scholarly journals CONTENT VARIATIONS OF CARBAMAZEPINE TABLETS IN IRAQI COMMUNITY PHARMACIES: APPLICATION OF HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY ASSAY METHOD

2018 ◽  
Vol 11 (2) ◽  
pp. 117
Author(s):  
Mohanad Naji Sahib
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Limit Of Detection ◽  
High Standard ◽  
Assay Method ◽  
Solution Stability ◽  
Limit Of Quantification ◽  
Rp Hplc ◽  
Middle East Countries

 Objective: There is paucity in the literature and documentation regarding the post-marketing product quality in Iraq and Middle East countries in general. Therefore, a simple reverse phase high-performance liquid chromatography (RP-HPLC) method was developed and validated for the determination of carbamazepine (CMZ) content in post-marketed tablet dosage form.Methods: The RP-HPLC analysis was run at a flow rate of 1 ml/min with a mixture of methanol: water (70:30) mobile phase using a Thermo Synchronise C18 column at a UV detection wavelength of 230 nm. The method was validated for selectivity, linearity, precision, accuracy, limit of detection (LOD), limit of quantification (LOQ), solution stability, and robustness.Results: The calibration curve was linear over a concentration range of 1–20 μg/ml (r2=0.9999) with LOD and LOQ of 0.01 and 0.04 μg/ml, respectively. The intraday and interday precision and accuracy were between 0.04–1.67% and 0.04–0.78%, respectively. The results of analysis of the four brands of CMZ tablets were passed the European Pharmacopoeia specification but with a high standard deviation of mean drug content of some brands.Conclusion: This study shows that the quality of post-marketed drugs and/or the storage conditions in developing countries must be carefully assessed for a better therapeutic response.

scholarly journals A NEW VALIDATED SIMULTANEOUS REVERSED-PHASE HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY ASSAY METHOD FOR ESTIMATION OF TWO FLAVONES (BAICALEIN AND CHRYSIN) IN API DRUGS

2018 ◽  
Vol 11 (1) ◽  
pp. 351
Author(s):  
Maddi Sesharao ◽  
Vallabaneni Madhavarao
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Reversed Phase ◽  
Assay Method ◽  
Array Detector ◽  
Solution Stability ◽  
Rp Hplc ◽  
System Suitability ◽  
Relative Standard

  Objective: The scope of the present work is a reversed-phase high-performance liquid chromatography (RP-HPLC) assay method developed for the simultaneous determination of baicalein and Chrysin in API drugs.Methods: The RP-HPLC method employed a Hypersil BDS C18 reversed-phase column (150×4.6 mm×5.0 μm) with an isocratic mixture of water and acetonitrile in the ratio of 55:45; v/v as the mobile phase. The column temperature was kept at 25°C. The flow rate was 1.0 mL/min, and detection was by means of a photodiode array detector at wavelength of 268 nm and validated for various parameters such as specificity, system suitability, method precision, linearity, accuracy, solution stability, ruggedness, and robustness.Results: The system suitability parameters were evaluated from standard chromatograms by calculating the % relative standard deviation (RSD) from six replicate injections for baicalein and Chrysin peak areas. The % RSD for the peak area of the principal peak from six replicate injections of each standard solution was <2.0%. The linearity and correlation coefficient of baicalein and Chrysin was found to be 0.999. Method precision was performed, and % RSD from six different preparations for baicalein and Chrysin were found to be <2.0. The % recovery for each level was found to be the range of 98.0–102%. In ruggedness and robustness, the % RSD of the peak area of all peaks for six replicate injections should be not more than 2.0.Conclusion: Hence, the chromatographic assay method developed for baicalein and chrysin is said to be rapid, simple, specific, sensitive, precise, accurate, and reliable that can be effectively applied for routine analysis in research institutions, quality control department in industries, approved testing laboratories, bio-pharmaceutics, and bio-equivalence studies and in clinical pharmacokinetic studies.

