scholarly journals Development and Validation of an HPLC Method to Quantify Camptothecin in Polymeric Nanocapsule Suspensions

2008 ◽  
Vol 91 (3) ◽  
pp. 551-556 ◽  
Author(s):  
Andra Granada ◽  
Fabio S Murakami ◽  
Tatiane Sartori ◽  
Elenara Lemos-Senna ◽  
Marcos A S Silva
Keyword(s):  
High Performance ◽  
Early Stage ◽  
Current Method ◽  
Entrapment Efficiency ◽  
High Performance Liquid Chromatographic ◽  
Reversed Phase ◽  
Calibration Graph ◽  
Formulation Development ◽  
Relative Standard ◽  
Limit Of Quantitation

Abstract A simple, rapid, and sensitive reversed-phase column high-performance liquid chromatographic method was developed and validated to quantify camptothecin (CPT) in polymeric nanocapsule suspensions. The chromatographic separation was performed on a Supelcosil LC-18 column (15 cm 4.6 mm id, 5 m) using a mobile phase consisting of methanol10 mM KH2PO4 (60 + 40, v/v; pH 2.8) at a flow rate of 1.0 mL/min and ultraviolet detection at 254 nm. The calibration graph was linear from 0.5 to 3.0 g/mL with a correlation coefficient of 0.9979, and the limit of quantitation was 0.35 g/mL. The assay recovery ranged from 97.3 to 105.0. The intraday and interday relative standard deviation values were <5.0. The validation results confirmed that the developed method is specific, linear, accurate, and precise for its intended use. The current method was successfully applied to the evaluation of CPT entrapment efficiency and drug content in polymeric nanocapsule suspensions during the early stage of formulation development.

scholarly journals Development of a New High-Performance Liquid Chromatographic Method for the Determination of Ceftazidime

2008 ◽  
Vol 91 (4) ◽  
pp. 739-743 ◽  
Author(s):  
Andréia de Haro Moreno ◽  
Hérida Regina Nunes Salgado
Keyword(s):  
High Performance ◽  
High Performance Liquid Chromatographic ◽  
Reversed Phase ◽  
Hplc Method ◽  
Calibration Graph ◽  
Raw Material ◽  
Relative Standard ◽  
Validation Parameters ◽  
Liquid Chromatographic

Abstract A rapid, accurate, and sensitive high-performance liquid chromatographic (HPLC) method was developed and validated for the determination of ceftazidime in pharmaceuticals. The method validation parameters yielded good results and included range, linearity, precision, accuracy, specificity, and recovery. The excipients in the commercial powder for injection did not interfere with the assay. Reversed-phase chromatography was used for the HPLC separation on a Waters C18 (WAT 054275; Milford, MA) column with methanolwater (70 + 30, v/v) as the mobile phase pumped isocratically at a flow rate of 1.0 mL/min. The effluent was monitored at 245 nm. The calibration graph for ceftazidime was linear from 50.0 to 300.0 g/mL. The values for interday and intraday precision (relative standard deviation) were <1. The results obtained by the HPLC method were calculated statistically by analysis of variance. We concluded that the HPLC method is satisfactory for the determination of ceftazidime in the raw material and pharmaceuticals.

scholarly journals Development and Validation of Column High-Performance Liquid Chromatographic and Ultraviolet Spectrophotometric Methods for Citalopram in Tablets

2008 ◽  
Vol 91 (1) ◽  
pp. 52-58 ◽  
Author(s):  
Jlia Menegola ◽  
Martin Steppe ◽  
Elfrides E S Schapoval
Keyword(s):  
Spectrophotometric Method ◽  
High Performance ◽  
Limit Of Detection ◽  
High Performance Liquid Chromatographic ◽  
Reversed Phase ◽  
Spectrophotometric Methods ◽  
Relative Standard ◽  
Limit Of Quantitation ◽  
Significant Difference ◽  
Liquid Chromatographic

Abstract Column high-performance liquid chromatographic (LC) and UV spectrophotometric methods for the quantitative determination of citalopram, a potent and selective serotonin reuptake inhibitor, in tablets were developed. The parameters linearity, precision, accuracy, specificity, robustness, limit of detection, and limit of quantitation were studied according to International Conference on Harmonization guidelines. Chromatography was carried out by the reversed-phase technique on an ACE C18 column with a mobile phase composed of 0.30 triethylamine solutionacetonitrile (55 + 45, v/v) adjusted to pH 6.6 with 10 ortho-phosphoric acid at a flow rate of 1.0 mL/min and 25C. The UV spectrophotometric method was performed at 239 nm. The linearity of the LC method was in the range of 10.0070.00 g/mL, and 2.5017.50 g/mL for the UV spectrophotometric method. The interday and intraday assay precision was <1.5 (relative standard deviation) for the LC and UV spectrophotometric methods. The recoveries were in the range 100.70101.35 for the LC method and 98.4898.65 for the UV spectrophotometric method. Statistical analysis by Student's t-test showed no significant difference between the results obtained by the 2 methods. The proposed methods are highly sensitive, precise, and accurate and can be used for the reliable quantitation of citalopram in tablets.

