scholarly journals VALIDATED STABILITY-INDICATING HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY METHOD FOR THE ESTIMATION OF TORSEMIDE

Author(s):  
LALITHA KV ◽  
RAVEENDRA REDDY J ◽  
DEVANNA N

Objective: This assessment depicts the strength of exhibiting reverse-phase high performance liquid chromatography (RP-HPLC) method for the estimation of torsemide in pharmaceutical estimation structures. Methods: In the present work, total protein-HPLC technique has been produced for the estimation of torsemide active pharmaceutical ingredient (API). Constrained degradation HPLC strategy was created with versatile mobile phase of methanol:water in the proportion of 90:10 v/v. The stream pace of 1 ml/min was utilized on Inertsil ODS 3V segment (250 mm×4.6 mm, 5 μm molecule size). Results: The retention time of torsemide was seen at 8.267 min, method was validated for all validation parameters as per the International Council for Harmonization guidelines. The linearity range was 10–60 μg/ml, correlation coefficient was 0.9993, and percentage relative standard deviation in the precision studies was <2%, with percentage recovery 100.56–101.03 (within acceptable range of 98–102%). The assay result was found to be 100.88% (i.e., within 95–105%), passes the specifications for robustness parameters. Limit of detection of torsemide was found to be 0.0162 μg/ml and limit of quantitation of torsemide was found to be 0.0534 μg/ml. Conclusion: The medication was exceptionally delicate to antacid pursued by at risk to corrosive, photolytic, warm, and oxidative conditions. The created and approved method showing HPLC technique is observed to be direct, exact, precise, explicit, and powerful. Henceforth, the technique can be utilized routinely for the estimation of torsemide API.

2010 ◽  
Vol 7 (3) ◽  
pp. 962-966 ◽  
Author(s):  
Naveen Kumar ◽  
Nishant Verma ◽  
Omveer Songh ◽  
Naveen Joshi ◽  
Kanwar Gaurav Singh

A simple, precise, sensitive, fast and accurate high performance liquid chromatography method has been developed for the determination of atenolol using mixture of phosphate buffer and acetonitrile (53:47 v/v) as mobile phase. Buffer was prepared by mixing 0.02 M K2PO4and 0.003 M KH2PO4in equal proportion. Detection was carried out using UV detector at λmax230 nm. Column was ODS and dimensions of column was 25 mm × 4.6 mm. Atenolol was eluted out at retention time of 2.1 min. Method was validated at 1.2 mL/min flow rate. Calibration curve was linear between ranges of 40 to 200 mcg concentration. The limit of detection was calculates 120 nano gram and limit of quantitation is 510 nano gram. The relative standard deviation (RSD) of atenolol was 0.6. The percentage recovery of atenolol was 99.6%.


2014 ◽  
Vol 68 (7) ◽  
Author(s):  
Joanna Ronowicz ◽  
Bogumiła Kupcewicz ◽  
Łukasz Pałkowski ◽  
Piotr Bilski ◽  
Tomasz Siódmiak ◽  
...  

AbstractThe aim of the study was to design and validate a reversed phase high performance liquid chromatography method for the separation and quantification of two active pharmaceutical ingredients (ciprofloxacin hydrochloride, hydrocortisone) and a preservative (benzyl alcohol) in ear drops. Effective separation of the examined compounds was achieved on a GraceSmart™ RP 18 column (150 mm × 4.6 mm, 5 μm) with gradient elution and a diode array detector. The total assay run time was 25 min. Analytical method validation assays were performed. Validation parameters used for the evaluation were: specificity, linearity, trueness, precision (repeatability and reproducibility), limit of detection and limit of quantitation. Results of the validation procedure (high recoveries, good standard deviations, no interfering peaks at the retention times corresponding to the analytes) confirm that the developed chromatographic method can be applied for routine analysis of ear drops.


