scholarly journals Simultaneous Determination of Rofecoxib and Tizanidine by HPTLC

2009 ◽  
Vol 6 (1) ◽  
pp. 295-302 ◽  
Author(s):  
Uttam D. Pawar ◽  
Aruna V. Sulebhavikar ◽  
Abhijit V. Naik ◽  
Satish G. Pingale ◽  
Kiran V. Mangaonkar
Keyword(s):  
Simultaneous Determination ◽  
High Performance ◽  
Dosage Form ◽  
Limit Of Detection ◽  
Internal Standard ◽  
Volume Ratio ◽  
Standard Addition ◽  
Limit Of Quantification ◽  
Chromatography Method

An innovative high performance thin layer chromatography method was developed and validated for simultaneous determination of rofecoxib and tizanidine from tablet dosage form. Rosiglitazone maleate was used as an internal standard. The separation was achieved using HPTLC plates (Merck #5548) precoated with silica gel 60F254on aluminum sheets and a mobile phase comprising of toluene: ethyl acetate: methanol: triethyl amine in volume ratio of 6:3:0.5:0.1 (v/v/v/v), with chamber saturation of 15 min. The plate was developed up to 8 cm and air dried. The plate was then scanned and quantified at 235 nm. The linearity of rofecoxib and tizanidine were in the range of 3.75 µg/spot to 11.25 µg/spot and 0.30 µg/spot to 0.90 µg/spot respectively. The limit of detection for rofecoxib and tizanidine was found to be 45.00 ng/spot and 30.00 ng/spot respectively. The limit of quantification for rofecoxib and tizanidine was found to be 135.00 ng/spot and 90.00 ng/spot respectively. The percentage assay was found between the range of 99.58% to 103.21% for rofecoxib and 98.73% to 101.55% for tizanidine respectively, whereas recovery was found between 99.97% to 100.43% for rofecoxib and 100.00% to 101.00% for tizanidine by standard addition method. The proposed method is accurate, precise and rapid for the simultaneous determination of rofecoxib and tizanidine in dosage form

scholarly journals A Simple High-Performance Liquid Chromatography Method for Simultaneous Determination of Three Triazole Antifungals in Human Plasma

2012 ◽  
Vol 57 (1) ◽  
pp. 484-489 ◽  
Author(s):  
Mei Zhang ◽  
Grant A. Moore ◽  
Murray L. Barclay ◽  
Evan J. Begg
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Simultaneous Determination ◽  
Human Plasma ◽  
High Performance ◽  
Internal Standard ◽  
Gradient Elution ◽  
Limit Of Quantification ◽  
Chromatography Method

ABSTRACTA rapid and simple high-performance liquid chromatography (HPLC) assay was developed for the simultaneous determination of three triazole antifungals (voriconazole, posaconazole, and itraconazole and the metabolite of itraconazole, hydroxyitraconazole) in human plasma. Sample preparation involved a simple one-step protein precipitation with 1.0 M perchloric acid and methanol. After centrifugation, the supernatant was injected directly into the HPLC system. Voriconazole, posaconazole, itraconazole, its metabolite hydroxyitraconazole, and the internal standard naproxen were resolved on a C6-phenyl column using gradient elution of 0.01 M phosphate buffer, pH 3.5, and acetonitrile and detected with UV detection at 262 nm. Standard curves were linear over the concentration range of 0.05 to 10 mg/liter (r2> 0.99). Bias was <8.0% from 0.05 to 10 mg/liter, intra- and interday coefficients of variation (imprecision) were <10%, and the limit of quantification was 0.05 mg/liter.

scholarly journals Simultaneous Determination of Aceclofenac, Paracetamol and Chlorzoxazone by HPLC in Tablet Dose Form

2009 ◽  
Vol 6 (1) ◽  
pp. 289-294 ◽  
Author(s):  
Uttam D. Pawar ◽  
Abhijit V. Naik ◽  
Aruna V. Sulebhavikar ◽  
Tirumal A. Datar ◽  
Kiran. V. Mangaonkar
Keyword(s):  
Simultaneous Determination ◽  
High Performance ◽  
Limit Of Detection ◽  
Potassium Dihydrogen Phosphate ◽  
Standard Addition ◽  
High Performance Liquid Chromatographic ◽  
Reversed Phase ◽  
Dihydrogen Phosphate ◽  
Limit Of Quantification

