scholarly journals Simultaneous RP-HPLC determination of sparfloxacin and dexamethasone in pharmaceutical formulations

2013 ◽  
Vol 49 (2) ◽  
pp. 301-309 ◽  
Author(s):  
Syed Naeem Razzaq ◽  
Muhammad Ashfaq ◽  
Irfana Mariam ◽  
Islam Ullah Khan ◽  
Syed Saleem Razzaq
Keyword(s):  
Degradation Products ◽  
Pharmaceutical Formulations ◽  
Hplc Method ◽  
Array Detector ◽  
Diode Array ◽  
Stability Studies ◽  
Diode Array Detector ◽  
Rp Hplc ◽  
Peak Purity

The present study describes the development and subsequent validation of simple and accurate stability indicating RP-HPLC method for the determination of sparfloxacin and dexamethasone in pharmaceutical formulations in the presence of their stress-induced degradation products. Both the drugs and their stress-induced degradation products were separated within 10 minutes using C8 column and mixture of methanol and 0.02 M phosphate buffer pH 3.0 (60:40 v/v, respectively) as mobile phase at 270 nm using diode array detector. Regression analysis showed linearity in the range of 15-105 µg/mL for sparfloxacin and 5-35 µg/mL for dexamethasone. All the analytes were adequately resolved with acceptable tailing. Peak purity of the two drugs was also greater than 0.9999, showing no co-elution peaks. The developed method was applied for simultaneous determination of sparfloxacin and dexamethasone in pharmaceutical formulations for stability studies.

QBD BASED RP-HPLC METHOD FOR SCREENING AND ANALYSIS OF TELAPRAVIR AND 7 OTHER ANTIRETROVIRAL AGENTS

INDIAN DRUGS ◽  
2015 ◽  
Vol 52 (02) ◽  
pp. 20-33
Author(s):  
N. S Kumar ◽  
◽  
R Kumaraswamy ◽  
S. Shantikumar ◽  
D. Paul
Keyword(s):  
Quality By Design ◽  
Pharmaceutical Formulations ◽  
Active Pharmaceutical Ingredient ◽  
Hplc Method ◽  
Array Detector ◽  
Simultaneous Estimation ◽  
Rp Hplc ◽  
Ich Guidelines ◽  
Full Factorial

The present study describes the separation and simultaneous estimation of eight anti-retroviral drugs, namely, Telaprevir (TPV), Emtricitabine (ECB), Fosamprenavir (FANV), Tenofavir (TNF), Ritonavir (RNV), Raltegravir (RGV) and Oseltamivir (OSMV) and Zidovudine (ZDV) as an active pharmaceutical ingredient, by RP-HPLC method by applying the principles of Quality by Design (QbD). An application of DoE (Design of Experiments) full factorial design was used for initial screening and optimization. The final optimized method consists of separation being carried out on a Fortis C18 column (150 mm × 4.6 mm, 5μ particle size) using acetonitrile and 10 mm ammonium formate buffer (pH 3 adjusted with formic acid) using a gradient program. The quantitative evaluation was performed with a diode array detector at 251 nm and 230 nm with a flow rate of 1 mL min–1. Suitability of this method for the quantitative determination of the drugs was proved by validation in accordance with the International Conference on Harmonization (ICH) guidelines. The method is selective, precise, robust and accurate and can be used for routine analysis of pharmaceutical formulations in quality control and counterfeit screening.

scholarly journals DEVELOPMENT AND VALIDATION OF STABILITY INDICATING RP-HPLC METHOD FOR DETERMINATION OF β-ACETYLDIGOXIN

2016 ◽  
Vol 9 (1) ◽  
pp. 54
Author(s):  
Megha Sharma ◽  
Neeraj Mahindroo
Keyword(s):  
High Performance ◽  
Degradation Products ◽  
Hplc Method ◽  
Stability Study ◽  
Array Detector ◽  
Forced Degradation ◽  
Simple Method ◽  
Stability Indicating ◽  
Rp Hplc

