Current Issue : January - March Volume : 2021 Issue Number : 1 Articles : 6 Articles
Due to the lack of ecofriendly/green reversed-phase high-performance thin-layer chromatography (RP-HPTLC) methods for trans-anethole (TAL) and its simplicity over routine analytical techniques, there was a necessity to establish a suitable HPTLC methodology for the quantitative analysis of TAL. Therefore, the first objective of this research was to develop an accurate, rapid and green RP-HPTLC densitometry methodology for the quantitative analysis of TAL in essential oil, traditional and ultrasound-assisted extracts of Foeniculum vulgare Mill and commercial formulations. The second objective was to compare the traditional method of extraction of TAL with its ultrasound-assisted method of extraction. The chromatogram of TAL from essential oil and traditional and ultrasound-assisted extracts of fennel and commercial formulations was verified by recoding its single spectra at Rf = 0.31 ± 0.01 in comparison to standard TAL. The proposed analytical methodology has been found to be superior in terms of linearity, accuracy and precision compared to most of the reported analytical methods for TAL analysis. The amount of TAL in the essential oil of fennel was recorded as 8.82 mg per g of oil. The content of TAL in traditional extracts of fennel, formulation 1 (dietary supplement 1) and formulation 2 (dietary supplement 2), was recorded as 6.44, 4.88 and 4.48 mg per g, respectively. The amount of TAL in ultrasound-assisted extracts of fennel, formulation 1 and formulation 2, was recorded as 8.34, 6.46 and 5.81 mg per g, respectively. The ultrasound method of extraction of TAL was found to be better than the traditional method of extraction. The results of validation studies and phytochemical analysis showed that the proposed methodology could be efficiently utilized for the quantification of TAL in the wide range of products having TAL as a component....
Nanotechnology has enabled the development of novel therapeutic strategies such as targeted nanodrug delivery systems, control and stimulus-responsive release mechanisms, and the production of theranostic agents. As a prerequisite for the use of nanoparticles as drug delivery systems, the amount of loaded drug must be precisely quantified, a task for which two approaches are currently used. However, both approaches suffer from the inefficiencies of drug extraction and of the solid-liquid separation process, as well as from dilution errors. This work describes a new, reliable, and simple method for direct drug quantification in polymeric nanoparticles using attenuated total reflection Fourier transform infrared spectroscopy, which can be adapted for a wide variety of drug delivery systems. Silk fibroin nanoparticles and naringenin were used as model polymeric nanoparticle carrier and drug, respectively. The specificity, linearity, detection limit, precision, and accuracy of the spectroscopic approach were determined in order to validate the method. A good linear relation was observed within 0.00 to 7.89% of naringenin relative mass with an R2 of 0.973. The accuracy was determined by the spike and recovery method. The results showed an average 104% recovery. The limit of detection and limit of quantification of the drug loading content were determined to be 0.3 and 1.0%, respectively. The method’s robustness is demonstrated by the notable similarities between the calibrations carried out using two different equipment setups at two different institutions....
The cytotoxic effects of the crude extract of Loranthus acaciae Zucc. and its n-hexane, chloroform, and n-butanol fractions were assessed against three cancer cell lines using the 3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyl tetrazolium bromide assay. Cell apoptosis was determined using an annexin V-phycoerythrin/7-aminoactinomycin kit. We observed that the L. acaciae n-hexane extract (LAHE) could inhibit cancer cell growth, particularly ofMCF7and A549 cells. Chromatographic purification of LAHE and nuclear magnetic resonance analysis led to the identification of two compounds from this plant species, namely, betulinic acid and β-sitosterol, for the first time. Flow cytometry study suggested that betulinic acid induced cell death via apoptosis, as a distinguished marked enhancement in the early and late apoptosis of human lung (A549) and breast (MCF-7) cancer cell lines. The isolated compounds were further estimated concurrently in LAHE using a validated high-performance thin-layer chromatographic (HPTLC) method on a 10 × 10 cm2 HPTLC plate with chloroform, methanol, and glacial acetic acid (97:2:1, v/v/v) as the mobile phase and a λmax of 540 nm. The amounts of betulinic acid and β-sitosterol in LAHE were 69.46 and 135.53 μg/mg of dried weight of extract, respectively. The excellent cytotoxic effect of LAHE could be attributed to the presence of ample amounts of betulinic acid....
Ezetimibe is the drug of choice from the novel class of anti-hyperlipidemic drugs. An analytical literature survey for the determination of ezetimibe revealed few articles based on different techniques. However, there is a need of a suitable analytical technique that will be simple and reproducible. A reversed-phase HPLC method was developed to quantify the ezetimibe in the presence of degradation products and pharmaceutical excipients. A stress study was performed on ezetimibe. The separation was carried out on Waters Spherisorb CNRP column using acetonitrile: water (40:60 v: v) as a mobile phase with a flow rate of 1 ml/min. The wavelength of the detection was set at 232 nm. The calibration curve for ezetimibe was found linear (R2=0.999) in the concentration range 5-30 microgram/ml. The relative standard deviation for all the key parameters (selectivity, specificity, linearity, accuracy and precision) was found to be less than 2%. The recovery of the drug after standard addition was found in the range of 95.15-96.30 %. Stress study showed complete degradation in alkaline conditions, whereas less degradation was observed in acidic, thermal, oxidizing and photolytic conditions. The developed RP-HPLC method would be suitable for the identification and quantification of ezetimibe in various pharmaceutical dosage forms....
A selective, accurate, and precise stability-indicating HPLC method for analysis of levamisole hydrochloride in bulk and in their injection and oral solution formulations has been developed and validated in accordance with ICH guidelines. The chromatographic separation was carried out on a C8 column (250 × 4.6mm with a particle size of 5 micrometer) using a mixture of phosphate buffer pH 8.0 and acetonitrile (70 : 30 v/v) as the mobile phase pumped at a flow rate of 1.5 ml/min with UV detection at 215 nm. The calibration curve was linear over the 10–50 μg/ml concentration range with a correlation coefficient of 1.0000. The limit of detection (LOD) and the limit of quantitation (LOQ) were 0.29 μg/ml and 0.89 μg/ml, respectively. The accuracy and the precision of the developed method were significantly good (RSD < 2%). The validity of the proposed method was further confirmed through the statistical comparison of the obtained data with those of the official method....
A simple, rapid, sensitive, and precise reversed-phase liquid chromatographic method was developed and validated for the simultaneous determination of four direct-acting antivirals, sofosbuvir (SF), ledipasvir (LD), declatasvir (DC), and simeprevir (SM), in their respective pharmaceutical formulations. Effective chromatographic separation was achieved on an Agilent Eclipse plus C8 column (250 mm × 4.6 mm, 5 μm) at 40 ◦C with gradient elution using a mobile phase composed of acetonitrile:phosphate buffer (pH 6.5). The quantification of SF and DC was based on peak area measurements at 260 nm, while the quantification of LD and SM was achieved at 330 nm. The linearity was acceptable from 1.0 to 20.0 μg/mL for the studied drugs, with correlation coefficients >0.999. The analytical performance of the newly proposed HPLC procedure was thoroughly validated according to ICH guidelines in terms of linearity, precision (RSD%, 0.39–1.57), accuracy (98.05–101.90%), specificity, limit of detection (LOD) (0.022–0.039 μg/mL), limit of quantification (LOQ) (0.067–0.118 μg/mL), and robustness. The validated HPLC method was successfully used to analyze the abovementioned drugs in their pure and dosage forms without interference from common excipients present in commercial formulations....
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