A simple, fast and precise reversed phase high performance liquid chromatographic method is developed for the simultaneous determination of aceclofenac, paracetamol and chlorzoxazone. Chromatographic separation of the three drugs was performed on an Intersil C18column (250 mm × 4.6 mm, 5µm) as stationary phase with a mobile phase comprising of 10 mM potassium dihydrogen phosphate (pH adjusted to 5.55 with ammonia): acetonitrile in the ratio 60:40 (v/v) at a flow rate of 1.0 mL/min and UV detection at 205 nm. The linearity of aceclofenac, paracetamol and chlorzoxazone were in the range of 5.00-15.00 µg/µL, 25.00-75.00 µg/µL and 25.00-75.00 µg/µL respectively. The limit of detection for aceclofenac, paracetamol and chlorzoxazone was found to be 18.0 ng/mL, 22.0 ng/mL and 9.0 ng/mL respectively whereas, the limit of quantification was found to be 55 ng/mL, 65 ng/mL and 27.0 ng/mL respectively. The recovery was calculated by standard addition method. The average recovery was found to be 99.04%, 99.57% and 101.63% for aceclofenac, paracetamol and chlorzoxazone respectively. The proposed method was found to be accurate, precise and rapid for the simultaneous determination of aceclofenac, paracetamol and chlorzoxazone

scholarly journals DEVELOPMENT AND VALIDATION OF A STABILITY INDICATING REVERSE PHASEHIGH PERFORMANCE LIQUID CHROMATOGRAPHY METHOD FOR SIMULTANEOUS DETERMINATION OF CLINDAMYCIN, METRONIDAZOLE, AND CLOTRIMAZOLE IN PHARMACEUTICAL COMBINED DOSAGE FORMS

2016 ◽  
Vol 10 (1) ◽  
pp. 111 ◽  
Author(s):  
Revathi Naga Lakshmi Ponnuri ◽  
Prahlad Pragallapati ◽  
Mastanamma Sk ◽  
Ravindra N ◽  
Venkata Basaveswara Rao Mandava ◽  
...  
Keyword(s):  
Liquid Chromatography ◽  
Simultaneous Determination ◽  
High Performance ◽  
Limit Of Detection ◽  
Degradation Products ◽  
Reverse Phase ◽  
Limit Of Quantification ◽  
Chromatography Method ◽  
Liquid Chromatography Method

ABSTRACTObjective: The objective of present work was to develop and validate a simple, fast, precise, selective, and accurate reverse phase high-performanceliquid chromatography method for the simultaneous determination of Clindamycine, Metronidazole and Clotrimazole in a pharmaceutical dosageform.Methods: The separation of these three drugs was achieved on ODS 250×4.6 mm, 5 mm C column. Mobile phase containing 0.1% ortho phosphoricacid buffer and acetonitrile in the ratio of 55:45 v/v was pumped through column at a flow rate of 1 ml/minute. Temperature was maintained at 30°Cand ultraviolet detection at 238 nm.18Results: The retention times were observed to be 2.591, 3.584, and 4.221 minutes for Clindamycine, Metronidazole, and Clotrimazole, respectively.Linearity was found to be 25-150 μg/ml Clindamycine, Metronidazole, and Clotrimazole, respectively. The method was statistically validated forlinearity, recovery, the limit of detection (LOD), limit of quantification (LOQ), accuracy, and precision. The stress testing of the drugs individually andtheir mixture are carried out under acidic, alkaline, oxidation, photostability, and thermal degradation conditions and its degradation products arewell resolved from the analyte peaks.Conclusion: This method was successfully validated for accuracy, precision, and linearity, LOD, and LOQ.Keywords: Clindamycine, Metronidazole, Clotrimazole, Reverse phase-high performance liquid chromatography, Simultaneous determination,Degradation studies.

scholarly journals DETERMINATION OF 10-GINGEROL IN INDIAN GINGER BY VALIDATED HPTLC METHOD OF SAMPLES COLLECTED ACROSS SUBCONTINENT OF INDIA

