In this research paper we describe validated high-performance liquid chromatographic (HPLC) and high-performance thin-layer chromatographic (HPTLC) methods for simultaneous analysis of tamsulosin hydrochloride and dutasteride in tablet formulations. HPLC was performed on a C18 column with 85:15 (υ/υ) methanol-0.02 m ammonium acetate buffer (pH 9.5, adjusted with triethylamine) as mobile phase. HPTLC was performed on aluminium foil-backed silica gel G60F254 layers with toluene-methanol-triethylamine 9:1.5:1 (υ/υ/υ) as mobile phase. In HPLC, quantification was achieved by photo diode-array (PDA) detection at 274 nm over the concentration range 1–20 μg mL−1 for both; mean recovery was 98.18 ± 0.698 and 99.94 ± 0.611% for TAM and DUTA, respectively. In HPTLC, quantification was achieved by UV detection at 280 nm over the concentration range 200–2000 ng per band for both; mean recovery was 99.66 ± 0.892 and 100.05 ± 1.012% for TAM and DUTA, respectively. These methods are simple, precise, and sensitive, and are suitable for simultaneous analysis of TAM and DUTA in tablet formulations.
Authors:D. S. Patel, N. Sharma, M. C. Patel, B. N. Patel, P. S. Shrivastav, and M. Sanyal
A rapid, selective, and sensitive liquid chromatography-tandem mass spectrometry (LC-MS/MS) assay has been proposed for the determination of aripiprazole in human plasma. The analyte and propranolol as internal standard (IS) were extracted from 200 μL of human plasma via liquid-liquid extraction using methyl tert-butyl ether under alkaline conditions. The best chromatographic separation was achieved on an Aquasil C18 (100 × 2.1 mm, 5 μm) column using methanol-deionized water containing 2 mM ammonium trifluoroacetate and 0.02% formic acid (65:35, v/v) as the mobile phase under isocratic conditions. Detection of analyte and IS was done by tandem mass spectrometry, operating in positive ion and multiple reaction monitoring (MRM) acquisition mode. The method was fully validated for its selectivity, interference check, sensitivity, carryover check, linearity, precision and accuracy, reinjection reproducibility, recovery, matrix effect, ion suppression/enhancement, stability, ruggedness, and dilution integrity. The assay was linear over the concentration range of 0.10–100 ng mL−1 for aripiprazole. The intra-batch and inter-batch precision (%CV) was ≤4.8%, while the mean extraction recovery was >96% for aripiprazole across quality control levels. The method was successfully applied to a bioequivalence study of 10 mg aripiprazole orally disintegrating tablet formulation in 27 healthy Indian subjects under fasting and fed condition. The reproducibility in the measurement of study data was demonstrated by reanalysis of 260 incurred samples.
Authors:S. Gandhi Gandhi, N. Barhate Barhate, B. Patel Patel, D. Panchal Panchal, and K. Bothara Bothara
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 ± 0.019 and 0.74 ± 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 ± 0.282 for aceclofenac and 0.354 ± 0.212 for paracetamol. Interday variation, as RSD (%) ± SE, was 0.57 ± 0.41 for aceclofenac and 0.90 ± 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 cost-effective quality-control tool for routine simultaneous analysis of aceclofenac and paracetamol in combined dosage forms.
Authors:D. Gadhiya, N.P. Shah, A.R. Patel, and J.B. Prajapati
Current study was taken up to develop probiotic chocolate using indigenous probiotic culture L. helveticus MTCC 5463. Preliminary trials included optimization of culture inoculums and physical form (freeze-dried or frozen concentrated) of addition and finally optimized product was tested for probiotic viability, texture, and organoleptic parameters at regular intervals during storage at 10±2 °C for 30 days. Probiotic chocolates prepared via incorporation of freeze dried culture (3% w/w) had acceptable organoleptic quality and had a similar behaviour as the control chocolate during storage. However, the viability of probiotic bacteria (2.42×108 CFU g–1) was achieved only up to 15 days of storage at 10±2 °C.