scholarly journals SEPARATION AND DETERMINATION OF THE R-ISOMER OF KETOPROFEN IN A BULK DRUG SUBSTANCE BY NORMAL PHASE LIQUID CHROMATOGRAPHY

2016 ◽  
Vol 10 (1) ◽  
pp. 302
Author(s):  
Appasaheb Bajirao Lawande
Keyword(s):  
Liquid Chromatography ◽  
High Performance ◽  
Limit Of Detection ◽  
High Performance Liquid Chromatographic ◽  
Normal Phase ◽  
Limit Of Quantification ◽  
Chromatography Method ◽  
Phase Liquid ◽  
Bulk Drug

ABSTRACTObjective: The objective is defined to develop and validate simple, rapid, precise, and accurate for separation and determination of R-isomer impurityof ketoprofen bulk drug material by the normal phase high-performance liquid chromatographic method as per the International Conference ofHarmonization Guideline (ICH) guidelines.Methods: The R-isomer and S-isomer were baseline resolved on a Chiralcel OJ-H, 150 mm × 4.6 mm, and 5 µm stationary phase column. Mobile phasesystem containing n-hexane:isopropyl alcohol:glacial acetic acid (50:50:0.1 v/v.). The detector wavelength has been selected 254 nm and column oventemperature 25°C. The chromatographic resolutions between R-isomer and S-isomer were more than two. The developed method was extensivelyvalidated according to ICH guidelines.Results: Ketoprofen linearity was found for R-isomer over the concentration range of 600-6000 ng/ml, with the linear regression (Correlationcoefficient R=0.999) and proved to be robust. The limit of detection and limit of quantification of ketoprofen R-isomer were found to be 200 and600 ng/ml. The percentage recovery of R-isomer has been ranged from 97.5 to 102.0 in bulk drug material samples of ketoprofen. The proposedmethod was found to be suitable and accurate for the quantitative determination of R-isomer of ketoprofen in bulk drug sample.Conclusion: A simple, rapid, precise, and accurate normal phase liquid chromatography method has been developed and validated to determineR-isomer impurity of ketoprofen in bulk drugs material as per ICH.Keywords: Ketoprofen, High-performance liquid chromatography, Known impurity, Normal phase, Chiralcel OJ-H, Validation.

scholarly journals SEPARATION AND DETERMINATION OF THE R-ISOMER OF ETODOLAC IN A BULK DRUG SUBSTANCE BY NORMAL-PHASE LIQUID CHROMATOGRAPHY

2016 ◽  
Vol 9 (6) ◽  
pp. 327
Author(s):  
Appasaheb Bajirao Lawande
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Analytical Method ◽  
Mobile Phase ◽  
High Performance ◽  
Limit Of Detection ◽  
Normal Phase ◽  
Limit Of Quantification ◽  
Bulk Drug

ABSTRACT Objective:  The objective of the this work is to develop and validate a novel, simple,rapid and reliable analytical method for separation and determination of R-isomer impurity in Etodolac bulk drug material by normal-phase high-performance liquid chromatography as per International Conference on Harmonization guidelines. Methods: The Etodolac R- isomer and S-isomer were separated on a Chiralcel OD-H (150 x 4.0 mm, 5 micron) column by using Ethanol : n-Hexane:Trifluoroacetic acid (50:50:0.1 v/v.) mobile phase with equipped detector at wavelength 225 nm and 25 °C column oven temperature. The resolution between R-isomer and S-isomer were more than two recorded on chromatogram. The specified method was developed and validated for various parameters like reproducibility, limit of detection, limit of quantification, linearity and range, robustness, solution stability and mobile phase stability according to the International Conference on Harmonization (ICH) guidelines.  Results: Linearity were found for Etodolac R-isomer over the concentration range of 600–6000 ng/ml, with the linear regression (Correlation coefficient R = 0.998) and proved to be robust. Limit of detection and limit of quantification of Etodolac R-isomer was found to be 200 and 600 ng/ml. The retention time of R-isomer was considered to be 2.8 min. The percentage recovery of Etodolac R-isomer has been ranged from 97.0 to 102.0 in bulk drug material sample. The proposed analytical method has been found to be suitable, precise,reliable and accurate for the separation and quantitative determination of Etodolac R-isomer in bulk drug sample.                                                                                                                   Conclusion: A novel, speedy, accurate, precise, reliable and rugged analytical method has been developed and validated for normal phase high performance liquid chromatography to determine R-isomer impurity in Etodolac bulk drugs material as per ICH guideline. Keywords: Etodolac, HPLC, Known Impurity. Normal Phase, Validation.