Objective: The objective of the present study was to develop and validate a novel stability indicating reverse phase-high performance liquid chromatography (RP-HPLC) method for determination of β-acetyldigoxin, an active pharmaceutical ingredient (API).Methods: The chromatographic separation was carried out on Agilent Technologies 1200 series HPLC system equipped with photo diode array detector and C-18 (4.6x250 mm, 5 µ) column. The mobile phase consisted of water: acetonitrile (65:35 v/v), delivered at a flow rate of 1.5 ml/min and eluents were monitored at 225 nm.Results: The retention time of β-acetyldigoxin was 9.2 min. The method was found to be linear (R2= 0.9995) in the range of 31.25-500 µg/ml. The accuracy studies showed the mean percent recovery of 101.02%. LOD and LOQ were observed to be 0.289 µg/ml and 0.965 µg/ml, respectively. The method was found to be robust and system suitability testing was also performed. Forced degradation analysis was carried out under acidic, alkaline, oxidative and photolytic stress conditions. Significant degradation was observed under tested conditions, except for oxidative condition. The method was able to separate all the degradation products within runtime of 20 min and was able to determine β-acetyldigoxin unequivocally in presence of degradation products.Conclusion: The novel, economic, rapid and simple method for analysis of β-acetyldigoxin is reported. The developed method is suitable for routine quality control and its determination as API, and in pharmaceutical formulations and stability study samples.

scholarly journals RP-HPLC Estimation of Bumetanide and its Impurities in Oral Solid Dosage Form

2019 ◽  
Vol 31 (10) ◽  
pp. 2215-2221
Author(s):  
P. Suresh Kumar ◽  
G.V. Krishna Mohan ◽  
A. Naga Babu
Keyword(s):  
Limit Of Detection ◽  
Degradation Products ◽  
Drug Product ◽  
Pharmaceutical Formulations ◽  
Hplc Method ◽  
Fixed Dose ◽  
Array Detector ◽  
Rp Hplc ◽  
Photodiode Array Detector ◽  
Limit Of Quantitation

A novel and simultaneous stability indicating RP-HPLC method has been developed for quantitative analysis of bumetanide in fixed dose pharmaceutical formulations. Bumetanide and its degradation products are well separated by the Discovery C18, 250 × 4.6 mm, 5 μm column as a stationary phase and (50:50 v/v) of 0.1 % o-phthalaldehyde and acetonitrile as a mobile phase. All the compounds are monitored using photodiode array detector at 254 nm with an isocratic method and the flow rate of 1.0 mL/min was maintained. Validation of method was performed as per International Council for Harmonization (ICH) guidelines and the parameters namely; precision, accuracy, specificity, stability, robustness, linearity, limit of quantitation (LOQ) and limit of detection (LOD) were evaluated. The linearity of the proposed method was found to be 0.315-1.875 μg/mL for bumetanide and its impurities. The developed method is more economical and suitable for laboratory use because of solvent consumption is very less. Hence, the developed method can be used for the determination of bumetanide and its impurities in drug product stability studies and pharmaceutical formulations.

scholarly journals Quantitative Determination of Chemical Constituents from Seeds of Nigella sativa L. Using HPLC-UV and Identification by LC-ESI-TOF

2010 ◽  
Vol 93 (6) ◽  
pp. 1778-1787 ◽  
Author(s):  
Bharathi Avula ◽  
Yan-Hong Wang ◽  
Zulfiqar Ali ◽  
Ikhlas A Khan
Keyword(s):  
Nigella Sativa ◽  
Chemical Constituents ◽  
Hplc Method ◽  
Array Detector ◽  
Diode Array ◽  
Gradient System ◽  
Diode Array Detector ◽  
Column Material ◽  
Positive Ion

Abstract An HPLC method was developed for the simultaneous determination of nine compounds of Nigella sativa L. The separation was achieved within 23 min by using C18 column material, a wateracetonitrile mobile phase, both containing 0.1 acetic acid gradient system and a temperature of 35C. The method was validated for linearity, repeatability, LOD, and LOQ. The LOD and LOQ of nine compounds were in the range of 0.0910 and 0.325 g/mL, respectively. The wavelength used for quantification with the diode array detector was 205 and 260 nm. LC/MS coupled with electrospray ionization interface method is described for the identification of compounds in N. sativa L. samples. This method involved the use of [MH]<sup/> and [MNa]<sup/> ions in the positive ion mode with extracted ion chromatogram.