Maceration-Mediated Liquid–Liquid Extraction and Reverse-Phase High-Performance Liquid Chromatography-Based Pragmatic Analysis of Silybins

2020 ◽  
Vol 58 (8) ◽  
pp. 779-787
Author(s):  
Syeda Mariam Hasany ◽  
Rahila Huma ◽  
Sumia Akram ◽  
Rizwan Ashraf ◽  
Muhammad Mushtaq
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Limit Of Detection ◽  
Curcuma Longa ◽  
Liquid Extraction ◽  
Reverse Phase ◽  
Limit Of Quantification ◽  
Liquid Liquid Extraction ◽  
Rp Hplc

Abstract This study presents a pragmatic and easily scalable maceration-mediated liquid–liquid extraction (MMLLE) and reverse-phase high-performance liquid chromatography (RP-HPLC)-based determination of Silybins from plant material (Curcuma longa L.). The processing of calibration standards revealed that the RP-HPLC method was linear over a concentration range of 1–100 μg/mL with regression coefficient (R2) &gt; 0.9950, limit of detection 0.02 μg/mL and limit of quantification &lt;0.07 μg/mL. The optimum chromatographic conditions resolved Silybin A, Silybin B, Isosilybin A and Isosilybin B within 5 min of analysis time. The reproducible recovery rates of spiked flavonolignans (96.24–115.40%) from quality controls established the effectiveness of MMLLE procedure prior to HPLC determination. The real-time analysis revealed the presence of silybins in C. longa roots. The results further endorse that MMLLE prior to chromatographic determination may provide a more pragmatic analytical solution for the analysis/isolation of silybins.

scholarly journals A NEW VALIDATED SIMULTANEOUS REVERSED-PHASE HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY ASSAY METHOD FOR ESTIMATION OF TWO FLAVONES (BAICALEIN AND CHRYSIN) IN API DRUGS

2018 ◽  
Vol 11 (1) ◽  
pp. 351
Author(s):  
Maddi Sesharao ◽  
Vallabaneni Madhavarao
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Reversed Phase ◽  
Assay Method ◽  
Array Detector ◽  
Solution Stability ◽  
Rp Hplc ◽  
System Suitability ◽  
Relative Standard

  Objective: The scope of the present work is a reversed-phase high-performance liquid chromatography (RP-HPLC) assay method developed for the simultaneous determination of baicalein and Chrysin in API drugs.Methods: The RP-HPLC method employed a Hypersil BDS C18 reversed-phase column (150×4.6 mm×5.0 μm) with an isocratic mixture of water and acetonitrile in the ratio of 55:45; v/v as the mobile phase. The column temperature was kept at 25°C. The flow rate was 1.0 mL/min, and detection was by means of a photodiode array detector at wavelength of 268 nm and validated for various parameters such as specificity, system suitability, method precision, linearity, accuracy, solution stability, ruggedness, and robustness.Results: The system suitability parameters were evaluated from standard chromatograms by calculating the % relative standard deviation (RSD) from six replicate injections for baicalein and Chrysin peak areas. The % RSD for the peak area of the principal peak from six replicate injections of each standard solution was <2.0%. The linearity and correlation coefficient of baicalein and Chrysin was found to be 0.999. Method precision was performed, and % RSD from six different preparations for baicalein and Chrysin were found to be <2.0. The % recovery for each level was found to be the range of 98.0–102%. In ruggedness and robustness, the % RSD of the peak area of all peaks for six replicate injections should be not more than 2.0.Conclusion: Hence, the chromatographic assay method developed for baicalein and chrysin is said to be rapid, simple, specific, sensitive, precise, accurate, and reliable that can be effectively applied for routine analysis in research institutions, quality control department in industries, approved testing laboratories, bio-pharmaceutics, and bio-equivalence studies and in clinical pharmacokinetic studies.