Rapid and Sensitive Liquid Chromatographic Method for Determination of Anastrozole in Different Polymer–Lipid Hybrid Nanoparticles

2021 ◽  
pp. 247263032098230
Author(s):  
Dilshad Ahmad ◽  
Faisal A. Al Meshaiti ◽  
Yazeed K. Al Anazi ◽  
Osama Al Owassil ◽  
Alaa Eldeen B. Yassin
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
Reversed Phase ◽  
Hplc Method ◽  
Hybrid Nanoparticles ◽  
Array Detector ◽  
Relative Standard ◽  
Validation Parameters ◽  
Limit Of Quantitation ◽  
Inhibitor Drug

Anastrozole, an aromatase inhibitor drug, is used for the treatment of breast cancer in pre- and postmenopausal women. Anastrozole’s incorporation into nanoparticulate carriers would enhance its therapeutic performance. To perceive the exact loaded amount of drug in nanocarriers, a valid analytical method is required. The reversed-phase high-performance liquid chromatography (RP-HPLC) method was developed and validated by using the C18 column, 150 × 4.6 mm, 5 µm particle size, in isocratic mobile phase composed of 50:50 V/V (volume/volume) acetonitrile–phosphate buffer (pH 3) flowing at a rate of 1.0 mL/min, and a diode array detector (DAD) set at λmax = 215 nm. The validation parameters such as linearity, accuracy, specificity, precision, and robustness have proven the accuracy of the method, with the relative standard deviation percentage (% RSD) values < 2. The limit of detection of the method was found equal to 0.0150 µg/mL, and the limit of quantitation was 0.0607 µg/mL. The percent recovery of sample was in the range of 98.04–99.25%. The method has the advantage of being rapid with a drug retention time of 2.767 min, specific in terms of resolution of peaks void of interference with any of the excipients, and high reproducibility. This makes it highly applicable for quality control purposes.

scholarly journals Determination of Finasteride in Tablets by High Performance Liquid Chromatography

2007 ◽  
Vol 4 (1) ◽  
pp. 109-116 ◽  
Author(s):  
K. Basavaiah ◽  
B. C. Somashekar
Keyword(s):  
High Performance ◽  
Internal Standard ◽  
High Performance Liquid Chromatographic ◽  
Reversed Phase ◽  
Calibration Graph ◽  
Official Method ◽  
Pharmaceutical Dosage Forms ◽  
Bulk Drug ◽  
Liquid Chromatographic

A rapid, highly sensitive high performance liquid chromatographic method has been developed for the determination of finasteride(FNS) in bulk drug and in tablets. FNS was eluted from a ODS C18reversed phase column at laboratory temperature (30 ± 2°C) with a mobile phase consisting of methanol and water (80+20) at a flow rate of 1 mL min-1with UV detection at 225 nm. The retention time was ∼ 6.1 min and each analysis took not more than 10 min. Quantitation was achieved by measurement of peak area without using any internal standard. Calibration graph was linear from 2.0 to 30 μg mL-1with limits of detection (LOD) and quantification (LOQ) being 0.2 and 0.6 μg mL-1, respectively. The method was validated according to the current ICH guidelines. Within-day co efficients of variation (CV) ranged from 0.31 to 0.69% and between-day CV were in the range 1.2-3.2%. Recovery of FNS from the pharmaceutical dosage forms ranged from 97.89 – 102.9 with CV of 1.41-4.13%. The developed method was compared with the official method for FNS determination in its tablet forms.

scholarly journals SENSITIVE DETERMINATION OF RELATED SUBSTANCES IN PIOGLITAZONE HYDROCHLORIDE BY HPLC

2017 ◽  
Vol 9 (2) ◽  
pp. 34
Author(s):  
N. Balaji ◽  
Sayeeda Sultana
Keyword(s):  
Mobile Phase ◽  
High Performance ◽  
Limit Of Detection ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Internal Diameter ◽  
Related Substances ◽  
Relative Standard ◽  
Limit Of Quantitation

