated to be simple and rapid for the determination of CHRM and PRED in injection formulation, providing recoveries between 101.6–102.3%, whereas complete separation of degradation products, from analyte under investigation, provided the specificity of the proposed HPLC method.

2

Total error-based validation including the experimental design-based robustness evaluation of a stability-indicating method for the simultaneous quantification of hydrochlorothiazide and valsartan in tablet formulations

Elkarbane M., Amood M., Bouchafra H., Azougagh M., Cherrah Y., Hubert Ph., Heyden Y., Bouklouze A.

Acta Chromatographica

|

2015

|

Vol. 27, no. 2

195--214

EN

A gradient reversed phase high-performance liquid chromatography (RP-HPLC) method with ultraviolet (UV) detection to analyze hydrochlorothiazide (HCT) and valsartan (VS) simultaneously in a tablet formulation during forced degradation studies was developed. This method was validated using a novel approach, namely, the accuracy profile or total errors approach. The robustness of the method was evaluated using a Plackett-Burman design for eight factors. The algorithm of Dong was applied to determine the significant factor effects. The validation results showed that the method is precise (RSD: 1.14% for HCT and 0.43% for VS) and accurate (mean recovery: 99.90% for HCT and 99.98% for VS). On the other hand, the results of the robustness study showed that the type of column was the important factor which affects a number of responses, namely, the asymmetry factor (AF), retention time (RT), and resolution (RS). However, the assay results were not affected; therefore, the method can be considered robust. Finally, the method was applied to study the stability of HCT and VS under forced conditions. Significant results were obtained with basic hydrolysis, oxidation, and thermal stress, while the accelerated and acidic conditions did not affect the stability of HCT or VS.

3

Stress degradation studies on aliskiren and the development of a sensitive stability-indicating MEKC method

Sangoi M. S., Wrasse-Sangoi M., Hurtado F. K., Rolim C. M. B.

Acta Chromatographica

|

2013

|

Vol. 25, no. 4

711--724

EN

A sensitive, fast, and stability-indicating micellar electrokinetic chromatographic (MEKC) method was developed and validated for the analysis of aliskiren (ALI) in tablets using nimesulide as internal standard (IS). Optimal conditions for the separation of ALI and its degradation products were investigated. The method employed 60 mM Tris buffer and 50 mM anionic detergent sodium dodecyl sulfate (SDS) solution at pH 9.8. MEKC method was performed on a fused-silica capillary (50 μm id; effective length, 40 cm). The capillary temperature was maintained at 35°C, and the applied voltage was 30 kV, with detection by photodiode array (PDA) detector set at 204 nm. The method was validated in accordance with the International Conference on Harmonisation (ICH) requirements. The stability-indicating capability of the method was established by enforced degradation studies combined with peak purity assessment using PDA detection. The method was linear over the concentration range of 5–150 μg mL -1 (r2 = 0.9996) of ALI. Intraday and interday precision and accuracy evaluated by relative standard deviation, respectively, were lower than 2%. The limit of detection was 1.31 μg mL -1. The method proved to be robust by a one-variable-at-a-time evaluation. The proposed MEKC method was successfully applied for the quantitative analysis of ALI in tablets to support the quality control.

4

Development and validation of HPTLC method for the estimation of diosgenin in In Vitroculture and rhizome of Dioscorea deltoidea