High performance liquid chromatography (HPLC) method development and validation for the determination of flunixin: Animal plasma based study

2021 ◽  
pp. 1-11
Author(s):  
Sultan M. Alshahrani ◽  
John Mark Christensen
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Method Development ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Limit Of Quantification ◽  
Mobile Phases ◽  
Hplc Method Development ◽  
Development And Validation

This study was designed to develop and validate a simple and efficient high performance liquid chromatography (HPLC) method to determine flunixin concentrations in Asian elephant’s (Elephas maximus) plasma. Flunixin was administered orally at a dose of 0.8 mg/kg, and blood samples were collected. Flunixin extraction was performed by adding an equal amount of acetonitrile to plasma and centrifuging at 4500 rpm for 25 minutes. The supernatant was removed, and flunixin was analyzed using HPLC-UV detection. Two methods were developed and tested utilizing two different mobile phases either with or without adding methanol (ACN: H2O vs. ACN: H2O: MeOH). Both methods showed excellent linearity and reproducibility. The limit of detection was 0.05 ug/ml and limit of quantification was 0.1 ug/ml. the efficiency of flunixin recovery was maximized by the addition of methanol to mobile phase (ACN: H2O: MeOH as 50:30:20) at 95% in comparison to 23% without methanol. In conclusion, adding methanol to HPLC methods for extraction of flunixin from elephants’ plasma yielded higher recovery rate than without methanol.

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 ESTIMATION OF GUGGULSTERONE-Z IN GOKSHURADI GUGGULU USING REVERSED-PHASE HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY

2018 ◽  
Vol 11 (11) ◽  
pp. 204
Author(s):  
Kanan G Gamit ◽  
Niraj Y Vyas ◽  
Nishit D Patel ◽  
Manan A Raval
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Limit Of Detection ◽  
Reversed Phase ◽  
Array Detector ◽  
Limit Of Quantification ◽  
Photodiode Array Detector ◽  
Validation Parameters ◽  
Photodiode Array

Objective: A study was aimed to estimate guggulsterone-Z (GZ) in Gokshuradi Guggulu (GG).Methods: An analytical method was developed and validated using Waters Alliance high-performance liquid chromatography system (Empower software), equipped with photodiode array detector. Separation was achieved using Phenomenex, C-18 (250 mm×4.6 mm, 5 μ) column. Mobile phase consisted of acetonitrile:water (70:30,v/v). Flow rate was set to 1 ml/min and detection was performed at 251 nm.Results and Discussion: Validation parameters such as linearity, precision, accuracy, limit of detection, limit of quantification, and robustness were performed. Amount of GZ was estimated using linearity equation.Conclusion: GG was found to contain 0.815±0.03 g% w/w GZ. Validated method may be used as one of the parameters to standardize the formulation.

scholarly journals Estimation of Abamectin Residues Present in Tea: High-Performance Liquid Chromatography Technique

2013 ◽  
Vol 2013 ◽  
pp. 1-5 ◽  
Author(s):  
Madasamy Kottiappan ◽  
Shanmugaselvan Veilumuthu Anandhan ◽  
Selvaganapathi Chandran
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Limit Of Detection ◽  
Black Tea ◽  
Water Mixture ◽  
Fluorescence Detector ◽  
Limit Of Quantification ◽  
Acetone Water ◽  
Sensitive Method

A simple, reliable, and sensitive method was based on high-performance liquid chromatography (HPLC) was developed and validated for the estimation of abamectin residues present in tea. The abamectin residues extracted with acetone-water mixture (70 : 30, v/v) and derivatised with 1-methylimidazole (1-MIM) and trifluoroacetic anhydride (TFAA) were estimated by HPLC using fluorescence detector (FLD). The technique was validated in terms of linearity, precision, recovery, specificity, limit of detection (LOD), and limit of quantification (LOQ). A good linear relationship () was absorbed in the abamectin concentration range from 0.01 to 1.0 μg mL−1. The limit of detection and limit of quantification of the method were 0.01 and 0.02 μg g−1, respectively. The average recoveries of the pesticide from black tea and dried green leaves ranged from 83.3 to 103.8% and 83.8 to 98.0%, respectively.