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.

scholarly journals Extraction and Determination of Oxymatrine Pesticide in Environmental Sample and in its Formulation using High-Performance Liquid Chromatography

2020 ◽  
Vol 8 (2) ◽  
pp. 1-7
Author(s):  
Ihsan M. Shaheed ◽  
Saadiyah A. Dhahir
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Water Samples ◽  
High Performance ◽  
Limit Of Detection ◽  
Limit Of Quantification ◽  
Chromatography Method ◽  
Relative Standard ◽  
Dispersive Liquid Liquid Microextraction

The quinolizindine alkaloid compound, oxymatrine pesticide, was analysis in the river water samples collected from different agriculture areas in the Iraqi city of Kerbala and also in its formulation using developed reverse-phase high-performance liquid chromatography method. Acetonitrile:methanol (60:40 v/v) was chosen as mobile phase at pH (7.0), flow rate 0.5 mL/min, and 20 µL as volume injection. Modified ecological-friendly method, dispersive liquid-liquid microextraction, was used for the extraction of oxymatrine from water samples. Linearity study was constructed from 0.1 to 70 μg/mL at λmax 205 nm. The limit of detection and limit of quantification were 0.025 and 0.082 μg/mL, respectively, and the relative standard deviation (RSD) % was 0.518%. Three spiked levels of concentration (20.0, 40.0, and 70.0 μg/mL) were used for the validation method. The percentage recovery for the three spiked samples was ranged between 98.743 and 99.432 and the RSD% was between 0.051 and 0.202%, the formulation studies of oxymatrine between 99.487 and 99.798, and the RSD% was ranged from 0.045 to 0.057%. The developed method can be used accurately and selectively for the determination of oxymatrine in environmental samples and in the formulation.

scholarly journals EXTRACTION AND DETERMINATION OF TEBUCONAZOLE IN ENVIRONMENTAL SAMPLES FROM THE CITY OF KERBALA, IRAQ AND IN ITS FORMULATION USING HIGH- PERFORMANCE LIQUID CHROMATOGRAPHY (HPLC)

2020 ◽  
Vol 17 (34) ◽  
pp. 1046-1054
Author(s):  
Ihsan Mahdi SHAHEED ◽  
Saadiyah Ahmed DHAHIR
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Water Samples ◽  
High Performance ◽  
Limit Of Detection ◽  
Limit Of Quantification ◽  
Chromatography Method ◽  
Percentage Recovery ◽  
Relative Standard

The triazole, tebuconazole pesticide, was determined in its formulation and also in the river water samples collected from different agriculture areas in the Iraqui city of Kerbala using developed high-performance liquid chromatography method(HPLC) with UV-visible detection, The mobile composition phase was a mixture of acetonitrile:methanol (50:50 v/v) and the column was C18 (250 cm x 4.6 mm,5μm). Also modified dispersive liquidliquid microextraction (DLLME), which is regarded as an ecological -friendly method, was used for the extraction of tebuconazole from water samples using acetonitrile and chloroform as solvents extraction and dispersive agent, respectively. Linearity to maintain the calibration curve was achieved from (0.1-70) μg.mL-1 with a limit of detection(0.053) μg.mL-1 and limit of quantification (0.174) μg.mL-1. Three spiked levels of concentration (1.0, 5.0, and 10) μg.mL-1 were used for the validation of the method. The relative standard deviation (RSD%) was (0.294- 0.813)%, and the percentage recovery was (100.001-100.005). The formulation studies for two different concentrations (10 and 40) μg.mL-1, which prepared from tebuconazole formulation (Raxil ODS2 2%), gave acceptable percentage recovery between (98.956-99.833). The developed method can be used accurately for the determination of tebuconazole in water samples and in the formulation of tebuconazole effectively.

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 INULIN FROM MULTIVITAMIN SYRUP PRODUCT BY HIGH PERFORMANCE LIQUID CHROMATOGRAPHY WITH RI DETECTOR

2012 ◽  
Vol 12 (2) ◽  
pp. 201-205 ◽  
Author(s):  
Yuni Retnaningtyas
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Limit Of Detection ◽  
Regression Function ◽  
Hplc Method ◽  
Limit Of Quantification ◽  
Chromatography Method ◽  
Label Claim

At present, inulin is often added to multivitamin syrup product. The determination of the component of preparation both qualitatively and quantitatively is important to ensure quality of the product. This research is aimed to develop a high performance liquid chromatography method to analyze inulin in multivitamin syrup preparation. Separation of inulin from the sample, was performed using Aminex column HPX-87H (300 x 7.8 mm) Ion Exclusion at a temperature of 80 °C with isocratic elution system using deionized water as mobile phase at a flow rate of 0.5 mL/min, and detected by using refractive index detector. This method validation showed a good linearity with correlation coefficient (r) of 0.999 while the coefficient of variation of the regression function (Vx0) was 2.00%. The limit of detection (LOD) and the limit of quantification (LOQ) of the method were respectively 0.12 mg/mL and 0.37 mg/mL. The mean absolute recovery of inulin from the simulation sample was 99.42% and the method precision was less than 2%. The proposed method has been applied to the determination of inulin in commercial multivitamin syrup and the recovery of label claim was 99.9 mg/100 mL. The proposed HPLC method is rapid, simple, and selective for routine analysis.

