Analysis of pharmaceutical and natural compounds and newer drugs is commonly used in all the stages of drug discovery and development process. High-performance thin layer chromatography is one of the sophisticated instrumental techniques based on the full capabilities of thin layer chromatography. The advantages of automation, scanning, full optimization, selective detection principle, minimum sample preparation, hyphenation, and so on enable it to be a powerful analytical tool for chromatographic information of complex mixtures of pharmaceuticals, natural products, clinical samples, food stuffs, and so on.

High-performance thin layer chromatography: A powerful analytical technique in pharmaceutical drug discovery.

A simple, isocratic, and sensitive reverse phase high performance liquid chromatographic (RP‐LC) method has been developed, for the first time, for quantitative determination of atorvastatin and ezetimibe in pharmaceutical formulations. Atorvastatin and ezetimibe were chromatographed using 0.01 M ammonium acetate buffer (pH∶3.0): Acetonitrile (50∶50 v/v) as mobile phase. The detection was monitored at 254 nm. The retention times of ezetimibe and atorvastatin were 15.50±0.07 and 19.30±0.06, respectively. The linearity of the method was studied over the concentration range of 4–400 µg/mL for atorvastatin and 5–500 µg/mL for ezetimibe. The limit of detection for atorvastatin and ezetimibe were found as 1.25 µg/mL and 1.48 µg/mL, respectively. The proposed method was applied for the quantitative determination of atorvastatin and ezetimibe in commercial combination formulations.

HPLC Analysis for Simultaneous Determination of Atorvastatin and Ezetimibe in Pharmaceutical Formulations

Microalgae is one of the major sources of natural compounds with antimicrobial activity. The metabolite profiling of the extracts could identify the bioactive compounds based on methanol (MET), ethanol (ETH), chloroform (CHL), hexane (HEX) and water (W) solvent systems. The microalgal crude extracts in co-application with silver nanoparticles (AgNPs) had enhanced antimicrobial activity with potential to overcome the global problem of microbial antibiotic resistance. Chlorella sp. exhibited the highest lipid, N. oculata the highest total saturated fatty acids (TSFA), and T. suecica the highest mono-unsaturated (MUFA) and poly-unsaturated fatty acids (PUFA). The highest carbohydrate, protein and total phenolics contents (TPCs) were attained by N. oculata. The highest total flavonoids contents (TFCs), and chlorophyll a and b were in T. suecica, while comparable level of carotenoids were found in all species. For high-performance thin-layer chromatography (HPTLC) analyses, the eicosapentaenoic acid (EPA) with high peaks were detected in T. suecica-HEX and N. oculata-CHL; and β-carotene in Chlorella sp.-ETH. The gas chromatography–mass spectrometry (GC–MS) analyses showed high 13-docosenamide (Z)- in T. suecica-HEX; phytol in N. oculata-HEX; and neophytadiene in Chlorella sp.-ETH. The AgNPs–MCEs–MET and HEX at the 1.5:1 ratios exhibited strong activities against Bacillus subtilis, Streptococcus uberis, and Salmonella sp.; and the AgNPs–T. suecica-HEX and MET and AgNPs–Chlorella sp.-HEX at the 1.5:1 ratios exhibited activities against Klebsiella pneumoniae. Different bioactive components were detected in the MCEs based on the HPTLC and GC–MS analyses. Significant antimicrobial activities against the pathogenic microbes were demonstrated by the synergistic effects of the MCEs in co-application with the AgNPs. This could be beneficial in the fight against sensitive and multidrug-resistant bacteria.

/pdf/phytochemical-screening-metabolite-profiling-and-enhanced-4uh4gypuph.pdf

Phytochemical screening, metabolite profiling and enhanced antimicrobial activities of microalgal crude extracts in co-application with silver nanoparticle

Spectrophotometric and TLC-densitometric methods for the simultaneous determination of Ezetimibe and Atorvastatin calcium.

Background: Atorvastatin, a lipid-regulating drug, was the best-selling drug in the world in the early 2000s. Thus, monitoring of this drug is important because it is accessible to a large portion of the population. In addition, its quality control is fundamental to provide quality medicines. Method of analysis can be the first step in the rational use of pharmaceuticals. Objective/Methods: In this context, a critical review of analytical methods present in the literature and official compendia for the pharmaceutical quality control of atorvastatin was made. Results: Among the analytical methods most used in the evaluation of atorvastatin, HPLC is highlighted, followed by HPLC coupled to MS, and spectrophotometry in UV. Tablets are the most studied pharmaceutical samples, and plasma is the most studied biological matrix. In the literature, studies with atorvastatin-based pharmaceutical products are more common than biological materials. Acetonitrile is the organic solvent most commonly used in the methods surveyed to evaluate atorvastatin. Conclusions: Currently, awareness of the impact that the analytical choice has on the health of the operator and the environment is growing. Therefore, the suitability of existing methods for the determination of atorvastatin can be made to adhere to the current analytical chemistry. In this way, the analytical, environmental, and human consciousness will remain united. Highlights: Although the literature shows interesting methods from an economic and environmental point of view, such as UV, Vis miniaturized, and TLC, they can still be improved to meet the requirements of the current sustainable analytical chemistry.

Atorvastatin: A Review of Analytical Methods for Pharmaceutical Quality Control and Monitoring.

A simple, precise, accurate and rapid high-performance thin-layer chromatographic method has been developed and validated for the estimation of atorvastatin calcium and ezetimibe simultaneously in combined dosage forms. The stationary phase used was precoated silica gel 60F254. The mobile phase used was a mixture of chloroform: benzene: methanol: acetic acid (6.0:3.0:1.0:0.1 v/v/v/v). The detection of spots was carried out at 250 nm. The method was validated in terms of linearity, accuracy, precision and specificity. The calibration curve was found to be linear between 0.8 and 4.0 µg/spot for atorvastatin calcium and 0.1 and 1.0 µg/spot for ezetimibe. The limit of detection and the limit of quantification for atorvastatin calcium were found to be 170 ng/spot and 570 ng/spot respectively, and for ezetimibe, 20 ng/spot and 70 ng/spot respectively. The proposed method can be successfully used to determine the drug content of marketed formulation.

https://www.ijpsonline.com/articles/development-and-validation-of-a-hptlc-method-for-the-simultaneous-estimation-of-atorvastatin-calcium-and-ezetimibe.pdf

Development and validation of a HPTLC method for the simultaneous estimation of atorvastatin calcium and ezetimibe

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Development and validation of a HPTLC method for the simultaneous estimation of atorvastatin calcium and ezetimibe