scholarly journals DEVELOPMENT AND VALIDATION OF REVERSE PHASE-HIGH PERFORMANCE LIQUID CHROMATOGRAPHY ASSAY METHOD FOR ESTIMATION OF FENOFIBRATE IN TABLET DOSAGE FORM PREPARED USING CRYSTALLO-CO-AGGLOMERATES OF THE DRUG

2021 ◽  
Vol 19 (1) ◽  
pp. 19-28
Author(s):  
SANTOSH GANDHI ◽  
MANGESH BHALEKAR ◽  
RAVINA MUTHA
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Linear Regression Analysis ◽  
Hplc Method ◽  
Assay Method ◽  
Reverse Phase ◽  
Rp Hplc ◽  
Specificity And Sensitivity ◽  
Tablet Dosage

The aim of the present study was to develop a simple isocratic reverse phase-high performance liquid chromatography (RP-HPLC) method and validate for the determination of fenofibrate in tablet dosage forms. RP-HPLC method was developed using Hi Q Sil C18 (250 cm × 4.6 mm, 5 μm) and mobile phase comprising 1 mM ammonium acetate buffer: Acetonitrile (10:90 v/v) at a flow rate of 1.0 mL/min. The detection was carried out at 290 nm. The retention time was found to be 6.15 ± 0.03 min. Validation of the method was performed for precision, accuracy, linearity, robustness, specificity and sensitivity to conform to the International Conference on Harmonization (ICH) guidelines. The data of linear regression analysis indicated a good linear response in the concentration range of 5 μg/mL–30 μg/mL with correlation co-efficient (R2) of 0.997. The developed method was found to be simple, sensitive, accurate and repeatable for assay of tablets of fenofibrate prepared using crystallo-co-agglomerates of the drug.

scholarly journals Determination of Sulfonamides in Feeds by High-Performance Liquid Chromatography after Fluorescamine Precolumn Derivatization

Molecules ◽  
2019 ◽  
Vol 24 (3) ◽  
pp. 452 ◽  
Author(s):  
Ewelina Patyra ◽  
Monika Przeniosło-Siwczyńska ◽  
Krzysztof Kwiatek
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Limit Of Detection ◽  
Phase System ◽  
Precolumn Derivatization ◽  
Detection Capability ◽  
Limit Of Quantification ◽  
Decision Limit ◽  
Limit Detection

A new multi-residue method for the analysis of sulfonamides (sulfadiazine, sulfamerazine, sulfamethazine, sulfaguanidine and sulfamethoxazole) in non-target feeds using high-performance liquid chromatography-fluorescence detection (HPLC-FLD) and precolumnderivatization was developed and validated. Sulfonamides (SAs) were extracted from feed with an ethyl acetate/methanol/acetonitrile mixture. Clean-up was performed on a Strata-SCX cartridge. The HPLC separation was performed on a Zorbax Eclipse XDB C18 column with a gradient mobile phase system of acetic acid, methanol, and acetonitrile. The method was validated according to EU requirements (Commission Decision 2002/657/EC). Linearity, decision limit, detection capability, detection and quantification limits, recovery, precision, and selectivity were determined, and adequate results were obtained. Using the HPLC-FLD method, recoveries were satisfactory (79.3–114.0%), with repeatability and reproducibility in the range of 2.7–9.1% to 5.9–14.9%, respectively. Decision limit (CCα) and detection capability (CCβ) were 197.7–274.6 and 263.2–337.9 µg/kg, respectively, and limit of detection (LOD) and limit of quantification (LOQ) were 34.5–79.5 and 41.3–89.9 µg/kg, respectively, depending on the analyte. Results showed that this analytical procedure is simple, rapid, sensitive, and suitable for the routine control of feeds.

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.

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