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1

Simultaneous estimation of anti-cancer terpenoids in pharmaceutical nanoformulation by RP-HPLC and HPTLC

Parveen R., Ahmad F. J., Iqbal Z., Singh M., Kamal Y., Ahmad S.

Acta Chromatographica

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2014

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Vol. 26, no. 2

391--400

EN

Andrographolide and betulinic acid are the terpenoids having potential anti-cancer activity. The cytotoxicity activity of both the drugs was carried out separately and in combination on liver cancer HepG2 cell lines. High-performance liquid chromatography (HPLC) and high-performance thin-layer chromatography (HPTLC) methods were developed and validated for simultaneous estimation of these two terpenoids as per the International Conference on Harmonization (ICH) guidelines, which was applied for quantification in nanoformulation. The retention time by HPLC and retardation factor by HPTLC for andrographolide and betulinic acid were found to be 2.2 and 6.6 min, and 0.24 ± 0.01 and 0.66 ± 0.01, respectively. Both the methods were validated for accuracy, precision, repeatability, robustness, limit of detection (LOD), and limit of quantitation (LOQ). The content of andrographolide and betulinic acid in nanoformulation was found to be 96.0% and 98.0% by HPLC and 96.59% and 98.33% by HPTLC, respectively, of labelled claim.

2

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.

3

A validated densitometric TLC method for analysis of cefuroxime axetil and potassium clavulanate in combined tablet dosage forms

Sengar M. R, Gandhi S. V., Patil U. P., Rajmane V. S, Bothara K. G.

Acta Chromatographica

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2010

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Vol. 22, no. 1

91--97

EN

A simple, specific, accurate, and precise high-performance thin-layer chromatographic method for analysis of cefuroxime axetil and potassium clavulanate in a combined tablet dosage form is reported. The compounds were separated on aluminium foil plates precoated with silica gel 60 F 254 , with chloroform-methanol-toluene 4:3:3 ( v / v ) as mobile phase. Densitometric evaluation of the separated bands was performed at 225 nm. The two drugs were satisfactorily separated with R F 0.77 ± 0.0114 and 0.29 ± 0.0114 for cefuroxime axetil and potassium clavulanate, respectively. Response was a linear function of amount over the calibration ranges 500–2500 and 2000–10 000 ng per band, respectively. The method was successfully validated and used for analysis of the drugs in a pharmaceutical formulation. Recovery was 100.05 ± 0.98% for cefuroxime axetil and 99.94 ± 0.538% for potassium clavulanate (mean ± RSD).

4

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.

5

Development and validation of an HPTLC method for analysis of zerumbone, the anticancer marker from Zingiber zerumbet

Rout K. K, Mishra S. K, Sherma J

Acta Chromatographica

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2009

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Vol. 21, no. 3

443--452

EN

A simple, accurate, and rapid high-performance thin-layer chromatographic (HPTLC) method for quantification of the anticancer marker zerumbone in different parts of Zingiber zerumbet Smith has been established and validated. Chromatography was performed on aluminium foil-backed silica gel 60 F 254 HPTLC plates with the binary mobile phase ethyl acetate-hexane 1.5:8.5. Ultraviolet detection was performed densitometrically at the maximum absorbance wavelength, 250 nm. Regression analysis data for the calibration plot showed there was a linear relationship between response and concentration in the range 60–260 ng with a regression coefficient of 0.9997. The limits of detection and quantification were 20 and 60 ng, respectively. The instrumental precision and repeatability of the method were found to be 0.80 and 1.08%, respectively. Recovery ranging from 97.85 to 100.12% indicated the excellent accuracy of the method. The developed HPTLC method was successfully used for analysis of the marker in different parts of Z. zerumbet , and the maximum zerumbone content (1.81%) was found in the rhizome.