Bhanubhai N. Suhagia

Preparation and characterization of etoricoxib-β-cyclodextrin complexes prepared by the kneading method

Preparation and characterization of etoricoxib-β-cyclodextrin complexes prepared by the kneading method The binary system of etoricoxib with β-cyklodextrin (β-CD) was prepared by the kneading method. Drug-cyclodextrin interactions in solution were investigated by the phase solubility analysis. Differential scanning calorimetry, infrared spectroscopy, powder X-ray diffractometry and microscopic study were used to characterize the solid state of all binary systems, whereas their dissolution properties were evaluated according to the USP XXIII paddle method. The results indicate partial interaction of the drug with β-CD in the physical mixture and complete interaction in the kneaded complex. The dissolution of etoricoxib was notably increased as compared to pure drug as well as its physical mixture. The complex showed more than 75% drug released in 30 min. Priprava kompleksa etorikoksiba s β-ciklodekstrinom metodom gnječenja i njihova karakterizacija Metodom gnječenja pripravljen je binarni sustav etorikoksiba s β-ciklodekstrinom (β-CD). Tijekom 30 minuta iz kompleksa se oslobodilo više od 75% ljekovite tvari, što je značajno više u odnosu na fizičku smjesu etorikoksiba i β-CD ili čistu ljekovitu tvar. Interakcije lijeka i ciklodekstrina u otopini ispitivane su analizom fazne topljivosti. Za karakterizaciju čvrstog stanja svih binarnih sustava korištena je diferencijalna pretražna kalorimetrija, infracrvena spektroskopija, difrakcija rentgenskih zraka na praškastom uzorku i mikroskopija. Oslobađanje je praćeno metodom lopatice prema USP XXIII. Rezultati ukazuju na djelomičnu interakciju ljekovite tvari s β-CD u fizičkoj smjesi te potpunu interakciju u kompleksu.

HPLC Analysis for Simultaneous Determination of Rabeprazole and Domperidone in Pharmaceutical Formulation

Abstract A simple and sensitive reversed phase high performance liquid chromatographic (RP‐HPLC) method has been developed for the quantitative estimation of rabeprazole and domperidone in their combined dosage forms. Rabeprazole and domperidone were chromatographed using 0.01 M, pH 6.5 ammonium acetate buffer:methanol:acetonitrile (40:30:30 v/v, pH 7.44) as the mobile phase at a flow rate of 1.0 mL min−1 at ambient temperature and detected at 287 nm. The retention time (RT) of rabeprazole and domperidone were found to be 6.13±0.01 and 8.38±0.02, respectively. The linearities of rabeprazole and domperidone were in the range of 200–2000 ng/mL and 300–3000 ng/mL, respectively. The limit of detection was found to be 65.67 ng/mL for rabeprazole and 98.33 ng/mL for domperidone. The proposed method was applied for the determination of rabeprazole and domperidone in combined dosage forms.

A simple and sensitive HPTLC method for quantitative analysis of darunavir ethanolate tablets

A quantitative high-performance thin-layer chromatography (HPTLC) method for determination of darunavir ethanolate (DRV) in tablets has been established and validated. DRV from the formulations was separated and identified on silica gel 60 F254 HPTLC plates with toluene-ethyl acetate-methanol 7.0:2.0:1.0 (v/v) as mobile phase. The plates were developed to a distance of 8 cm. Quantification was performed at λ = 267 nm. Well-resolved bands were obtained for DRV. The method was validated for specificity, precision, robustness, and accuracy. The calibration plot for DRV standard was linear in the range 250–1750 ng per band with r = 0.9994, slope = 0.4253, and intercept = 44.81. The limits of detection and quantification were 15.28 and 45.84 ng per band, respectively. The method is selective, sensitive, and specific, with potential application in pharmaceutical analysis.

Simultaneous Determination of Omeprazole and Domperidone in Capsules by RP‐HPLC and Densitometric HPTLC

Abstract A rapid, simple, and sensitive HPLC and a densitometric HPTLC method for the determination of omeprazole and domperidone in capsule formulations were developed and validated. For HPLC, the separation of components was achieved on a Phenomenex Rp‐C18 column. Isocratic elution with a mobile phase consisting of 0.01 M pH 6.5, ammonium acetate buffer: methanol:acetonitrile (40:30:30 v/v, pH 7.44±0.02), at a flow rate 1.0 mL/min was employed. Rabeprazole was used as the internal standard. In densitometric HPTLC, separation was achieved on aluminum sheets of silica gel 60F254 using ethyl acetate:methanol:benzene (40:20:40 v/v) as mobile phase. Linear concentration range of HPLC and HPTLC methods were between 400–2000 ng/mL and 120–360 ng/spot for both the drugs, respectively. In HPLC, the detection limit was 131.27 ng/mL for omeprazole and 131.20 ng/mL for domperidone, the mean analytical recovery in determination of omeprazole and domperidone capsules was 99.14±1.81 for omeprazole and 99.63±1.68 for domperidone. Whereas, the detection limit was 40.83 ng/spot for omeprazole and 40.53 ng/spot for domperidone, the mean analytical recovery in determination of omeprazole and domperidone capsules was 99.51±0.91 and 99.48±1.15, respectively, in HPTLC. The components were detected by UV detection at 295 nm. Thus, the proposed method is applicable for routine determination of omeprazole and domperidone in pharmaceutical formulations.