Objective: An efficient, high performance liquid chromatographic method has been developed and validated for the quantification of related substances in pioglitazone hydrochloride drug substance.Methods: This method includes the determination of three related substances in pioglitazone hydrochloride. The mobile phase A is 0.1% w/v triethylamine in water with pH 2.5 adjusted by dilute phosphoric acid. The mobile phase B is premixed and degassed mixtures of acetonitrile and methanol. The flow rate was 1 ml/min. The elution used was gradient mode. The HPLC column used for the analysis was symmetry C18 with a length of 250 mm, the internal diameter of 4.6 mm and particle size of 5.0 microns.Results: The developed method was found to be linear with the range of 0.006-250% with a coefficient of correlation 0.99. The precision study revealed that the percentage relative standard deviation was within the acceptable limit. The limit of detection and limit of quantitation of the impurities was less than 0.002%and 0.006% with respect to pioglitazone hydrochloride test concentration of 2000 µg/ml respectively. This method has been validated as per ICH guidelines Q2 (R1).Conclusion: A reliable, economical HPLC method was magnificently established for quantitative analysis of related substances of pioglitazone hydrochloride drug substance.

scholarly journals Validated Reversed-Phase Column High-Performance Liquid Chromatographic Method for Separation and Quantification of Polyphenolics and Furocoumarins in Herbal Drugs

2008 ◽  
Vol 91 (5) ◽  
pp. 1020-1024
Author(s):  
Raghavan Govindarajan ◽  
Dhirendra Pratap Singh ◽  
Ajay Kumar Singh Rawat
Keyword(s):  
High Performance ◽  
High Performance Liquid Chromatographic ◽  
Reversed Phase ◽  
Herbal Drugs ◽  
Whole Plant ◽  
Relative Standard ◽  
Different Types ◽  
Photodiode Array ◽  
Almost All ◽  
Liquid Chromatographic

Abstract A rapid column high-performance liquid chromatographic-photodiode array method has been developed for the separation and identification of secondary metabolites, especially different types of phenols and furocoumarins, in a 35 min chromatographic run. The method has been optimized and validated for selectivity, precision, recovery, and robustness with the aim of application for standardization of selected herbal drugs. Almost all of the tested compounds had linearity of &gt;98, with relative standard deviation &lt;10 in terms of variation of retention time. Interday and intraday variability was &lt;5. The developed method has been successfully applied in identification and quantification of phenols and furocoumarins present in different plants, viz., Artemisia pallens (whole plant), Hibiscus rosa-sinensis DC (flower), Heracleum candicans DC (fruit), and Ficus carica Linn (bark). The results indicate that the method is rapid, accurate, and robust for the analysis of different types of phenols and furocoumarins and, hence, can be successfully used in the quality control and standardization of plant extracts and herbal drugs.

scholarly journals Simple and Rapid Liquid Chromatography Method for Determination of Rifabutin in Plasma

2013 ◽  
Vol 9 (2) ◽  
pp. 26-29 ◽  
Author(s):  
AK Hemanth Kumar ◽  
V Sudha ◽  
Geetha Ramachandran
Keyword(s):  
High Performance ◽  
High Performance Liquid Chromatographic ◽  
Reversed Phase ◽  
Pharmacokinetic Studies ◽  
Chromatography Method ◽  
Liquid Chromatographic Method ◽  
Relative Standard ◽  
Liquid Chromatography Method ◽  
Liquid Chromatographic

A high performance liquid chromatographic method for determination of rifabutin in human plasma was  developed. The method involved deproteinisation of the sample with acetonitrile and analysis of the  supernatant using a reversed-phase C18 column (250mm) and UV detection at a wavelength of 265nm.  The assay was specific for rifabutin and linear from 0.025 to 10.0μg/ml. The relative standard deviation  of intra- and inter-day assays was lower than 10%. The method was able to remove interfering materials  in plasma, yielding an average recovery of rifabutin from plasma of 101%. Due to its simplicity, the assay  can be used for pharmacokinetic studies of rifabutin. SAARC Journal of Tuberculosis, Lung Diseases & HIV/AIDS; 2012; IX(2) 26-29 DOI: http://dx.doi.org/10.3126/saarctb.v9i2.7975

scholarly journals Quantitation of Sitagliptin in Drug Product by Validated Reversed Phase Liquid Chromatographic Technique

2018 ◽  
Vol 17 (1) ◽  
pp. 123-129
Author(s):  
Sharifa Sultana ◽  
Md Shahadat Hossain ◽  
Md Samiul Islam ◽  
Abu Shara Shamsur Rouf
Keyword(s):  
High Performance ◽  
Drug Product ◽  
Linear Regression Analysis ◽  
Analysis Data ◽  
High Performance Liquid Chromatographic ◽  
Reversed Phase ◽  
Chromatographic Technique ◽  
Pharmaceutical Dosage Form ◽  
Relative Standard ◽  
Liquid Chromatographic

