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.

scholarly journals A microemulsion high-performance liquid chromatography (MELC) method for the separation and determination of hydrolyzed tenuifolin in Radix Polygalae

2019 ◽  
Vol 9 (1) ◽  
Author(s):  
Hui Yan ◽  
Zhuan-Di Zheng ◽  
Hong-Fei Wu ◽  
Xiao-Chuang Liu ◽  
An Zhou
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Mobile Phase ◽  
High Performance ◽  
Limit Of Detection ◽  
Sodium Dodecyl ◽  
Limit Of Quantification ◽  
Analyte Molecule ◽  
Oil In Water

AbstractTenuifolin was used as a reliable chemical marker for the quality control of Radix Polygalae. The determination of tenuifolin is challenging because the analyte molecule lacks a suitable chromophore. The aim of this study was to establish a microemulsion high-performance liquid chromatography (MELC) method which is robust and sensitive, and can separate and determine tenuifolin in Radix Polygalae using an oil-in-water (O/W) microemulsion mobile phase. The separations were performed on a C18 (4.6 × 250 mm, 5 μm) column at 25 °C using a flow rate of 1.0 mL/min, and an ultraviolet detection wavelength of 210 nm. The microemulsion mobile phase comprised 2.8% (w/v) sodium dodecyl sulfate (SDS), 7.0% (v/v) n-butanol, 0.8% (v/v) n-octane and 0.1% (v/v) aqueous orthophosphate buffer (H3PO4). The linearity analysis of tenuifolin showed a correlation coefficient of 0.9923 in the concentration range of 48.00–960.00 µg/mL. The accuracy of the method based on three concentration levels ranged from 96.23% to 99.28%; the limit of detection (LOD) was 2.34 µg/mL, and the limit of quantification (LOQ) was 6.76 µg/mL. The results of our study indicated that the optimized MELC method was sensitive and robust, and can be widely applied for the separation and determination of tenuifolin in Radix Polygalae.

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 HPLC Determination of Formaldehyde in Flour Samples using 2,4,6-Trichlorophenyl Hydrazine as Derivatization Reagent

2021 ◽  
Vol 33 (4) ◽  
pp. 930-936
Author(s):  
Khaldun M. Al Azzam ◽  
Ahmad Makahleh ◽  
Bahruddin Saad
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Mobile Phase ◽  
High Performance ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Limit Of Quantification ◽  
Injection Volume ◽  
Concentration Levels

A new simple and sensitive high-performance liquid chromatography (HPLC) method for the determination of formaldehyde in flour samples has been developed. Formaldehyde was quantified after derivatization with a readily available reagent, 2,4,6-trichlorophenyl hydrazine (TCPH) under basic conditions. The formaldehyde-TCPH derivative was eluted with chromatographic mobile phase of 70:30 (v/v) acetonitrile:water at a flow rate of 1.0 mL min–1; wavelength, 222 nm; injection volume, 50 μL, using a C18 ODS Hypersil column (250 mm × 4.5 mm, 5 μm). The calibration curve was linear over the range of 0.001-10 μg mL-1 with R2 = 0.999. Recoveries at three different concentration levels (0.1, 1.0 and 5 μg mL-1) ranged from 92.0-101.7% with RSD less than of 2.2%. The limit of detection (LOD) and limit of quantification (LOQ) were 0.3 and 1.0 ng mL-1, respectively. The developed method was used for the determination of formaldehyde in various flour-based samples.

scholarly journals Development and validation of reversed phase high performance liquid chromatography (RP-HPLC) for quantification of captopril in rabbit plasma

2020 ◽  
Author(s):  
Muhammad Fawad Rasool ◽  
Umbreen Fatima Qureshi ◽  
Nazar Muhammad Ranjha ◽  
Imran Imran ◽  
Mouqadus Un Nisa ◽  
...  
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Mobile Phase ◽  
High Performance ◽  
Limit Of Detection ◽  
Reversed Phase ◽  
Rabbit Plasma ◽  
Rp Hplc ◽  
Relative Standard

AbstractTh accurate rapid, simple and selective reversed phase high performance liquid chromatography (RP-HPLC) has been established and validated for the determination of captopril (CAP). Chromatographic separation was accomplished using prepacked ODSI C18 column (250 mm × 4.6 mm with 5 μm particle size) in isocratic mode, with mobile phase consisting of water: acetonitrile (60:40 v/v), pH adjusted to 2.5 by using 85% orthophosphoric acid at a flow rate of 1 mL/min and UV detection was performed at 203 nm. RP-HPLC method used for the analysis of CAP in mobile phase and rabbit plasma was established and validated as per ICH-guidelines. It was carried out on a well-defined chromatographic peak of CAP was established with a retention time of 4.9 min and tailing factor of 1.871. The liquid–liquid extraction method was used for extraction of CAP from the plasma. Excellent linearity (R2 = 0.999) was shown over range 3.125–100 µg/mL with mean percentage recoveries ranges from 97 to 100.6%. Parameters of precision and accuracy of the developed method meet the established criteria. Intra and inter-day precision (% relative standard deviation) study was also performed which was less than 2% which indicate good reproducibility of the method. The limit of detection (LOD) and quantification for the CAP in plasma were 3.10 and 9.13 ng/mL respectively. The method was suitably validated and successfully applied to the determination of CAP in rabbit plasma samples.

scholarly journals HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY ANALYTICAL METHOD VALIDATION FOR GLUTARALDEHYDE AND BENZALKONIUM CHLORIDE IN DISINFECTANTS