2017 ◽  
Vol 2017 ◽  
pp. 1-7
Author(s):  
Paula Karina S. Uchoa ◽  
Leandro Bezerra de Lima ◽  
Antonia T. A. Pimenta ◽  
Maria da Conceição F. de Oliveira ◽  
Jair Mafezoli ◽  
...  

A high-performance liquid chromatography method was developed and validated for the quantification of the cytotoxic compounds produced by a marine strain ofAspergillus niger. The fungus was grown in malt peptone dextrose (MPD), potato dextrose yeast (PDY), and mannitol peptone yeast (MnPY) media during 7, 14, 21, and 28 days, and the natural products were identified by standard compounds. The validation parameters obtained were selectivity, linearity (coefficient of correlation > 0.99), precision (relative standard deviation below 5%), and accuracy (recovery > 96).


2020 ◽  
Vol 11 (02) ◽  
pp. 219-223
Author(s):  
Ansari Yaasir Ahmed ◽  
Qazi Shoeb ◽  
Umme Rumana ◽  
Patel Afroza ◽  
Pathan Vahid Tajkhan ◽  
...  

The new stability-indicating high performance liquid chromatography (HPLC) method has been developed and validated with different parameters for atenolol (ATE) and nifedipine (NIFE) in the combined dosage form. The chromatographic conditions were optimized using a mobile phase of MeOH:OPA (70:30) with a flow rate of 0.7 mL/min. Column (C18) of 4.6 × 250 mm dimension was used as a stationary phase; the particle size capacity of the column was 5 μm. The detection was carried out at 233 nm. The method was validated according to ICH guidelines for linearity, precision, repeatability, the limit of detection (LoD), and limit of quantitation (LoQ). The response was found to be linear in the concentration range of 20 to 100 mcg/mL for ATE and 1 to 5 mcg/mL for NIFE. The developed method shows the minimum quantity of drugs to be identified (LoD) and minimum drug to be quantified (LoQ). The LoD and LoQ were found to be 0.1415 and 0.4289, respectively, for ATE, and 0.1834 and 0.5558, respectively, for NIFE. The method was linear, simple, precise, and accurate and, therefore, suitable for routine analysis of drugs in tablet form. The forced degradation studies were also done through the exposure of analyte solution to four different stress conditions.


Author(s):  
MUCHTARIDI MUCHTARIDI ◽  
IDA MUSFIROH ◽  
AHMAD FAUZI

Objective: The aim of this study is to develop a simple, precise and accurate analytical method of deoxyarbutin in anhydrous emulsion system preparation. Methods: The analysis was conducted using high-performance liquid chromatography (HPLC). Chromatographic analysis was carried out using a reversed phase-C18 column. The mobile consists of two phases methanol and water (60: 40 v/v) at a flow rate of 1.0 ml/min. The determinations were performed using UV detector set at 225 nm. All validation procedures were added with hydroquinone as an internal standard. Results: The method showed coefficient correlation is 0.9978, relative standard deviation (RSD) smaller than 2%, Limit of Detection (LOD) and Limit of Quantitation (LOQ) are 0.599 µg/ml and 1.817 µg/ml respectively. The total amount deoxyarbutin in anhydrous emulsion preparation is 1.964+0.02 % with 98% recovery percentage. Conclusion: The developed HPLC analytical method meets the validation criteria made by International Conference on Harmonisation (ICH).


2018 ◽  
Vol 10 (1) ◽  
pp. 403
Author(s):  
Baitha Palanggatan Maggadani ◽  
Harmita . ◽  
Milza Lubnan

Objective: This study aimed to validate an high-performance liquid chromatography method for analyzing undenatured Type II collagen preparationsusing a fluorescence detector.Methods: Based on the optimum analysis conditions, the compound was detected at an excitation wavelength of 255 nm and an emission wavelengthof 320 nm. The optimum mobile phase was determined to be acetate (pH 4.2) and acetonitrile (60:40) with a flow rate of 1.0 ml/min. Hydroxyprolineis a compound that does not have chromophore moiety; thus, it has to be derivatized first using 9-fluorenylmetoxycarbonyl-chloride.Results: The developed method was validated with linearity and an equation of y=3,249,704 x+141,945,072, with a value of r=0.9994. The detectedrange of hydroxyproline was 4–15 ppm. The limit of detection was determined to be 0.49, with an limit of quantitation of 1.64.Conclusion: Our results indicated that the average level of hydroxyproline was 98.66%, 99.12%, and 99.85%.


