scholarly journals Determination of dehydroepiandrosterone in dietary supplements by reversed-phase HPLC

2022 ◽  
Vol 20 (2) ◽  
pp. 383-387
Author(s):  
Yahia Z. Tabaza ◽  
Kamal M. Mansi ◽  
Hanan A. Azzam ◽  
Farah F. Al-Mamoori ◽  
Ali M. Al-Samydai ◽  
...  
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Dietary Supplements ◽  
High Performance ◽  
Cost Effective ◽  
Reversed Phase ◽  
Hplc Method ◽  
Time Saving ◽  
Relative Standard

Purpose: To develop a reversed phase high performance liquid chromatography (HPLC) method for the determination of dehydroepiandrosterone (DHEA) in dietary supplements. Methods: A reversed-phase high performance liquid chromatography (HPLC) method was developed for the determination of DHEA in dietary supplements. An isocratic system consisting of methanol and water (70:30 v/v) was run at a flow rate of 1 mL/min on a C18 HPLC column to achieve the separation. The method was validated with regard to linearity, intra-day and inter-day precision, and limits of both detection and quantification. Results: The method achieved a retention time of 10.8 min, a resolution of 4.12, a detection limit (LOD) of 50 ng/μL, a quantification limit (LOQ) of 166.7 ng/μL and a label claim of 108.6 % with a relative standard deviation (RSD) of 0.38 % over a range of 0.0625 – 0.50 mg/mL with a correlation coefficient of 0.9997. Conclusion: The method is simple, cost effective, time-saving and reliable for determining DHEA when compared to other reported methods in literature. Thus, it will be of benefit to manufacturers of this dietary supplement to adopt the method for quantitative laboratory analysis.

Developing a High-performance Liquid Chromatography Method for Simultaneous Determination of Loratadine and its Metabolite Desloratadine in Human Plasma

2020 ◽  
Vol 20 (13) ◽  
pp. 1053-1059
Author(s):  
Mahmoud M. Sebaiy ◽  
Noha I. Ziedan
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Human Plasma ◽  
High Performance ◽  
Allergic Diseases ◽  
Reversed Phase ◽  
Hplc Method ◽  
H1 Receptor ◽  
Chromatography Method

Background: Allergic diseases are considered as the major burden on public health with increased prevalence globally. Histamine H1-receptor antagonists are the foremost commonly used drugs in the treatment of allergic disorders. The target drug in this study, loratadine, belongs to this class of drugs and its biometabolite desloratadine which is also a non-sedating H1 receptor antagonist with anti-histaminic activity being 2.5 to 4 times greater than loratadine. This study aimed to develop and validate a novel isocratic Reversed-phase High-Performance Liquid Chromatography (RP-HPLC) method for rapid and simultaneous separation and determination of loratadine and its metabolite, desloratadine in human plasma. Methods: The drug extraction method from plasma was based on protein precipitation technique. The separation was carried out on a Thermo Scientific BDS Hypersil C18 column (5μm, 250 x 4.60 mm) in a mobile phase of MeOH: 0.025M KH2PO4 adjusted to pH 3.50 using orthophosphoric acid (85: 15, v/v) at an ambient temperature. The flow rate was maintained at 1 mL/min and maximum absorption was measured using the PDA detector at 248 nm. Results: The retention times of loratadine and desloratadine in plasma samples were recorded to be 4.10 and 5.08 minutes, respectively, indicating a short analysis time. Limits of detection were found to be 1.80 and 1.97 ng/mL for loratadine and desloratadine, respectively, showing a high degree of sensitivity of the method. The method was then validated according to FDA guidelines for the determination of the two analytes in human plasma. Conclusion: The results obtained indicate that the proposed method is rapid, sensitive in the nanogram range, accurate, selective, robust and reproducible compared to other reported methods.

scholarly journals A Selective High-Performance Liquid Chromatography Method for the Determination of Reboxetine in Bulk Drug and Tablets