2016 ◽  
Vol 8 (12) ◽  
pp. 190
Author(s):  
Kamran Ashraf ◽  
Syed Adnan Ali Shah ◽  
Mohd Mujeeb
Keyword(s):  
Thin Layer ◽  
Thin Layer Chromatography ◽  
High Performance ◽  
Limit Of Detection ◽  
Limit Of Quantification ◽  
Chromatography Method ◽  
Aluminum Plates ◽  
Layer Chromatography ◽  
Hptlc Method

<p><strong>Objective: </strong>A simple, sensitive, precise, and accurate stability indicating HPTLC (high-performance thin-layer chromatography) method for analysis of 10-gingerol in ginger has been developed and validated as perICH guidelines.</p><p><strong>Methods: </strong>The separation was achieved on TLC (thin layer chromatography) aluminum plates pre-coated with silica gel 60F<sub>254</sub> using n-hexane: ethyl acetate 55:45 (%, v/v) as a mobile phase. Densitometric analysis was performed at 569 nm.</p><p><strong>Results: </strong>This system was found to have a compact spot of 10-gingerol at <em>R</em><sub>F</sub> value of 0.57±0.03. For the proposed procedure, linearity (<em>r</em><sup>2</sup> = 0.998±0.02), limit of detection (18ng/spot), limit of quantification (42 ng/spot), recovery (ranging from 98.35%–100.68%), were found to be satisfactory.</p><p><strong>Conclusion: </strong>Statistical analysis reveals that the content of 10-gingerol in different geographical region varied significantly. The highest and lowest concentration of 10-gingerol in ginger was found to be present in a sample of Patna, Lucknow and Surat respectively which inferred that the variety of ginger found in Patna, Lucknow are much superior to other regions of India.</p>

Determination of tigecycline in turkey plasma by LC-MS/MS: validation and application in a pharmacokinetic study

2017 ◽  
Vol 20 (2) ◽  
pp. 241-249 ◽  
Author(s):  
A. Jasiecka-Mikołajczyk ◽  
J.J. Jaroszewski
Keyword(s):  
Pharmacokinetic Study ◽  
High Performance ◽  
Limit Of Detection ◽  
Internal Standard ◽  
Reversed Phase ◽  
Selected Reaction Monitoring ◽  
Limit Of Quantification ◽  
Complicated Skin ◽  
Intravenous And Oral Administration

Abstract Tigecycline (TIG), a novel glycylcycline antibiotic, plays an important role in the management of complicated skin and intra-abdominal infections. The available data lack any description of a method for determination of TIG in avian plasma. In our study, a selective, accurate and reversed-phase high performance liquid chromatography-tandem mass spectrometry method was developed for the determination of TIG in turkey plasma. Sample preparation was based on protein precipitation and liquid-liquid extraction using 1,2-dichloroethane. Chromatographic separation of TIG and minocycline (internal standard, IS) was achieved on an Atlantis T3 column (150 mm × 3.0 mm, 3.0 μm) using gradient elution. The selected reaction monitoring transitions were performed at 293.60 m/z → 257.10 m/z for TIG and 458.00 m/z → 441.20 m/z for IS. The developed method was validated in terms of specificity, selectivity, linearity, lowest limit of quantification, limit of detection, precision, accuracy, matrix effect, carry-over effect, extraction recovery and stability. All parameters of the method submitted to validation met the acceptance criteria. The assay was linear over the concentration range of 0.01-100 μg/ml. This validated method was successfully applied to a TIG pharmacokinetic study in turkey after intravenous and oral administration at a dose of 10 mg/kg at various time-points.

scholarly journals Determination of Formaldehyde by HPLC with Stable Precolumn Derivatization in Egyptian Dairy Products

2018 ◽  
Vol 2018 ◽  
pp. 1-5 ◽  
Author(s):  
Ahmed Salem Sebaei ◽  
Ahmed M. Gomaa ◽  
A. A. El-Zwahry ◽  
E. A. Emara
Keyword(s):  
Dairy Products ◽  
High Performance ◽  
Limit Of Detection ◽  
Precolumn Derivatization ◽  
Limit Of Quantification ◽  
Chromatography Method ◽  
Derivatizing Agent ◽  
Array Detection ◽  
Liquid Chromatography Method