A novel reversed phase ultra-high performance liquid chromatographic (RP-UHPLC) method was developed for the estimation of sitagliptin in pharmaceutical dosage form. Separation was done by a X-bridge C18 column (4.6 i.d.× 150 mm, 5 μm particle size) with a flow rate of 1 ml/min using phosphate buffer (pH 6) and acetonitrile (70:30, v/v) as mobile phase at 268 nm using photodiode array plus (PDA+) detector. The retention time was found at 4.607 min. The developed method was validated as per the requirements of ICH-Q2B guidelines for specificity, system suitability, linearity, precision, accuracy, sensitivity and robustness. The linear regression analysis data for the linearity plot showed correlation coefficient values of 0.999 with LOD value of 0.06 μg/ml and LOQ of 0.225 μg/ml. The relative standard deviation (%RSD) for inter-day and intra- day precision was not more than 2.0%. The method was found to be accurate with percentages recovery of 98.50±0.03 to 99.70±0.05 and the % RSD was less than 2. The results showed that the proposed method is highly convenient for routine analysis of sitagliptin.Dhaka Univ. J. Pharm. Sci. 17(1): 123-129, 2018 (June)

scholarly journals Gas Chromatographic Analysis of Capsaicin in Gochujang

2008 ◽  
Vol 91 (2) ◽  
pp. 387-391 ◽  
Author(s):  
Jaeho Ha ◽  
Kyu-Jai Han ◽  
Ki-Jin Kim ◽  
Seung-Weon Jeong
Keyword(s):  
High Performance ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Calibration Graph ◽  
Internal Diameter ◽  
Determination Limit ◽  
Flame Ionization ◽  
Relative Standard ◽  
Validation Parameters ◽  
Liquid Chromatographic

Abstract A sensitive, precise, and specific gas chromatographic (GC) method was developed for the analysis of capsaicin in Gochujang and validated by comparing with a column high-performance liquid chromatographic (HPLC) method (AOAC 995.03). The method validation parameters yielded good results, including linearity, precision, accuracy, and recovery. The GC separation was performed on a (5 phenyl)-methylpolysiloxane column [length 30 m, internal diameter (id) 250 μm, film thickness 0.25 μm] followed by flame ionization detection. The conditions of temperature programming were initially 220Cfor 1min, rampat5C/minto270C, and hold for 10 min. The recovery of capsaicin in Gochujang was more than 92, and the detection limit and lower determination limit of the GC analysis were 1.0 and 5.0 μg/g, respectively. The calibration graph for capsaicin was linear from 1 to 250 μg/mL for GC and 0.5 to 50 μg/mL for HPLC. The interday and intraday precisions (relative standard deviations) were &lt;4.02.

Analysis of spectinomycin in fermentation broth by reversed-phase chromatography

2009 ◽  
Vol 63 (6) ◽  
Author(s):  
Hong Yan ◽  
Pei Xu ◽  
Hai Huang ◽  
Juan Qiu
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
Fermentation Broth ◽  
Correlation Coefficients ◽  
High Performance Liquid Chromatographic ◽  
Reversed Phase ◽  
Hplc Method ◽  
Standard Curve ◽  
Relative Standard ◽  
Liquid Chromatographic

AbstractA pre-column derivatized high-performance liquid chromatographic (HPLC) method with ultraviolet-visible detection was developed to measure the concentrations of spectinomycin in fermentation broth. Derivatization reagents, 2,4-dinitrophenylhydrazine in acetonitrile (5 mg mL−1) and trifluoroacetic acid in acetonitrile (0.8 mol L−1), were added to an aliquot of the fermentation broth, and the mixture was incubated for 60 min at 70°C. The resulting derivative was separated from other compounds by isocratic elution in a reversed-phase column Zorbax SB-C18 (250 mm × 4.6 mm, 5 µm). Mobile phase consisted of acetonitrile, tetrahydrofuran, and water (φ r = 40: 35: 25) and the flow rate was 1.0 mL min−1. The detection wavelength was 415 nm. The standard curve for spectinomycin sulfate was linear with correlation coefficients of 0.9997 in the range of 25 µg mL−1 to 600 µg mL−1. The relative standard deviation values ranged from 0.43 % to 2.18 % depending on the concentration of samples. The average recovery was 101.5 %. The limit of detection was 50 ng mL−1.

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