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.

Prazosin hydrochloride is the first developed selective antagonist for 1 – adrenoceptors, which is used as antihypertensive agent. Statins are used in the treatment of various types of hypercholesterolemia. In the present paper a simple, specific an accurate RP-HPLC method was developed and validated for the simultaneous determination of prazosin, atorvastatin, rosuvastatin and simvastatin in active and in dosage formulations. Anucleosil100-10, C-18, 10column having 250 4.6 mmi.d. in isocratic mode, with mobile phase containing methanol:water:acetonitrile (70:20:10) adjusted to pH 2.5 ± 0.02 using orthophosphoric acid. The flow rate was 1 mLmin -1 and effluents were monitored at 240 nm. The % recovery for all thedrugsin formulationswasfound to be94-105%.Theparameterssuch asaccuracy(%RSD lessthan 2), precision (%RSD less than 2), linearity (>0.999) were found to be satisfactory. The presented method was applied without any interference of excepients for the determination of tablets. The proposed method due to its low LOQ, excellent accuracy, precision and selectivity could be used for routine quality control.

Simultaneous Determination of Prazosin, Atorvastatin, Rosuvastatin and Simvastatin in API, Dosage Formulations and Human Serum by RP‐HPLC

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

Simple and reproducible HPTLC method was developed for the separation and quantitation of simvastatin, pravastatin sodium and rosuvastatin calcium, cholesterol lowering agents in pharmaceutical dosage forms. The stationary phase used was precoated silica gel 60F 254 . The mobile phase used was a mixture of chloroform:methanol:toluene (6:2:2, v/v/v). The method has been completely validated and proved to be rugged. Calibration curves were linear over the studied ranges with correlation coefficients grater than 0.999. All the drugs were extracted from the respective tablets using methanol. The percentage recoveries ranged from 100 to 101 for simvastatin, 98 to 101 for pravastatin sodium and 98 to 102 for rosuvastatin calcium. The LOD for simvastatin, pravastatin sodium and rosuvastatin calcium were found to be 15, 9 and 8 ng/spot, respectively and LOQ were 200 ng/spot for simvastatin and 100 ng/spot for pravastatin sodium and rosuvastatin calcium. The method can be useful in the quality control of bulk manufacturing and tablet dosage forms.

/pdf/determination-of-simvastatin-pravastatin-sodium-and-3vs9notcvk.pdf

Determination of simvastatin, pravastatin sodium and rosuvastatin calcium in tablet dosage forms by HPTLC

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

Determination of simvastatin, pravastatin sodium and rosuvastatin calcium in tablet dosage forms by HPTLC