Formaldehyde is one of the most dangerous chemical compounds affecting the human health; exposure to it from food may occur naturally or by intentional addition. In this study a high performance liquid chromatography method for determination of formaldehyde in dairy products was described. The dairy samples were reacted and extracted with a warmed organic solvent in the presence of derivatizing agent 2,4-dinitrophenylhydrazine (DNPH) and formaldehyde; the mixture was centrifuged and followed by diode array detection. The method is validated and gives average recovery of formaldehyde at the three different levels 0.1, 5.0, and 10.0 mg/kg varied between 89% and 96%. The method is linear from the limit of quantification 0.1 mg/kg up to 10 mg/kg levels. This method is intended for formaldehyde analyses in dairy products simply with stable derivatization, minimum residue loss, excellent recovery, and accurate results with a sensitive limit of detection 0.01 mg/kg. 90 dairy samples from milk, cheese, and yogurt were investigated from seven Egyptian governorates and all samples were free from formaldehyde.

RAPID HIGH PERFORMANCE LIQUID CHROMATOGRAPHY METHOD FOR THE DETERMINATION OF RALTEGRAVIR IN HUMAN SALIVA

INDIAN DRUGS ◽  
2019 ◽  
Vol 56 (09) ◽  
pp. 68-73
Author(s):  
K Vijaya Sri ◽  
M. Shiva Kumar ◽  
M. A. Madhuri ◽  
Suresha K. ◽  
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
High Performance Liquid Chromatographic ◽  
Human Saliva ◽  
Hplc Method ◽  
Limit Of Quantification ◽  
Chromatography Method ◽  
Liquid Chromatography Method ◽  
Liquid Chromatographic

In this study, a high-performance liquid chromatographic method (HPLC) was developed, validated and applied for the determination of raltegravir in biological sample like saliva. Liquid- liquid extraction was performed for isolation of the drug and elimination of saliva interferences. Samples of saliva was extracted with 50µL of ortho phosphoric acid and 3ml of methanol was added and spiked with raltegravir. The chromatographic separation was performed on Agilent Eclipse C18 (100 mm × 4.6 mm, 3.5µm) column, by using 80:20 v/v acetonitrile: water as a mobile phase under isocratic conditions at a flow rate of 1.0 mL/min for UV detection at 240 nm. Retention time of raltegravir was found to be 1.030 min. Linearity was found to be in the range of 25-1000 ng/mL with regression equation y = 13864x + 40495 and correlation coefficient 0.999. The low % RSD value indicates the method is accurate and precise. The limit of detection (LOD) and limit of quantification (LOQ) were found to be 0.76 and 2.28 ng/mL, respectively. It can be concluded that this validated HPLC method is easy, precise, accurate, sensitive and selective for determination of raltegravir in saliva.

RP-HPLC-DAD method for simultaneous determination of desmedipham, phenmedipham and ethofumesate in a pesticide formulation

2012 ◽  
Vol 31 (1) ◽  
pp. 39 ◽  
Author(s):  
Lenče Velkoska-Markovska ◽  
Biljana Petanovska-Ilievska ◽  
Lila Vodeb
Keyword(s):  
Simultaneous Determination ◽  
High Performance ◽  
Limit Of Detection ◽  
Retention Factor ◽  
Reversed Phase ◽  
Limit Of Quantification ◽  
Column Temperature ◽  
Pesticide Formulation ◽  
Factor Separation

A fast, simple, precise and accurate reversed-phase high-performance liquid chromatography (RPHPLC)method with UV-DAD for simultaneous determination of desmedipham, phenmedipham and ethofumesate in the pesticide formulation “Inter OF” has been developed. The analysis was performed on a LiChrospher 60 RP-select B (25 cm × 0.4 cm, 5 μm, Merck) analytical column, with mobile phase of methanol/water (60/40, V/V), flow rate of 1 ml/min, UV-detection at 230 nm and constant column temperature at 25 ºC. The following parameters were determined for the developed method: retention factor, separation factor, limit of detection (LOD), limit of quantification (LOQ), precision of obtained results for peak area, linearity, recovery of analyte and active ingredients quantity in a pesticide formulation.