Application of RP-HPLC-Diode Array Detector after SPE to the Determination of Pesticides in Pepper Samples

2012 ◽  
Vol 95 (5) ◽  
pp. 1357-1361 ◽  
Author(s):  
Tomasz Tuzimski
Keyword(s):  
Quantitative Analysis ◽  
Plant Material ◽  
Food Samples ◽  
Array Detector ◽  
Diode Array ◽  
Diode Array Detector ◽  
Green Pepper ◽  
Rp Hplc ◽  
Chemical Groups

Abstract The application of HPLC-diode array detector (DAD) after SPE for identification and quantitative analysis of pesticides in red and green pepper samples is demonstrated. An HPLC procedure on an RP column (C18) was developed for analysis of selected pesticides from different chemical groups: metamitron, metalaxyl, linuron, and prometryn. Average recoveries for C18 Polar Plus cartridges and solvents by the proposed RP-HPLC-DAD method after SPE are presented. Average recoveries from the spiked samples and the SDs were 22.5 ± 2.2, 138.0 ± 4.1, 78.6 ± 2.8, and 109.2 ± 2.3% for metamitron, metalaxyl, linuron, and prometryn, respectively, at concentrations of 7 μg/g in the plant material. The efficiency of the SPE procedure was evaluated using real food samples. The quantities of prometryn, linuron, metalaxyl, and metamitron determined were in the ranges of 0.02–2.24 μg/g (n = 24), 0.08–1.01 μg/g (n = 9), 1.61–2.28 μg/g (n = 4), and 0.05–1.07 μg/g (n = 3), respectively, in plant material sampled in 2011. The method was validated for precision, repeatability, and accuracy.

scholarly journals Quantititative Determination of Lycorine and Galanthamine in Galanthus trojanus and G. cilicicus by HPLC-DAD

2014 ◽  
Vol 9 (8) ◽  
pp. 1934578X1400900
Author(s):  
Gulen Irem Kaya ◽  
Derya Cicek Polat ◽  
Buket Sarikaya ◽  
Mustafa Ali Onur ◽  
Nehir Unver Somer
Keyword(s):  
Biological Activities ◽  
Hplc Method ◽  
Array Detector ◽  
Diode Array ◽  
Diode Array Detector ◽  
Simple Method ◽  
Aerial Parts ◽  
Flowering Season ◽  
Low Mass

Lycorine and galanthamine have various biological activities. A reliable HPLC method coupled with DAD detection was developed and validated for the determination of galanthamine and lycorine in Galanthus trojanus and G. cilicicus. A simple method for the extraction of the alkaloids in low-mass plant samples was employed utilizing columns pre-packed with diatomaceous earth (Extrelut®). This method was applied to the aerial parts and bulbs of G. trojanus and G. cilicicus (Amaryllidaceae) collected during the flowering season. The chromatographic separation was performed using an isocratic system with a mobile phase of trifluoroacetic acid-water-acetonitrile (0.01:92.5:7.5) applied at a flow rate of 1 mL min−1 and using a diode array detector. Validation procedures showed that the method was specific, accurate and precise. The highest amount of lycorine (0.012%) was detected in the bulbs of G. trojanus collected from Çan (Çanakkale), whereas the aerial parts of this species collected from Bayramiç (Çanakkale) was not found to contain this alkaloid. In G. cilicicus samples, lycorine was only determined in the bulbs, giving yields of 0.004%; galanthamine yields were between 0.015-0.016%, but none of the G. trojanus samples contained this latter alkaloid.

scholarly journals Content of phenolic acids in rye caryopses determined using DAD-HPLC method

2013 ◽  
Vol 19 (No. 6) ◽  
pp. 201-205 ◽  
Author(s):  
R. Amarowicz ◽  
S. Weidner
Keyword(s):  
Phenolic Compounds ◽  
Phenolic Acids ◽  
Hplc Method ◽  
Uv Spectra ◽  
Array Detector ◽  
Diode Array ◽  
Diode Array Detector ◽  
Uv Spectrum ◽  
Free Phenolic Acids

Phenolic compounds were extracted from rye caryopses with 80% (v/v) methanol. Phenolic acids were determined as free compounds and those liberated from soluble esters and glycosides. The analyses were performed using a Waters HPLC system equipped with a diode array detector (DAD). The following free phenolic acids were found: p-coumaric, ferulic and sinapic; the phenolic acids liberated from soluble esters were as follows: vanillic, caffeic, p-coumaric, ferulic and sinapic; and those liberated from soluble glycosides were the following: vanillic, p-coumaric, ferulic and sinapic. In rye caryopses, phenolic acids were chiefly in the form of soluble esters. A diode array detector was especially useful for the determination of vanillic acid: the UV spectrum of this compound showed a maximum at 260 nm whereas UV spectra of other phenolic acids were characterised by maxima at longer wavelengths.

scholarly journals RP-HPLC method with indirect UV detection for determination of sodium ibandronate in pharmaceuticals

