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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

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2012

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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.

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Quantitative estimation of mimosine in anti-psoriatic ayurvedic formulation containing whole plant extract of Mimosa pudica Linn. by validated isocratic RP-HPLC method

Musthaba S, Athar M. T, Kamal Y. T, Ahmad S., Ali J., Baboota S.

Acta Chromatographica

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2011

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Vol. 23, no. 3

531--538

EN

In this chapter, an isocratic reverse phase HPLC determination of mimosine was developed and validated in an anti-psoriatic topically applied formulation “Lajjalu”. The chromatography was performed on a C18 column with water-orthophosphoric acid (98.8:0.2, υ/υ) as a mobile phase with a pH of 3.0 at a flow rate of 1.0 mL min-1. Detection was performed at 284 nm, and a sharp peak was obtained for mimosine at a retention time of 2.62 ± 0.01 min. Linear regression analysis data for the calibration plot showed a good linear relationship between response curve and concentration in the range of 0.050–5000 ng mL-1 and the regression coefficient was 0.9998 with the linear regression equation y = 4766.8x−17726. The detection (LOD) and quantification (LOQ) limits were 10.3 and 35.6 ng mL-1, respectively. The wide linearity range, sensitivity, accuracy, short retention time, and simple mobile phase imply the method is suitable for routine quantification of mimosine with high precision and accuracy.

3

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

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

Acta Chromatographica

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2008

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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.

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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

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2007

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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.

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Development and validation of a stability-indicating HPLC method for analysis of celecoxib (CXB) in bulk drug and microemulsion formulations

Baboota S., Faiyaz S., Ahuja A., Ali J., Shafiq S., Ahmad S.

Acta Chromatographica

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2007

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No. 18

116-129

EN

A simple, economic, selective, precise, and stability-indicating HPLC method has been developed and validated for analysis of celecoxib (CXB), a selective COX-2 inhibitor, both in bulk drug and in microemulsions. Reversed-phase chromatography was performed on a C18 column with methanol–water, 75:25 (%, v/v), as mobile phase at a flow rate of 1.25 mL min-1. Detection was performed at 250 nm and a sharp peak was obtained for CXB at a retention time of 4.8 ± 0.01 min. Linear regression analysis data for the calibration plot showed there was a good linear relationship between response and concentration in the range 0.27–80 µg mL-1; the regression coefficient was 0.996 and the linear regression equation was y = 48415x + 54359. The detection (LOD) and quantification (LOQ) limits were 0.086 and 0.2625 µg mL-1 respectively. The method was validated for accuracy, precision, reproducibility, specificity, robustness, and detection and quantification limits, in accordance with ICH guidelines. Statistical analysis proved the method was precise, reproducible, selective, specific, and accurate for analysis of CXB. The wide linearity range, sensitivity, accuracy, short retention time, and simple mobile phase imply the method is suitable for routine quantification of CXB with high precision and accuracy.