scholarly journals A Simple and Cost-Effective TLC-Densitometric Method for the Quantitative Determination of Acetylsalicylic Acid and Ascorbic Acid in Combined Effervescent Tablets

Molecules ◽  
2018 ◽  
Vol 23 (12) ◽  
pp. 3115 ◽  
Author(s):  
Alina Pyka-Pająk ◽  
Małgorzata Dołowy ◽  
Wioletta Parys ◽  
Katarzyna Bober ◽  
Grażyna Janikowska
Keyword(s):  
Ascorbic Acid ◽  
Quantitative Determination ◽  
Acetylsalicylic Acid ◽  
High Performance ◽  
Limit Of Detection ◽  
Volume Ratio ◽  
Cost Effective ◽  
Pharmaceutical Formulations ◽  
Limit Of Quantification

A new, simple, and cost-effective TLC-densitometric method has been established for the simultaneous quantitative determination of acetylsalicylic acid and ascorbic acid in combined effervescent tablets. Separation was performed on aluminum silica gel 60F254 plates using chloroform-ethanol-glacial acid at a volume ratio of 5:4:0.03 as the mobile phase. UV densitometry was performed in absorbance mode at 200 nm and 268 nm for acetylsalicylic acid and ascorbic acid, respectively. The presented method was validated as per ICH guidelines by specificity, linearity, accuracy, precision, limit of detection, limit of quantification, and robustness. Method validations indicate a good sensitivity with a low value of LOD and LOQ of both examined active substances. The linearity range was found to be 1.50–9.00 μg/spot and 1.50–13.50 μg/spot for acetylsalicylic and ascorbic acid, respectively. A coefficient of variation that was less than 3% confirms the satisfactory accuracy and precision of the proposed method. The results of the assay of combined tablet formulation equal 97.1% and 101.6% in relation to the label claim that acetylsalicylic acid and ascorbic acid fulfill pharmacopoeial requirements. The developed TLC-densitometric method can be suitable for the routine simultaneous analysis of acetylsalicylic acid and ascorbic acid in combined pharmaceutical formulations. The proposed TLC-densitometry may be an alternative method to the modern high-performance liquid chromatography in the quality control of above-mentioned substances, and it can be applied when HPLC or GC is not affordable in the laboratory.

scholarly journals HPTLC Method for Simultaneous Determination of Lopinavir and Ritonavir in Capsule Dosage Form

2008 ◽  
Vol 5 (4) ◽  
pp. 706-712 ◽  
Author(s):  
A. V. Sulebhavikar ◽  
U. D. Pawar ◽  
K. V. Mangoankar ◽  
N. D. Prabhu-Navelkar
Keyword(s):  
Simultaneous Determination ◽  
Limit Of Detection ◽  
Uv Light ◽  
Pharmaceutical Preparation ◽  
Volume Ratio ◽  
Detector Response ◽  
Control Analysis ◽  
Limit Of Quantification ◽  
Hptlc Method

A rapid and simple high performance thin layer chromatography (HPTLC) method with densitometry at λ=263 nm was developed and validated for simultaneous determination of lopinavir and ritonavir from pharmaceutical preparation. Separation was performed on aluminum-backed silica gel 60F254HPTLC plates as stationary phase and using a mobile phase comprising of toluene, ethyl acetate, methanol and glacial acetic acid, in the volume ratio of 7.0:2.0:0.5:0.5 (v/v) respectively. After development, plates were observed under UV light. The detector response was linear in the range of 6.67 to 20.00 µg/spot and 1.67 to 5.00 µg/spot for lopinavir and ritonavir respectively. The validated lowest limit of detection was 21.00 ng/spot and 5.10 ng/spot whereas lowest limit of quantification was 7.00 ng/spot and 21.00 ng/spot for lopinavir and ritonavir respectively. The percentage assay of lopinavir and ritonavir was found between 98.23 to 102.28% and 98.03 to 103.50% respectively. The described method has the advantage of being rapid and easy. Hence it can be applied for routine quality control analysis of lopinavir and ritonavir from pharmaceutical preparation and stability studies.

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