Utilization of Chemometric-Aided UV Spectrophotometric Methods for Concurrent Assessment of Emtricitabine, Tenofovir Disoproxil Fumarate, Elvitegravir, and Cobicistat in Tablet Formulation.

BACKGROUND: Emtricitabine (ETC), tenofovir disoproxil fumarate (TNF), elvitegravir (EVG), and cobicistat (CBS) are antiviral drugs used to treat human immunodeficiency virus (HIV) infections. OBJECTIVE: To develop chemometric-aided UV spectrophotometric methods for concurrent estimation of the aforementioned drugs used to treat HIV. This method can be used to reduce modification of the calibration model by assessing the absorbance at various points in the zero-order spectra within the selected wavelength range. Additionally, it eliminates interfering signals and provides sufficient resolution in multi-component systems. METHODS: Two chemometric-assisted UV spectrophotometric methods, namely, partial least-squares (PLS) and principal component regression (PCR) models, were established for the concurrent assessment of EVG, CBS, TNF, and ETC in tablet formulations. The proposed methods were applied to decrease complexity of overlapped spectra and to achieve maximum sensitivity and the lowest error. These approaches were performed in accordance with International Council on Harmonization (ICH) criteria and compared to the reported HPLC method. RESULTS: The proposed methods were used to assess EVG, CBS, TNF, and ETC in the ranges of 5-30, 5-30 , 5-50, and 5-50 µg/mL, respectively, with an excellent correlation coefficient (r2 ≥ 0.998). The accuracy and precision results were found to be within the acceptable limits. No statistical difference was observed between the proposed and reported studies. CONCLUSION: The chemometric-aided UV spectrophotometric approaches could be considered as alternatives to chromatographic procedures in the pharmaceutical industry for routine analysis and testing of readily accessible commercial formulations. HIGHLIGHTS: Novel chemometric-assisted UV spectrophotometric techniques were developed for assessment of multicomponent antiviral combinations in single-tablet formulations. The proposed methods were performed without using harmful solvents, tedious preparation, or expensive instruments. The proposed methods were compared statistically with a reported HPLC method. Assessment of EVG, CBS, TNF, and ETC was performed without interference from excipients in their multicomponent formulations.

Box-Behnken design avenue for development and validation of high-performance thin-layer chromatography method for estimation of rutin in Hemidesmus indicus.

The aim of this study was to determine the content of rutin in Hemidesmus indicus and to optimize the high-performance thin-layer chromatography method. The method was validated in compliance with the International Council for Harmonisation guidelines Q2 (R1) for parameters such as linearity, accuracy, precision, robustness, limit of detection, and limit of quantitation. A Box-Behnken design and response surface methodology has been used to investigate the impact of independent variables on the response. Three independent variables, mobile phase composition (% v/v), mobile phase volume (mL), and duration of saturation (min), were studied. Rutin was verified, and its content was determined using a validated high-performance thin-layer chromatography method with good linearity within the range of 200-1000 ng spot-1 with r2 = 0.9998 and correlation coefficient with calibration curve equation y = 0.0297x + 0.0001. The average percentage recovery values varied from 99.03 to 101.15 and 98.88 to 100.12%, respectively, for in-house and marketed mother tincture). The peak area determination at three different concentration levels shows low values of percentage relative standard deviation (<2%) for inter-day (0.04-0.06) and intra-day (0.04-0.05) precision of rutin. The average content of rutin in extract and marketed mother tincture was 229 ± 0.57 and 210 ± 0.57 µg g-1 . The proposed method was simple, precise, and accurate for the determination of rutin with frequent quality control assessment of H. indicus.

Development and validation of multivariate calibration methods for simultaneous estimation of Paracetamol, Enalapril maleate and hydrochlorothiazide in pharmaceutical dosage form.

Three multivariate calibration spectrophotometric methods were developed for simultaneous estimation of Paracetamol (PARA), Enalapril maleate (ENM) and Hydrochlorothiazide (HCTZ) in tablet dosage form; namely multi-linear regression calibration (MLRC), trilinear regression calibration method (TLRC) and classical least square (CLS) method. The selectivity of the proposed methods were studied by analyzing the laboratory prepared ternary mixture and successfully applied in their combined dosage form. The proposed methods were validated as per ICH guidelines and good accuracy; precision and specificity were confirmed within the concentration range of 5-35µgmL-1, 5-40µgmL-1 and 5-40µgmL-1of PARA, HCTZ and ENM, respectively. The results were statistically compared with reported HPLC method. Thus, the proposed methods can be effectively useful for the routine quality control analysis of these drugs in commercial tablet dosage form.