2006 ◽  
Vol 89 (6) ◽  
pp. 1552-1556
Author(s):  
ArmaĞan Önal ◽  
Olcay SaĞiri ◽  
S Müge Çetin ◽  
Sidika Toker
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Depressive Disorders ◽  
Degradation Products ◽  
Severe Depression ◽  
Hplc Method ◽  
Chromatography Method ◽  
Relative Standard

Abstract Reboxetine is used as a selective noradrenaline reuptake inhibitor for the treatment of major depressive disorders. It is effective in the treatment of severe depression and safer to use than traditional tricyclic antidepressants. In this study, a novel, simple, and rapid stability-indicating high-performance liquid chromatography (HPLC) method for reboxetine methansulfonate was successfully developed and validated for the assay of tablets. The method was used to quantify reboxetine in tablets; it employed a C18 column (150 4.6 mm id) with an isocratic mobile phase consisting of methanolphosphate buffer (pH 7, 0.02 M; 55 + 45, v/v) at a flow rate of 1.0 μmL/min. Reboxetine was detected by an ultraviolet detector at 277 nm. The retention time of reboxetine was about 4.5 min. The developed HPLC method was validated with respect to linearity, precision, sensitivity, accuracy, and selectivity. The method was linear over the concentration range 150 g/mL (r 0.9999). The limits of detection and the quantitation of reboxetine were 0.1 and 0.3 μg/mL, respectively. The relative standard deviation values for intraday and interday precision were 0.781.01 and 1.081.37%, respectively. Selectivity was validated by subjecting a stock solution of reboxetine to neutral, acid, and alkali hydrolysis, as well as oxidation, dry heat treatment, and photodegradation. The peaks of the degradation products did not interfere with the peak of reboxetine. The results indicated that the proposed method could be used in a stability assay. The proposed method was successfully applied to the determination of reboxetine in tablets. Excipients present in the tablets did not interfere with the analysis.

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 SIMULTANEOUS DETERMINATION OF DIPHENHYDRAMINE, EPHEDRINE, NOSCAPINE, AND GLYCEROL GLYCOLATE USING STABILITY-INDICATING HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY: APPLICATION TO NOSCOF TABLETS

2019 ◽  
pp. 505-511
Author(s):  
PULAGURTHA BHASKARARAO ◽  
GOWRI SANKAR DANNANA
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Uv Light ◽  
Reversed Phase ◽  
Hplc Method ◽  
Stability Indicating ◽  
Rp Hplc ◽  
Relative Standard ◽  
Validation Parameters

Objective: Noscof tablet is a fixed dosage combination formulation having diphenhydramine (DH), ephedrine (ED), noscapine (NP), and glycerol glycolate (GG). A sensitive, selective, accurate, precise, and stability-indicating reversed-phase high-performance liquid chromatography (RP-HPLC) method with photodiode array detection has been developed and validated for simultaneous analysis of DH, ED, NP, and GG in bulk drug and Noscof tablets. Methods: Reversed-phase chromatographic separation and analysis of DH, ED, NP, and GG were done on an Altima C18 column with 0.01 M KH2PO4 buffer (pH 3.5) and acetonitrile (50:50%, v/v) as mobile phase at 0.8 ml/min flow rate in isocratic mode. Detection was performed at 260 nm. The method was validated in harmony with International Conference on Harmonization (ICH) guidelines. The tablet sample solution was subjected to diverse stress conditions using ICH strategy such as hydrolytic degradation (neutral - with distilled water, alkaline - with 2 N NaOH, and acidic - with 2 N HCl), oxidation (with 10% H2O2), photodegradation (exposing to UV light), and dry heat degradation (exposing to 105°C). Results: Using the above stated chromatographic conditions, sharp peaks were obtained for ED, NP, DH, and GG with retention time of 3.272 min, 4.098 min, 5.467 min, and 6.783 min, respectively. Good regression coefficient values were obtained in the range of 2–12 μg/ml for ED, 3.75–22.5 μg/ml for NP, 3.125–18.75 μg/ml for DH, and 25–150 μg/ml for GG. The quantification limits were 0.181 μg/ml, 0.187 μg/ml, 0.246 μg/ml, and 1.114 μg/ml for ED, NP, DH, and GG, respectively. The values of validation parameters are within the acceptance limits given by ICH. The ED, NP, DH, and GG showed more percent of degradation in acid condition and less percent of degradation in the neutral condition. The peaks of degradants did not interfere with the peaks of analytes. ED, NP, DH, and GG were assessed with a good percentage of the assay (near to 100%) and low percent relative standard deviation (<2%) in Noscof tablets using the proposed method. Conclusion: The stability indicating RP-HPLC method developed was suitable for quantifying ED, NP, DH, and GG simultaneously in bulk as well as in tablet formulation.