Amir M, Ahmad A., Siddique N. A, Mujeeb M, Ahmad S., Siddique W. A

Acta Chromatographica

|

2012

|

Vol. 24, no. 1

111--121

EN

A new simple, accurate, selective, precise, economical and stability-indicating high-performance thin layer chromatographic method for the analysis of diosgenin in callus and rhizome of Dioscorea deltoidea was developed and validated. The method was developed on TLC aluminium plates precoated with silica gel 60F254 using solvent system petroleum ether-isopropanol (12:1, v/v), which gives a compact spot of diosgenin (RF value 0.76 ± 0.02). Densitometric analysis of diosgenin was carried out in the absorbance mode at 366 nm after spraying with methanolic sulphuric acid. The linear regression analysis data for the calibration plots showed good linear relationship with r2 = 0.991 and 0.995 for diosgenin with respect to peak height and peak area, respectively, in the concentration range of 100–1000 ng per spot. The limits of detection and quantification for diosgenin were 16.58 and 50.25 ng per spot. The proposed method was applied for determination of diosgenin in rhizome of D. deltoidea (0.047% w/w) as well as in in vitro culture (callus) (0.092% w/w). Statistical analysis proves that the method is repeatable, selective and accurate for the estimation of diosgenin in D. deltoidea. The developed method effectively resolved the diosgenin in D. deltoidea; hence, it can be employed for routine analysis as a stability indicating method.

5

Development and validation of a stability-indicating LC-UV method for the determination of doripenem and biapenem in pharmaceutical dosage forms

Cielecka-Piontek J., Krause A, Zalewski P., Lunzer A, Jelińska A.

Acta Chromatographica

|

2012

|

Vol. 24, no. 2

207--219

EN

A stability-indicating LC assay method was developed and validated for the quantitative determination of doripenem and biapenem in pharmaceutical dosage forms in the presence of degradation products formed during forced degradation studies. An isocratic RP-HPLC method was developed with a C-18 (250 mm × 4.6 mm, 5 μm) column and 12 mM ammonium acetate-acetonitrile (96:4 υ/υ) as mobile phase. The flow rate of the mobile phase was 1.0 mL min-1 for doripenem and biapenem. The determination was carried out at the wavelength of 295 nm. The carbapenems were subjected to stress conditions of degradation in aqueous solutions including hydrolysis, oxidation, photolysis, and thermal degradation. The developed method was validated with respect to linearity, accuracy, precision, selectivity, and robustness.

6

Validated stability-indicating HPLC method for analysis of gemifloxacin in tablet formulations

Sharif S, Khan I. U., Sheikh T. A, Sharif Y, Ashfaq M.

Acta Chromatographica

|

2011

|

Vol. 23, no. 1

95--107

EN

A stability-indicating reversed-phase high-performance liquid chromatographic method has been developed for analysis of gemifloxacin in tablet formulations. When the drug was subjected to forced degradation under acidic, basic, thermal, oxidative, and photolytic conditions, the degradation products produced were successfully separated on a 250 mm × 4.6 mm, 5-μm particle, C18 column with ammonium acetate buffer (pH 2.7; 0.05 M)-acetonitrile 70:30 (υ/υ) as mobile phase at a flow rate of 0.7 mL min-1. Diode-array detection was performed at 272 nm. The method was validated in accordance with ICH guidelines. Response was a linear function of concentration over the range 0.256–128 μg mL-1 (correlation coefficient 0.9990). The limits of detection and quantification were 10 and 30 ng mL-1, respectively. Separation of gemifloxacin from its stress-induced degradation products and excipients was adequate; resolution was >1.5 within 11 min. The purity index for the gemifloxacin peak after all types of stress was >0.999, indicating complete separation of the analyte peak from the degradation products. The method can therefore be regarded as stability-indicating. It is rapid, and suitable for purity and assay determination not only for routine quality control but also in stability studies.

7

Stability-indicating liquid chromatographic method for analysis of pitavastatin calcium in tablet dosage forms

Panchal H. J, Suhagia B. N

Acta Chromatographica

|

2011

|

Vol. 23, no. 1

81--94

EN

A simple, specific, sensitive, precise, accurate, and robust stability-indicating reversed-phase liquid chromatographic (LC) method has been established for analysis of pitavastatin calcium in tablet dosage forms. LC separation was achieved on a 250 mm × 4.6 mm i.d., 5-μm particle, C18 column with acetonitrile-water-triethylamine 80:19.8:0.2 (υ/υ), adjusted to pH 3.5 ± 0.05 with orthophosphoric acid as isocratic mobile phase at a flow rate of 1.5 mL min-1. Detection, with a photodiode-array detector, was at 238 nm, the wavelength of maximum absorbance in a spectrum obtained from its solution in methanol. The retention time was approximately 5.70 min. The method was validated for linearity, accuracy, precision, limits of detection and quantification, and robustness. Quantification was performed over the concentration range 0.1–2.5 μg mL-1. Mean recovery was 100.26 ± 0.75%. The limit of detection (LOD) was 0.0055 µg mL-1. The method was successfully used for analysis of pitavastatin calcium in tablets and for stability studies, because the method separates pitavastatin calcium from its degradation products and from excipients.