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>

scholarly journals Oxytetracycline Residues in Honey Analyzed by Liquid Chromatography with UV Detection

2013 ◽  
Vol 57 (1) ◽  
pp. 25-32 ◽  
Author(s):  
Anna Gajda ◽  
Andrzej Posyniak ◽  
Andrzej Bober ◽  
Tomasz Błądek ◽  
Jan Żmudzki
Keyword(s):  
Liquid Chromatography ◽  
Oxalic Acid ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Experimental Treatment ◽  
Uv Detection ◽  
Limit Of Quantification ◽  
Chromatography Method ◽  
Liquid Chromatography Method

Summary A liquid chromatography method with UV detection for determination of oxytetracycline (OTC) in honey has been developed. The samples were extracted with the solution of oxalic acid. The clean-up procedure was performed by solid phase extraction (SPE) using polymeric Strata X and carboxylic acid cartridges. Chromatographic separation was carried out on the Luna C8 analytical column with mobile phase consisting of acetonitrile-0.02 M oxalic acid. The method has been successfully validated according to the requirements of the European Decision 2002/657/EC and this method is used in routine control of oxytetracycline in honey samples. The limit of detection (LOD) and limit of quantification (LOQ) of the presented method were 10 and 12.5 μg/kg, respectively. The developed method has also been verified in quantitative determination of oxytetracycline residues in honey after experimental treatment with this product in bee colonies.

scholarly journals DEVELOPMENT AND VALIDATION OF STABILITY INDICATING HPTLC METHOD FOR DETERMINATION OF APIXABAN AS BULK DRUG

2019 ◽  
pp. 37-42
Author(s):  
Mrinalini C. Damle ◽  
Swapnil S Waghmare ◽  
PURUSHOTAM SINHA
Keyword(s):  
Thin Layer ◽  
High Performance ◽  
Limit Of Detection ◽  
Chromatography Method ◽  
Stability Indicating ◽  
Chromatographic Condition ◽  
Bulk Drug ◽  
Development And Validation ◽  
Hptlc Method

Objective: To develop and validate simple, sensitive stability indicating HPTLC (High performance thin layer chromatography) method for apixaban. Methods: The chromatographic separation was performed on aluminium plates precoated with silica gel 60 F254 using toluene: ethyl acetate: methanol (3:6:1 v/v/v) as mobile phase followed by densitometric scanning at 279 nm. Results: The chromatographic condition shows sharp peak of apixaban at Rf value of 0.38±0.03. Stress testing was carried out according to international conference on harmonization (ICH)Q1A (R2) guidelines and the method was validated as per ICH Q2(R1) guidelines. The calibration curve was found to be linear in the concentration range of 100-500 ng/band for apixaban. The limit of detection and quantification was found to be 11.66ng/bandand35.33ng/band, respectively. Conclusion: A new simple, sensitive, stability indicating high performance thin layer chromatographic (HPTLC) method has been developed and validated for the determination of apixaban.

Determination of Mimosine and 2,3-Dihydroxypyridine in Leucaena leucocephala by Reversed Phase High-Performance Liquid Chromatography

2011 ◽  
Vol 140 ◽  
pp. 296-301 ◽  
Author(s):  
Cai Mei Wu ◽  
Hong Min Yuan ◽  
Gang Jia ◽  
Zhi Sheng Wang ◽  
Xiu Qun Wu
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Leucaena Leucocephala ◽  
High Performance ◽  
Limit Of Detection ◽  
Reversed Phase ◽  
Quantitative Detection ◽  
Uv Detector ◽  
Chromatography Method

A reversed high performance liquid chromatography method was developed for the quantitative determination of mimosine and 2,3-DHP in leaves ofLeucaena Leucocephala. Mimosine and 2,3DHP were extracted using 0.1N HCl.The chromatograph conditions were investigated and optimized. The optimal HPLC conditions as follows: Agilent HC-C18 column （4.6×150mm,5μm） was used at 30°C. The method used a variable wavelength UV detector at 280nm, the mobile phase consisted of 0.2 % (w/v) orthophosphoric acid and methanol, the gradient elution was adopted. The injection volume was 10μL. The linearity is favorable in the range of 1.0 to 50μg mL-1with a correlation coefficient of 0.99998 for mimosine and 0.99902 for 2,3DHP. Under the optimal conditions, the method limit of detection (LOD) of mimosine and 2,3DHP were 0.40mg/kg and 0.55mg/kg respectively. The recovery of mimosine was 87.00-94.70% with the RSD (n=5) of 2.75-3.81% in the spiked levels 0,1, 5, 20mg/g. At the same time, the recovery of 2,3DHP was 88-95.4% with the RSD (n=5) of 2.24-4.90%. The method was found to be simple, sensitive, fast and accurate, and has been applied successfully for the quantitative detection of mimosine and 2,3-DHP in leaves ofLeucaena Leucocephala, plasma and excretion of ruminant.

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