Development of a Method for the Determination of Pyrimethamine Concentrations in Feeds by Ion-Pairing High-Performance Liquid Chromatography

2002 ◽  
Vol 65 (4) ◽  
pp. 688-691 ◽  
Author(s):  
P. S. GONG ◽  
S. L. JENG ◽  
Y. F. HSU ◽  
C. C. LIN ◽  
S. Y. LIN
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Ion Pairing ◽  
Reversed Phase ◽  
Hplc Method ◽  
Alumina Column ◽  
Tetramethylammonium Chloride ◽  
Array Detection

An ion-pairing reversed-phase high-performance liquid chromatography (HPLC) method with diode array detection at 280 nm was developed to determine pyrimethamine concentrations in feed for laying hens. Pyrimethamine was extracted with a mixture of 5% isobutanol and 95% benzene, and the extract was cleaned up on an alumina column. The drug was eluted from an Intersil ODS-3V column (250 by 4.6 mm) with a mixture of 25% acetonitrile and 75% water (vol/vol) containing 0.01 M tetramethylammonium chloride as an ion-pairing agent and adjusted with acetic acid to pH 3.5. The flow rate was 1.0 ml/min. Mean recovery of pyrimethamine from supplemented feeds at concentrations of 2, 4, and 5 μg/g of feed were 100.5, 103.5, and 100.8%, respectively. Precision within a day ranged from 4.3 to 7.0% for the three concentrations, and day-to-day precision was 5.3% for feed supplemented at a concentration of 4 μg/g. No chromatographic interference was detected from other 2,4-diaminopyrimidine compounds or other major drugs used in poultry.

Validation of HPLC Method for Determination of Histamine in Human Immunoglobulin Formulations

2020 ◽  
Vol 103 (5) ◽  
pp. 1223-1229
Author(s):  
Michikazu Tanio ◽  
Toru Nakamura ◽  
Hideki Kusunoki ◽  
Kyohei Ideguchi ◽  
Kazuyuki Nakashima ◽  
...  
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Standard Deviation ◽  
High Performance ◽  
Gradient Elution ◽  
Hplc Method ◽  
Human Immunoglobulin ◽  
Histamine Dihydrochloride ◽  
Relative Standard

Abstract Background Histamine fixed-immunoglobulin formulations, which consisted of 0.15 µg of histamine dihydrochloride and 12 mg of human immunoglobulin in a vial, are used for anti-allergic treatments, and controlling the amounts of histamine in the formulations is essential to avoid histamine intoxication. Objective A high-performance liquid chromatography (HPLC) method for determination of histamine contents of the formulations was established and validated. Methods Histamine extracted from the formulation was labeled with 6-aminoquinolyl-N-hydroxysuccinimidyl carbamate and was analyzed by gradient elution HPLC with UV detection at 260 nm. Results The method showed linearity in the range 0.8–2.4 µM (R &gt; 0.999), accuracy (100.1–105.8% recovery), and precision (relative standard deviation ≤ 1.93%). The validated method was applied for five lots of the pharmaceutical, and their histamine contents were determined to be 0.149–0.155 µg/vial. Conclusions These results indicated that the validated method is useful to control amounts of histamine in biopharmaceutical products. Highlights The HPLC method was developed for quantitative determination of histamine content of the histamine fixed-immunoglobulin formulations.

scholarly journals ANALYITCAL METHOD DEVELOPMENT AND VALIDATION OF A REVERSED-PHASE HIGHPERFORMANCE LIQUID CHROMATOGRAPHY FOR THE DETERMINATION OF MODAFINIL IN BULK AND PHARMACEUTICAL DOSAGE FORMS