8

A validated stability-indicating method for simultaneous analysis of mevastatin and pravastatin in fermentation broth during bioconversion by Actinomadura macra

Ahmad A., Panda B. P, Mujeeb M

Acta Chromatographica

|

2011

|

Vol. 23, no. 1

121--131

EN

A simple, accurate, selective, precise, economical, and stability-indicating high-performance thin-layer chromatographic method for simultaneous analysis of mevastatin and pravastatin in fermentation broth has been established and validated. Compounds were separated on aluminium foil TLC plates precoated with silica gel 60F254; the mobile phase was toluene-ethyl acetate-formic acid 3:2:1 (v/v), which gave compact bands of mevastatin and pravastatin (RF 0.48 ± 0.02 and 0.31 ± 0.02, respectively). Detection at 237 nm resulted in r = 0.992 and 0.995 for mevastatin and r = 0.995 and 0.994 for pravastatin, for peak height and peak area, respectively. The limits of detection and quantification for mevastatin were 20.1 and 60.8 ng per band, and for pravastatin 19.2 and 58.3 ng per band, respectively. The method enabled effective quantification of mevastatin and pravastatin in the fermentation broth of Actinomadura macra and can therefore be used as a stability-indicating method for routine analysis of these compounds during bioconversion.

9

Development and validation of a stability-indicating HPTLC method for analysis of nebivolol hydrochloride and hydrochlorothiazide in the bulk material and in pharmaceutical dosage forms

Damle M. C., Topagi K. S., Bothara K. G.

Acta Chromatographica

|

2010

|

Vol. 22, no. 3

433--443

EN

An accurate, sensitive, rapid, and precise stability-indicating high-performance thin-layer chromatographic (HPTLC) method for analysis of nebivolol hydrochloride and hydrochlorothiazide as the bulk drug and in tablets has been developed and validated. Optimum separation was achieved on silica gel 60 F 254 plates with ethyl acetate-methanol-acetic acid 6.5:1:0.5 ( υ/υ ) as mobile phase. Detection and quantification were performed at 280 and 270 nm for nebivolol hydrochloride and hydrochlorothiazide, respectively. The drugs get resolved with R F 0.46 ± 0.02 and 0.78 ± 0.02 for nebivolol hydrochloride and hydrochlorothiazide, respectively. The drugs were subjected to hydrolysis under acidic, basic, and neutral conditions, oxidation, heat, and photolysis as stress conditions. Peaks of degradation products were observed when the drugs were subjected to oxidative stress. Acidic conditions were also found to affect the tablet sample substantially. The degradation products resulting from stress conditions did not interfere with the drug peak. The method can be used for stability testing of these drugs during stability studies.

10

Stability-indicating LC method for determination of tadalafil in bulk drug and pharmaceutical dosage form

Mathpati M.M., Sangshetti J.N., Rane V.P., Patil K.R., Shinde D.B.

Chemia Analityczna

|

2009

|

Vol. 54, No. 4

679-689

EN

A novel stability-indicating LC assay method for quantitative determination oftadalafil in bulk drug and pharmaceutical dosage form in the presence of forced-degradation products was developed and validated. An isocratic reversed phase LC method was developed to separate the drug from its degradation products using a Zorbax SB-C18 column and water-acetonitrile mixture as a mobile phase. Detection was carried out at the wavelength of 235 nm. Tadalafil was subjected to stress conditions in order to perform its hydrolytic (acid, base), oxidative, photolytic, and thermal degradation. Degradation oftadalafil was observed in the presence of acid, base, and 30% H2O2. The drug was found to be stable under other stress conditions. The signals of degradation products were well-resolved from the main peak oftadalafil. Percentage recovery oftadalafil in pharmaceutical dosage form ranged from 98.89% to 101.25%. The developed method was validated with respect to linearity, accuracy (recovery), precision, specificity, and robustness. Forced degradation studies proved the stability-indicating power of the method.

