Nitin Dubey

Stability-indicating HPTLC method for simultaneous estimation of famotidine, paracetamol, and ibuprofen in combined tablet dosage forms

A stability-indicating high-performance thin-layer chromatographic (HPTLC) method has been developed for the determination of simultaneous determination of famotidine (FAMO), paracetamol (PCM), and ibuprofen (IBU) in tablet dosage forms. The separation was achieved on TLC aluminum plates precoated with silica gel 60F-254 using chloroform-methanol-ethyl acetate-acetic acid (21.5:16.1:59.1:3.2%, v/v/v/v) as the mobile phase. The densitometric analysis was carried out at 256 nm. Compact spots appeared at RF 0.21 ± 0.01, 0.80 ± 0.02, and 0.89 ± 0.01 for FAMO, PCM, and IBU, respectively. Linear regression analysis revealed linearity in the range of 160–960 ng per spot for FAMO, 400–2400 ng per spot for PCM, and 600–3600 ng per spot for IBU. Drugs were subjected to acid and alkali hydrolyses, forced oxidation, thermal and photodegradation treatments. The degraded products were well separated from the pure drugs. Statistical analysis proved that the method is precise, accurate, selective, and economical and may be used for routine analysis of FAMO, PCM, and IBU in tablet dosage forms.

Cleaning level acceptance criteria and HPLC-DAD method validation for the determination of Nabumetone residues on manufacturing equipment using swab sampling

Prevention of cross contamination with active pharmaceutical ingredients is crucial and requires special attention in pharmaceutical industries. Current method validation describes the determination of Nabumetone (NAB) residue on a stainless steel surface using swab sampling with a sensitive HPLC-DAD analysis. The acceptance limit was decided as 2 μg swab per 100 cm2. Cotton swabs impregnated with extraction solution were used to determine residual drug content. Recoveries were 90.88%, 91.42%, and 92. 21% with RSD ranging from 2.2% to 3.88% at three concentration levels. Residual concentration was found to be linear in the range of 0.1–4.56 μg/mL, when estimated using a Phenomenex Luna C18 (25 cm×5 μm×4.6 mm i.d.) column at 1.0 mL/min flow rate and 230 nm. The mobile phase consisted of a mixture of methanol:acetonitrile:water (55:30:15, v/v/v). The LOD and LOQ for NAB were found to be 0.05 and 0.16 μg/mL, respectively. The validated method was found to be simple, selective and sensitive for demonstration of cleaning validation of NAB residues on a stainless steel surface.

Stability-Indicating HPTLC Method for Simultaneous Estimation of Amlodipine Besylate, Hydrochlorothiazide and Olmesartan Medoxomil in Combined Tablet Dosage Forms

Amlodipine besylate, or 3-ethyl-5-methyl-(4RS)-2-[(2-amino-ethoxy)methyl]-4-(2-chlorophenyl)-6-methyl-1,4-dihydropyri-dine-3,5-dicarboxylate benzene sulphonate is a cardiovascular(antianginal), dihydropyridine calcium channel blocker widelyused in antihypertensive pharmaceutical formulations [1–2].Hydrochlorothiazide, or 6-chloro-3,4-dihydro-2H-1,2,4-benzo-thiadiazine-7-sulfonamide-1,1-dioxide, is a diuretic of the class of benzothiadiazines widely used in antihypertensive phar-maceutical formulations, alone or in combination with otherdrugs, which decreases active sodium reabsorption and reducesperipheral vascular resistance [3]. Olmesartan, the medoxomilsalt of (5-methyl-2-oxo-1,3-dioxol-4-yl)methyl ester of 4-(1-hydroxy-1-methylethyl)-2-propyl-1-{[2’-(1H-tetrazol-5-yl)[1,1’-biphenyl]-4-yl]methyl}-1H-imidazole-5-carboxylic acid,is the ester prodrug of a new generation of effective and orallyactive angiotensin-II receptor antagonist. It blocks the vasocon-strictor and aldosterone-secreting effects of angiotensin-II, oneof the most important regulators of blood pressure [4]. Thedetermination of OLME from tablet formulation has been car-ried out by high-performance liquid chromatography (HPLC),high-performance thin-layer chromatography (HPTLC) andspectrophotometricaly, alone or in combination [5–7]. Assay ofAMLO and HCTZ in bulk and in dosage form is official in Indi-an Pharmacopoeia and British Pharmacopoeia in differentdosage forms. Several analytical methods have been reportedfor their determination alone or in combination with other drugsin different dosage forms, biological fluids and urine using dif-ferent analytical techniques [8–13]. Forced degradation studiesare used to facilitate the development of analytical methodolo-gy, to gain better understanding of the stability of the activepharmaceutical ingredient (API), drug product, and to provideinformation about degradation pathways and degradation prod-ucts. The objective of this work was to develop a stability-indi-cating HPTLC method for simultaneous analysis of AMLO,HCTZ, and OLME as no reported method is available for theirsimultaneous estimation in combined formulations. Chemicalstructure of the drugs is shown in Figure 1.HPTLC has advantages over other methods because of rapidity,selectivity, economy, and overall versatility in QC aspects ofdrugs. Literature survey revealed that various HPTLC methodshave been reported for determination of AMLO, HCTZ, andOLME individually and in combination with other drugs [3,5–15]. Currently, the HPLC method is the most frequently usedanalytical method for this kind of determinations. However, nosimultaneous estimation of these drugs was reported so far;hence, it was found worthwhile to develop an HPTLC methodfor the simultaneous determination of AMLO, HCTZ, andOLME in the presence of degradation products and relatedimpurities in pharmaceutical formulations.

Development and Validation of Selective High-Performance Liquid Chromatographic Method Using Photodiode Array Detection for Estimation of Aconitine in Polyherbal Ayurvedic Taila Preparations

A simple, sensitive, and selective high-performance liquid chromatographic (HPLC) method has been developed and validated for the analysis of aconitine in marketed ayurvedic taila (oil) formulations containing roots of Aconitum chasmanthum. Chromatography of methanolic extracts of these formulations was performed on C18 (5 μm × 25 cm × 4.6 mm i.d.) column using isocratic mobile phase consisting of (65 : 35% v/v) acetonitrile and buffer solution (aqueous 0.01 M ammonium bicarbonate buffer, adjusted to pH 9.6 using 30% ammonia solution) at a flow rate of 1 mL/min and SPD-10 photodiode array (PDA) UV-Visible detector. The analytical reference, aconitine, was quantified at 238 nm. The retention time of aconitine was about 42.54 min. The linear regression analysis data for the calibration plot showed a good linear relationship with correlation coefficient of 0.9989 in the concentration range of 15 to 90 μg/mL for aconitine with respect to peak area. The limit of detection and limit of quantitation values were found to be 0.03 μg/mL and 0.1 μg/mL respectively. Repeatability of the method was found to be 0.551–1.689 RSD. Recovery values from 97.75 to 99.91% indicate excellent accuracy of the method. The developed HPLC method is accurate and precise and it can be successfully applied for the determination of aconitine in marketed ayurvedic oil formulations containing Aconitum chasmanthum.