2016 ◽  
Vol 9 (5) ◽  
pp. 177
Author(s):  
Bijithra Cholaraja ◽  
Shanmugasundaram P ◽  
Ragan G ◽  
Sankar Ask ◽  
Sumithra M
Keyword(s):  
Particle Size ◽  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Reversed Phase ◽  
Dosage Forms ◽  
Hplc Method ◽  
Rp Hplc ◽  
Development And Validation

ABSTRACTObjective: To development and validation of a reversed-phase high-performance liquid chromatography (RP-HPLC) for the determination of modafinilin bulk and pharmaceutical dosage forms.Methods: A simple, precise, rapid, and accurate RP-HPLC method was developed for the estimation of modafinil in bulk and pharmaceutical dosageforms. Xterra RP 18 (250 mm × 4.6 mm, 5 µ particle size) with a mobile phase consisting of methanol:water 70:30 V/V was used. The flow rate1.0 ml/min and the effluents were monitored at 260 nm. The retention time and recovery time was 12 minutes. The detector response was linear inthe concentration of 10-50 µg/ml. The respective linear regression equation being Y=452.1x+65237. The limit of detection and limit of quantificationwere 4.547 and 1.377 mcg, respectively. The method was validated by determining its accuracy, precision, and system suitability.Result: The objective of the present work is to develop simple, precise, and reliable HPLC method for the analysis of modafinil in bulk andpharmaceutical dosage forms. This is achieved using the most commonly employed Xterra RP 18 (250 mm × 4.6 mm, 5 μ particle size) columndetection at 260 nm. The present method was validated according to ICH guidelines.Conclusion: In this study, a simple, fast and reliable HPLC method was developed and validated for the determination of modafinil in pharmaceuticalformulations.Keywords: Modafinil, Reversed-phase high-performance liquid chromatography, Estimation, ICH guidelines, Tablets. 

Determination of β -Sitosterol with Chemical Course and Material Applications in Jatropha Seed Oil by High Performance Liquid Chromatography

2012 ◽  
Vol 577 ◽  
pp. 69-72 ◽  
Author(s):  
Shu Yu Liu ◽  
Anaerguli Maihemuti
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Seed Oil ◽  
Reversed Phase ◽  
Analytical Recovery ◽  
Relative Standard ◽  
The Mean ◽  
Jatropha Seed

A simple and rapid high performance liquid chromatography (HPLC) assay was developed to identify and measure theβ-sitosterol with chemical course and material applications in jatropha seed oil. The stigmasterol was isolated with a good selectivity by HPLC employing reversed phase C18 columns. The components were separated by mobile phase of methanol-water (99/1, v/v) and detected at 205nm. The quantitation of the stigmasterol was reproducible and the method relative standard deviation is 1.1%. The mean analytical recovery was 96.2%.

Quantitation of Transdermal Tadalafil in Human Skin by Reversed-Phase High-Performance Liquid Chromatography

2012 ◽  
Vol 95 (4) ◽  
pp. 1064-1068 ◽  
Author(s):  
Mohammed H Mehanna ◽  
Abdel M Motawaa ◽  
Magda W Samaha
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Human Skin ◽  
Mobile Phase ◽  
High Performance ◽  
Reversed Phase ◽  
Hplc Method ◽  
Drug Deposition ◽  
Transdermal Permeation

Abstract A reliable and sensitive HPLC method was developed for the quantitation of tadalafil transdermal permeation through human skin. An RP column with UV detection at 290 nm was used for chromatographic separation at ambient temperature. The mobile phase was acetonitrile–water containing 20 mM pH 7 phosphate buffer (35/65, v/v) with a flow rate of 1.0 mL/min. The LOQ achieved was 1 ng/mL, and the calibration curve showed good linearity over the concentration range of 5–2000 ng/mL for tadalafil, with a determination coefficient (R2) of 0.998. The RSD values of intraday and interday analyses were all within 7%. Parameters of validation proved the precision of the method; this validated method was applied for the determination of tadalafil in transdermal permeation and drug deposition in human skin studies.

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