2019 ◽  
Vol 64 (02) ◽  
pp. 43-49
Author(s):  
Zharko Tanturovski ◽  
Zorica Arsova-Sarafinovska ◽  
Aneta Dimitrovska
Keyword(s):  
Sodium Salt ◽  
Pharmaceutical Formulations ◽  
Reversed Phase ◽  
Hplc Method ◽  
Uv Detection ◽  
Array Detector ◽  
Ibandronic Acid ◽  
Indirect Uv Detection ◽  
Rp Hplc

Ibandronate sodium (IBN) [(1-hydroxy-3- (methyl pentyl amino) propylidene bisphosphonic acid monosodium monohydrate)] is the sodium salt of ibandronic acid, a synthetic nitrogen-containing bisphosphonate drug. The aim of this study was to develop a sensitive and accurate RP-HPLC method with indirect UV detection for determination of IBN in pharmaceutical formulations. Chromatographic separation was performed on a Waters Bridge C18 reversed-phase column (250 x 4.6 mm I.D.; particle size 5 µm), in an isocratic mode with a mobile phase constituted of 90% buffer: 10% acetonitrile (V/V). The buffer was made using 1.5 mL ortho-phosphoric acid, 990 mg 1-Hexanesulfonic acid sodium salt 98%, 140 mg EDTA in 1000 mL flask diluted with HPLC grade water. The elution was carried out at a flow rate of 1.0 mL minˉ1. A diode array detector measured the UV absorbance at 198 nm, in inverse mode. The method was validated for specificity/selectivity, linearity, LOD, LOQ, accuracy, precision and robustness according to ICH validation guidelines. The limits of detection and quantification were calculated at 0.0163 µg/mL and 0.0495 µg/mL, respectively. The method was effectively used for determination of IBN from commercial tablets and provided good results without any interference from commonly used excipients. Keywords: RP-HPLC with indirect UV detection, Ibandronate sodium, validation, pharmaceuticals

scholarly journals Quantitative Determination by HPLC-DAD of Icariin, Epimedin A, Epimedin B, and Epimedin C in Epimedium (Berberidaceae) Species Growing in Turkey

2016 ◽  
Vol 11 (11) ◽  
pp. 1934578X1601101 ◽  
Author(s):  
Derya Cicek Polat ◽  
Maksut Coskun
Keyword(s):  
Quantitative Determination ◽  
Flow Rate ◽  
Mobile Phase ◽  
Hplc Method ◽  
Biologically Active ◽  
Array Detector ◽  
Diode Array ◽  
Gradient System ◽  
Diode Array Detector

The genus Epimedium is rich in terms of flavonoids, of which icariin, epimedin A, epimedin B and epimedin C are known especially to be biologically active. Therefore, it is important to quantify these compounds. In this study, a HPLC method coupled with DAD detection was developed and validated for the determination of icariin, epimedin A, epimedin B and epimedin C in Epimedium species growing in Turkey. The chromatographic separation was performed using a gradient system with a mobile phase of 0.1% formic acid (A) and acetonitrile (B) applied at a flow rate of 1 mL/min using a diode array detector. The highest values were, respectively, icariin 0.65%, epimedin A 0.13%, epimedin B 0.11%, epimedin C 0.06%. The highest values were obtained from the materials collected in Uzungol (Trabzon-Turkey).

Development and Validation of RP-HPLC Method for Determation of Acyclovir in Ointment

2021 ◽  
pp. 199-202
Author(s):  
Ajay Bedadurge ◽  
Kadare Mahesh ◽  
Vinod Matole ◽  
Parikshit Shirure ◽  
Sainath Suryawanshi ◽  
...  
Keyword(s):  
High Performance ◽  
Hplc Method ◽  
Array Detector ◽  
Diode Array Detector ◽  
Column Temperature ◽  
Development Method ◽  
Rp Hplc ◽  
Ich Guidelines ◽  
Development And Validation

The analytical method was developed and validated for determination of acyclovir in ointment by High performance liquid chromatography. The separation was carried out on Luna C18 column (250 × 4.6mm × 5µ). The mobile phase consists of water: acetonitrile in the ratio 88:12 at flow rate 0.8ml/min with diode array detector wavelength at 254nm.The column temperature was adjusted at 30ºC±40ºC with injection volume 20µl.The retention time of acyclovir was 4.747min. The linearity of the calibration curve was linear over the concentration range 80-120µg/ml (r2=0.9996). The validation was carried out as per ICH guidelines. The development method was easy, rapid, linear, precise, accurate and consistent.

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