Simultaneous HPTLC Analysis of Atorvastatin Calcium, Ramipril, and Aspirin in a Capsule Dosage Form

A simple, sensitive, accurate, and precise high-performance thinlayer chromatographic method has been established for simultaneous analysis of atorvastatin calcium, ramipril, and aspirin in a capsule dosage form. The compounds were separated on silica gel with methanol-benzene-ethyl acetate-glacial acetic acid 0.36:5.6:4.0: 0.04 (v/v) as mobile phase. Ultra-violet detection was performed at 210 nm. The RF values were approximately 0.38, 0.06, and 0.86 for atorvastatin calcium, ramipril, and aspirin, respectively. The method was validated for linearity, accuracy, precision, limits of detection and quantification, and robustness. The linearity ranges were 100–600 ng per band for atorvastatin calcium, 50–300 ng per band for ramipril, and 500–3000 ng per band for aspirin. Mean recoveries were 99.97 ± 0.07%, 100.01 ± 0.10%, and 100.02 ± 0.06 % for atorvastatin calcium, ramipril, and aspirin, respectively. Limits of detection (LOD) were 4.88 ng for atorvastatin calcium, 2.91 ng for ramipril, and 18.63 ng for aspirin. Salicylic acid (RF ~ 0.72) was found as an impurity in the capsule dosage form. The proposed method can be used for analysis of these drugs in combined dosage forms.

Estimation of Individual Sennosides in Plant Materials and Marketed Formulations by an HPTLC Method

Senna is a well‐known drug, used in the Ayurvedic and Allopathic systems of medicine, and is a treatment for constipation. The purgative action of senna and its formulations is due to the presence of sennosides A and B. An HPTLC method has been developed for the determination of individual sennosides (A, B, C, D) without any derivatization in marketed formulations (three tablet formulations, two granule formulations and one liquid formulation) and plant materials (senna leaf and pod).

Analysis of betalains from fruits of Opuntia species

Betalains are of great taxonomic significance in higher plants and occur only in 10 families of the order Caryophyllales (Centrospermae). They are water-soluble nitrogenous pigments. They can be divided into two major structural groups, the red to red-violet betacyanins and the yellow betaxanthins. Betalains are widely used as natural red food colorant as well as antioxidant potentials. Several methods have been published for the determination of betalain in fruits of Opuntia species. The purpose of the current review is to provide a systematic survey of the analytical techniques for the determination of betalain from fruits of Opuntia species.

A simple and sensitive HPTLC method for quantitative analysis of pitavastatin calcium in tablets

A quantitative high-performance thin-layer chromatographic method for determination of pitavastatin calcium in pharmaceutical preparations has been established and validated. Pitavastatin calcium from the formulations was separated and identified on silica gel 60F254 HPTLC plates with toluene-methanol-glacial acetic acid 7.6:2.36:0.04 (v/v) as mobile phase. The plates were developed to a distance of 8 cm and well resolved bands were obtained for pitavastatin calcium. Quantification was performed at 238 nm. The method was validated for specificity, precision, robustness, and accuracy. The calibration plot for pitavastatin calcium standard was linear in the range 40-250 ng per band with r = 0.9992, slope = 8.2415, and intercept = 203.2359. The limits of detection and quantification were 6.6 and 20.0 ng per band, respectively. The method is selective, sensitive, and specific with potential application in pharmaceutical analysis.

Development and Validation of a Stability‐Indicating HPTLC‐Densitometric Method for Satranidazole

Abstract A sensitive, selective, precise, and stability‐indicating high performance thin layer chromatography (HPTLC) method for analysis of satranidazole both as a bulk drug and in formulations was developed and validated. The method employed TLC aluminium plates precoated with silica gel 60F‐254 as the stationary phase. The solvent system consisted of toluene/acetonitrile (60:40, v/v). Densitometric analysis of satranidazole was carried out in the absorbance mode at 314 nm. This system was found to give compact spots for satranidazole (R f value of 0.53±0.02, for six replicates). Satranidazole was subjected to acid and alkaline hydrolysis, oxidation, and photo degradation. The drug undergoes degradation under acidic and basic conditions, oxidation, and photo degradation. Also, the degraded products were well resolved from the pure drug with significantly different R f values. The method was validated for linearity, precision, limit of detection (LOD), limit of quantitation (LOQ), and accuracy. Linearity was found to be in the range of 100–500 ng/spot with a significantly high value of correlation coefficient r 2=0.9979±0.66. The LOD and LOQ were 50 and 85 ng/spot, respectively. Statistical analysis proved that the method is repeatable and specific for the estimation of the said drug. As the method could effectively separate the drug from its degradation products, it can be employed as a stability‐indicating one. Moreover, the proposed HPTLC method was utilized to investigate the kinetics of the alkali degradation process.

Formulation of Fenofibrate Liquisolid Tablets Using Central Composite Design

Liquisolid technique has been widely used to enhance the dissolution of poorly water soluble drugs. The present investigation is on formulation of liquisolid tablets of fenofibrate, a lipid lowering agent. Liquisolid formulation was prepared by applying central composite design (CCD) to optimize various formulation parameters. Amounts of PEG 600 (X1), Avicel PH 102 (X2), and Aerosil 200 (X3) were selected as independent variables while the angle of repose, hardness, disintegration time, and T90% (time required to release 90% drug) of liquisolid tablets were selected as dependent variables. Optimization of formulation was done by multiple linear regression analysis. The results indicated amounts of PEG 600 and Aviel PH 102 show greater effect on dependant variables. In vitro dissolution of fenofibrate in liquisolid formulations was enhanced compared to the pure form. To conclude, Liquisolid technique is a promising strategy in improving dissolution of poorly water soluble fenofibrate.