2020 ◽  
Vol 8 (2) ◽  
pp. 1-7
Author(s):  
Ihsan M. Shaheed ◽  
Saadiyah A. Dhahir

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.


2021 ◽  
Vol 5 (4) ◽  
pp. 353-358
Author(s):  
Wiwin Winingsih ◽  
Sri Gustini Husein ◽  
Rozalia Putri Neno Ramdhani

Ethyl para-methoxycinamate (EPMS) is a major compound of Kaempferia galanga L that has anti-inflammatory effect.  The purpose of this study was to determine of EPMS in Kaempferiae galanga L rhizome extract by  High Performance Liquid Chromatography (HPLC) and evaluated the performance of the analysis. This study included determination of system suitability, accuracy, precision, linearity and range, limit of detection (LOD) and Limit of quantitation (LOQ) and selectivity.  The results of system suitability test  HPLC System for EPMS analysis were as follows isocratic elution system of a mobile phase mixture of methanol: water (70:30) containing 0.1% TFA, uv detector at a wavelength of 308 nm using column C18 (150 × 4, 6mm, 5μm) flow rate 1 ml / min. From the analysis, it was found that the average EPMS content was 78.74%. Then method had linear concentration range from 5-360 ppm, with R ² = 0.9999. The LOD and LOQ were 7.0722 ppm and 21.4311 ppm respectively. The accuracy of this method that represented by % recovery was 98.02% - 101.26%. The precision of this method that expressed by Relative Standard Deviation (RSD) was 1.57%. The selectivity of this method that showed by  resolution value was 2.6. Based on the results of the system suitability test and analysis performance evaluation,all parameters met the requirements.


2018 ◽  
Vol 2018 ◽  
pp. 1-8 ◽  
Author(s):  
Sasiprapa Choochuay ◽  
Jutamas Phakam ◽  
Prakorn Jala ◽  
Thanapoom Maneeboon ◽  
Natthasit Tansakul

A reliable and rapid method has been developed for the determination of aflatoxin B1 (AFB1) in four kinds of feedstuffs comprising broken rice, peanuts, corn, and fishmeal. A sample preparation was carried out based on the QuEChERS method with the exclusion of the clean-up step. In this study, AFB1 was extracted using acetonitrile/methanol (40/60 v/v), followed by partitioning with sodium chloride and magnesium sulfate. High-performance liquid chromatography with precolumn derivatization and fluorescence detection was performed. The coefficients of determination were greater than 0.9800. Throughout the developed method, the recovery of all feedstuffs achieved a range of 82.50-109.85% with relative standard deviation lower than 11% for all analytes at a concentration of 20-100 ng/g. The limit of detection (LOD) ranged from 0.2 to 1.2 ng/g and limit of quantitation (LOQ) ranged from 0.3 to 1.5 ng/g. The validated method was successfully applied to a total of 120 samples. The occurrence of AFB1 contamination was found at the following concentrations: in broken rice (0.44-2.33ng/g), peanut (3.97-106.26ng/g), corn (0.88-50.29 ng/g), and fishmeal (1.06-10.35 ng/g). These results indicate that the proposed method may be useful for regularly monitoring AFB1 contamination in feedstuffs.


2020 ◽  
Vol 17 (34) ◽  
pp. 1046-1054
Author(s):  
Ihsan Mahdi SHAHEED ◽  
Saadiyah Ahmed DHAHIR

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.


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