2018 ◽  
Vol 10 (1) ◽  
pp. 248
Author(s):  
Baitha Palanggatan Maggadani ◽  
Harmita . ◽  
Maizura Isfadhila
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Analytical Method ◽  
Benzalkonium Chloride ◽  
Mobile Phase ◽  
High Performance ◽  
Limit Of Detection ◽  
Analytical Method Validation ◽  
Limit Of Quantitation ◽  
Uv Visible

Objective: The aim of this study was to produce a selective, accurate, and faster high-performance liquid chromatography (HPLC) analytical methodfor benzalkonium chloride and glutaraldehyde in disinfectants using ultraviolet (UV)-visible detection.Methods: Glutaraldehyde has no chromophore, so it was first derivatized using 2,4 dinitro phenylhydrazine. Acetonitrile:water (75:25) was used asthe mobile phase for glutaraldehyde and acetonitrile-acetate pH 4 (75:25) for benzalkonium chloride, both at a flow rate of 1.2 mL/min. The optimizedassay was validated with respect to accuracy, precision, linearity, selectivity, limit of quantitation (LOQ), and limit of detection (LOD).Results: The method was linear for benzalkonium chloride, with correlation coefficient of 0.9995, LOD of 14.55 ppm, and LOQ of 48.51 ppm. Thecorrelation coefficient for glutaraldehyde was 0.9995, with LOD of 0.49 ppm and LOQ of 1.64 ppm. Accuracy was between 98% and 102%, andprecision was below 2% for both the tests.Conclusion: The HPLC analytical method for benzalkonium chloride and glutaraldehyde in disinfectants using UV-visible detection in this researchwas successful to produce a selective, accurate, and faster method.

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 SIMULTANEOUS DETERMINATION OF PARACETAMOL AND IBUPROFENE MIXTURES BY HIGH PERFORMANCE LIQUID CHROMATOGRAPHY

2010 ◽  
Vol 3 (1) ◽  
pp. 9-13 ◽  
Author(s):  
Sophi Damayanti ◽  
Slamet Ibrahim ◽  
Kurnia Firman ◽  
Daryono H Tjahjono
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Standard Deviation ◽  
Retention Time ◽  
Analytical Method ◽  
Phosphate Buffer ◽  
Mobile Phase ◽  
High Performance ◽  
Relative Standard

Analytical method for the determination of paracetamol and ibuprofene mixtures has been developed by High Performance Liquid Chromatography using C-18 column and acetinitrile - phosphate buffer pH = 4.5 (75:25) containing 0.075% sodium hexanesulfunate as a mobile phase. The detector was set at 215 nm. Using such conditions, retention time for paracetamol and ibuprofen was 4.89 and 7.11 min, respectively. The recovery for paracetamol and ibuprofen was found to be 101.07± 0.73% and 102.02 ± 1.58%, respectively. The detector limits of the method was 1.30 and 1.60 μg/mL with the relative standard deviation (RSD) 0.74 and 1.52% for paracetamol and ibuprofen, respectively.   Keywords: paracetamol, ibuprofen, multi-component, validation, HPLC.

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.

Determination of Chloramphenicol Residual in Freshwater Fish by HPLC

2013 ◽  
Vol 781-784 ◽  
pp. 1708-1711 ◽  
Author(s):  
Yi Qing Yang ◽  
Qian Wang ◽  
Qiao Wang ◽  
Shi Jie Yan
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Freshwater Fish ◽  
Mobile Phase ◽  
High Performance ◽  
Limit Of Detection ◽  
Chromatography Method ◽  
Average Recovery ◽  
Liquid Chromatography Method

HPLC (High Performance Liquid Chromatography) method for chloramphenicol residues in freshwater fish was developed. The samples were extracted with ethyl acetate. The LC was performed on a C18 column, mobile phase consisted of methanol-water (45:55 v/v) and eluted at 0.2mL/min at 20°C, inject volume was 20μl. The linear rang for chloramphenicol residual is within 0.5-20μg/mL, the limit of detection is 0.01ng/g. The average recovery is 80.06%-92.71%, and the RSD is 1.46%-5.61%. This method is employed to analyze freshwater fishes, such as catfish, chub and carp.

scholarly journals Determination of Indoxacarb Enantiomer Residues in Vegetables, Fruits, and Soil by High-Performance Liquid Chromatography

2010 ◽  
Vol 93 (3) ◽  
pp. 1007-1012 ◽  
Author(s):  
Li Cheng ◽  
Feng-Shou Dong ◽  
Xingang Liu ◽  
Wuying Chen ◽  
Yuanbo Li ◽  
...  
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Analytical Method ◽  
Complete Resolution ◽  
Mobile Phase ◽  
High Performance ◽  
Soil Samples ◽  
Agricultural Products

Abstract An effective chiral analytical method was developed for the resolution and determination of indoxacarb enantiomers in cucumber, tomato, apple, pear, and soil samples. Indoxacarb enantiomers were separated on a Chiralpak AS-H column with n-hexaneethanol (95 + 5, v/v) as the mobile phase. Validation involved complete resolution of each enantiomer, plus determination of linearity, precision, LOD, and LOQ. The estimated LOD was 0.0250.035 mg/kg, and the LOQ was 0.05 mg/kg for each indoxacarb enantiomer in different matrixes. The average recoveries of the pesticide from all matrixes ranged from 87.0 to 116.9 for fortification levels of 0.05, 0.1, and 5 mg/kg. The precision values associated with the analytical method, expressed as RSDr values, were <10.1 for the pesticide in all matrixes. This method can be used to evaluate environmental residues and the safety of agricultural products.

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