Wyniki wyszukiwania - BazTech

1

High-performance thin-layer chromatographic analysis of psoralen in marketed formulations and manufactured solid lipid nanoparticles (SLNs): Validation of the method

Akhtar N., Faiyazuddin Md., Mustafa G., Sultana Y., Baboota S., Ali J.

Acta Chromatographica

|

2012

|

Vol. 24, no. 4

603--613

EN

A quantitative method using precoated silica gel-60 Lichrosphere high-performance thin-layer chromatography (HPTLC) plates, automated band wise sample application, and n-hexane:acetone:formic acid (2:1:0.025 υ/υ/υ) as mobile phase, has been developed and validated for the analysis of psoralen in marketed formulations and novel solid lipid nanoparticles (SLNs). Densitometric analysis was performed at 250 nm in absorbance mode. Compact bands of psoralen were obtained at Rf 0.32 ± 0.02. The method was validated for linearity, precision, robustness, sensitivity, specificity, and recovery. Linearity (r2 = 0.995), limit of detection (8.0 ng band-1), limit of quantification (18.1 ng band) -1, recovery (98.06–99.64%), and precision (≤0.74) were satisfactory. Statistical analysis established that the developed method for quantification of psoralen in marketed formulation and from solid lipid nanoparticles is reproducible and selective.

2

Stability-indicating high-performance thin-layer chromatographic method for analysis of terbinafine in pharmaceutical formulations

Ahmad S., Jain G. K., Faiyazuddin Md., Iqbal Z., Talegaonkar S., Sultana Y., Ahmad F. J.

Acta Chromatographica

|

2009

|

Vol. 21, no. 4

631--639

EN

A new, simple, selective, precise, robust and stability-indicating high-performance thin-layer chromatographic (HPTLC) method has been established for analysis of terbinafine hydrochloride (TH) in the bulk drug and in pharmaceutical formulations. Separation was achieved on aluminium plates precoated with silica gel 60F 254 , with toluene-ethyl acetate-formic acid 4.5:5.5:0.1 ( v/v ) as mobile phase. Densitometric analysis was performed at 284 nm. Compact bands of TH were obtained at R F 0.31 ± 0.02. Linearity ( r 2 = 0.9985), limit of quantification (35 ng per band), recovery (97.6−101.6%), and precision (≤2.19) were satisfactory. The method was applicable for routine analysis and accelerated stability testing of TH in pharmaceutical drug-delivery systems. Because the method can effectively separate the drug from its degradation products, it can be used as a stability-indicating method.

3

Thin-layer chromatographic analysis of psoralen in babchi ( Psoralea corylifolia ) oil

Ali J., Akhtar N., Sultana Y., Baboota S., Ahmad S.

Acta Chromatographica

|

2008

|

Vol. 20, no. 2

277-282

EN

A simple, selective, precise, accurate, and cost-effective thin-layer chromatographic (TLC) method for analysis of psoralen in different brands of babchi (Psoralea corylifolia) oil has been developed and validated. Aluminium TLC plates precoated with silica gel 60F254 were used as the stationary phase and n-hexane-acetone-formic acid 2:1:0.025 (v/v) as mobile phase. A compact, resolved psoralen peak (RFvalue 0.32 š 0.02) was observed by densitometric analysis in absorbance mode at 250 nm. Calibration data revealed a good linear relationship (r2 = 0.9956) between peak area and concentration in the range 20-200 ng per spot. Mean š SD values of slope and intercept were 11.35 š 0.36 and 14.64 š 0.31, respectively. Statistical analysis proved the method to be a repeatable, selective, and accurate means of estimation of psoralen in different brands of babchi oil.

4

Development and validation of a stability-indicating HPTLC method for analysis of antitubercular drugs

Ali J., Ali N., Sultana Y., Baboota S., Faiyaz S.

Acta Chromatographica

|

2007

|

No. 18

168-179

EN

A simple, selective, precise, and stability-indicating high-performance thin-layer chromatographic (HPTLC) method has been established and validated for analysis of isoniazid and rifampicin both as the bulk drugs and in formulations. The compounds were separated on aluminumbacked silica gel 60 F254 plates with n-hexane–2-propanol–acetone–ammonia–formic acid, 3:3.8:2.8:0.3:0.1 (v/v) as mobile phase. This system was found to give compact spots for isoniazid and rifampicin (RF values 0.59 ± 0.02 and 0.73 ± 0.04, respectively). Densitometric analysis of isoniazid and rifampicin was performed at 254 nm. Regression analysis data for the calibration plots were indicative of good linear relationships between response and concentration over the range 100–700 ng per spot. The correlation coefficients, r2, were 0.994 and 0.997 for isoniazid and rifampicin respectively. The values of slope and intercept of the calibration plots were 3.755 ± 0.22 and 3099.1 ± 51.21, respectively, for isoniazid and 4.0957 ± 0.25 and 3567.6 ± 61.11, respectively, for rifampicin. The method was validated for precision, recovery, and robustness. The limits of detection and quantification were 20 ± 0.51 and 60 ± 1.05 ng, respectively, for isoniazid and 25 ± 0.63 and 75 ± 1.12 ng, respectively, for rifampicin. Isoniazid and rifampicin were subjected to acid, base, peroxide, and UV-induced degradation. In stability tests the drugs were susceptible to acid and basic hydrolysis, oxidation and photodegradation. Statistical analysis proved the method is repeatable, selective, and accurate for estimation of isoniazid and rifampicin. Because the method could effectively separate the drugs from their degradation products, it can be used as a stabilityindicating method.

5

A validated HPLC method for estimation of metoprolol in human plasma

Agil M., Ali A., Ahad A., Sultana Y., Najmi A. K., Saha N.

Acta Chromatographica

|

2007

|

No. 19

130-140

EN

A high-performance reversed-phase liquid chromatographic method for quantification of metoprolol tartrate (MT) in human plasma is presen-ted. A C18 column was used with acetonitrile–water–triethylamine 18:81:1 (v/v) as mobile phase and pinacidil monohydrate as internal standard (IS). UV detection was at 275 nm and MT and the IS were detected at retention times of 1.5 and 2.6 min, respectively. The method is sensitive with a li-mit of quantification of 20 ng mL-1. The calibration plot for MT in spiked plasma was linear in the concentration range 20–200 ng mL-1. Within-batch and total accuracy of the method ranged between 99.71% and 101.61%, and within-batch and total precision, expressed as the coefficient of varia-tion, was 0.20–2.13%. Recovery of MT from spiked plasma was 97.00% and the freeze–thaw and bench-top stability of samples ranged from 77.92 to 105.62%. The method can be successfully used for analysis of MT in human plasma during pharmacokinetic studies.