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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

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2009

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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.

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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

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2009

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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.

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Development and validation of a stability-indicating method for determination of ropinirole in the bulk drug and in pharmaceutical dosage forms

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

Acta Chromatographica

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2008

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Vol. 20, no. 1

95-107

EN

An accurate, sensitive, precise, rapid, and isocratic reversed phase HPLC (RP-HPLC) method for analysis of ropinirole in the bulk drug and in pharmaceutical preparations has been developed and validated. The best separation was achieved on a 250 mm × 4.6 mm i.d, 5-µm particle, C18 reversed-phase column with methanol-0.05 M ammonium acetate buffer (pH 7) 80:20 (v/v) as mobile phase, at a flow rate of 1 mL min-1. UV detection was performed at 250 nm. The method was linear over the concentration range 0.2-100 µg mL-1 (r = 0.9998), with limits of detection and quantitation of 0.061 and 0.184 µg mL-1, respectively. The drug was subjected to oxidation, hydrolysis, photolysis, and heat as stress conditions. Degradation products resulting from the stress did not interfere with detection and assay of ropinirole and thus the method can be regarded as stability-indicating. The method can be used for quality-control assay of ropinirole.

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Development and validation of an HPTLC method for determination of minocycline in human plasma

Jain G. K., Jain N., Iqbal Z., Talegaonkar S., Ahmad F. J., Khar R. K.

Acta Chromatographica

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2007

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No. 19

197-205

EN

A new high-performance thin-layer chromatographic (HPTLC) method has been established for determination of minocycline in human plasma. Chromatography was performed on aluminium plates coated with silica gel 60F254; the mobile phase was methanol–acetonitrile–isopropanol–water 5:4:0.5:0.5 (v/v). Densitometric analysis was performed at 345 nm. The method is rapid (single-step extraction with methanol), sensitive (limit of quantification 15.4 ng per zone), precise (CV ≤ 4.61 %), accurate (drug recovery 95.08–100.6%), and linear over the range 100–1200 ng per zone. Recovery of minocycline from plasma samples was 95.8 ± 4.5%. The halflife of minocycline in plasma was 9.9 h at 4°C and 6.3 h at 20°C. Minocycline is stable in human plasma for at least two months at -20°C and can tolerate two freeze–thaw cycles with losses <10%. The method was successfully used to determine therapeutic levels of minocycline.