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Validated stability-indicating HPTLC method for cefixime and azithromycin with preparative isolation, identification, and characterization of degradation products

Gawande V. T., Bothara K. G., Satija C. O.

Acta Chromatographica

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2018

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Vol. 30, no. 4

212--218

EN

Stability-indicating High-Performance Thin-Layer Chromatography (HPTLC) method for simultaneous estimation of cefixime trihydrate and azithromycin dihydrate was developed. Both the drugs were subjected to different stress conditions recommended by International Conference on Harmonization (ICH) guideline Q1A (R2). Forced degradation was carried out for hydrolytic, oxidative, photolytic, and thermal degradation conditions. Cefixime was susceptible for degradation under all stress conditions showing four degradation products (CI–IV). However, azithromycin formed only one degradation product (AI) under acid hydrolysis. Aluminum plates precoated with silica gel 60F254 were used as the stationary phase while mixture of ethyl acetate–methanol–acetone–toluene–ammonia (1:5:7:0.5:0.5, v/v) was used as mobile phase. Detection wavelength used was 235 nm for CEFI and CI–IV. AZI and AI were detected by post development derivatization, spraying with sulfuric acid–ethanol (1:4, v/v) followed by heating at 100 °C for 5 min. Degradation products were isolated by preparative HPTLC and characterized by MS/MS. The developed method was validated for linearity, precision, accuracy, specificity, and robustness and has been successfully applied in the analysis of these drugs in tablet dosage form.

2

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

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2010

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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.

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

A validated densitometric method for analysis of aceclofenac and paracetamol as the bulk drugs and in combined tablet dosage forms

Gandhi S. V., Barhate N. S., Patel B. R., Panchal D. D., Bothara K. G.

Acta Chromatographica

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2008

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Vol. 20, no. 2

175-182

EN

A simple, specific, accurate, and precise high-performance thin-layer chromatographic method for analysis of aceclofenac and paracetamol in combined tablet dosage forms is reported in this paper. The method uses aluminium plates coated with silica gel 60 F254 as stationary phase and ethyl acetate-n-butanol-glacial acetic acid 7.5:2.5:0.005 (v/v) as mobile phase. Densitometric evaluation of the separated bands was performed at 270 nm. The two drugs were satisfactorily resolved with RF values 0.29 š 0.019 and 0.74 š 0.025 for aceclofenac and paracetamol, respectively. The respective calibration plots were linear over the ranges 50-1000 and 200-1500 ng per band. Intra-day variation, as RSD (%), was 0.420 š 0.282 for aceclofenac and 0.354 š 0.212 for paracetamol. Interday variation, as RSD (%) š SE, was 0.57 š 0.41 for aceclofenac and 0.90 š 1.09 for paracetamol. The method, which was validated in accordance with ICH guidelines, can be used for analysis of ten or more formulations on a single plate and is a rapid and costeffective quality-control tool for routine simultaneous analysis of aceclofenac and paracetamol in combined dosage forms.