PL

Opracowano i zwalidowano nową metodę ilościowego oznaczania tadalafilu za pomocą chromatografii cieczowej, w obecności produktów rozkładu, pozwalającą na ocenę stabilności surowca i formy farmaceutycznej. Zastosowanie kolumny Zorbax SB-C18 i izokratycznej mieszaniny woda —acetonitryl pozwalało na rozdzielenie leku od produktów rozkładu. Detekcję przeprowadzono przy długości fali 235 nm. Tadalafil poddano ekstremalnym warunkom w celu uzyskania hydrolitycznych (kwas, zasada), oksydatywnych. tbtolitycznych i termicznych produktów rozkładu. Rozkład tadalafilu obserowwoano w obecności kwasów, zasad i 30% H,O2. Lek okazał się trwały w pozostałych ekstremalnych warunkach. Sygnały produktów rozkładu były dobrze oddzielone od głównego piku tadalafilu. Odzysk w przypadku badania postaci farmaceutycznej wynosił od 98,89% do 10 l ,25%. Opacowana. metodę zwalidowano w zakresie liniowości, dokładności (odzysku), precyzji, specyficzności i odporności na zmiany warunków otoczenia. Badania rozkładu w warunkach ekstremalnych wykazały przydatność opracowanej metody do oceny stabilności leku.

11

Stability-indicating HPTLC method for quantitation of quetiapine fumarate in the pharmaceutical dosage form

Dhaneshwar S. R., Patre N. G., Mahadik M. V.

Acta Chromatographica

|

2009

|

Vol. 21, no. 1

83-93

EN

A sensitive, selective, precise, and stability-indicating HPTLC method for quantitative analysis of quetiapine fumarate both as the bulk drug and in formulations has been established and validated. The stationary phase was silica gel and the mobile phase toluene-methanol 8:2 (v/v). This system gave compact bands for quetiapine fumarate ( R F 0.37 š 0.02). Densitometric analysis of quetiapine fumarate was performed in absorbance mode at 254 nm. There was no chromatographic interference from tablet excipients. Quetiapine fumarate was subjected to acid and alkaline hydrolysis, oxidation, and photodegradation. The drug is susceptible to all these treatments. The degradation products were well resolved from the pure drug with substantially different R F values. The method was validated for linearity, precision, accuracy, selectivity, and specificity in accordance with ICH guidelines. Because the method can effectively separate the drug from its degradation products, it can be used as a stability indicating method.

12

Development and validation of a stability-indicating LC-UV method for rapid analysis of buspirone in pharmaceutical dosage forms

Azeem A., Rizwan M., Ahmad F. J., Iqbal Z., Khar R. K., Aqil M, Talegaonkar S.

Acta Chromatographica

|

2009

|

Vol. 21, no. 2

283--297

EN

An accurate, sensitive, precise, rapid and isocratic reversed-phase HPLC (RPHPLC) method for analysis of buspirone in the bulk drug and in solid dosage formulations has been developed and validated. The best separation was achieved on a 250 mm × 4.6 mm i.d., 5-μm particle, RP C 18 column with 70:30 ( υ/υ ) methanol-0.01 M sodium dihydrogen phosphate buffer (pH 3.5) as mobile phase at a flow rate of 0.8 mL min -1. UV detection was at 244 nm. Response was a linear function of concentration over the range 0.05–20 μg mL -1 ( r = 0.9998) and the limits of detection and quantitation were 3.7 and 11.3 ng mL -1, respectively. The method was validated in accordance with ICH guidelines. The drug was subjected to oxidative, hydrolytic, photolytic, and thermal stress. Degradation products produced as a result of this stress did not interfere with detection of buspirone and the assay can thus be regarded as stability-indicating. The method was used for quantification of buspirone in commercial buspirone tablets and to check content uniformity. The excipients present in the formulation did not interfere with the assay. The method is suitable for application in quality-control laboratories, because it is simple and rapid with good accuracy and precision.