ESTIMATION OF TADALAFIL IN HUMAN PLASMA BY SPECTROFLUOROPHOTOMETRY

INDIAN DRUGS ◽  
2021 ◽  
Vol 58 (06) ◽  
pp. 60-63
Author(s):  
Sadhana Rajput ◽  
◽  
Samir Patel ◽  
Keyword(s):  
Human Plasma ◽  
Fluorescence Spectrum ◽  
Drug Monitoring ◽  
Limit Of Detection ◽  
Wave Length ◽  
Excitation Wavelength ◽  
Limit Of Quantification ◽  
Pharmacokinetic Investigation ◽  
Satisfactory Recovery

A new, specific, selective, simple, rapid and inexpensive spectrofluorophotometric method has been developed for the determination of tadalafil in spiked human plasma. The fluorescence spectrum of tadalafil in 0.1M methanolic sulphuric acid showed excitation wavelength at 315 nm and emission wave-length at 332 nm. The method for tadalafil was found to be linear over the concentration range of 10-50 ng/mL with a correlation coefficient of 0.9991. Limit of detection and limit of quantification were found to be 0.235 ng/mL and 0.701 ng/mL, respectively. The method was validated and found to be suitable for the estimation of tadalafil from human plasma. Satisfactory recovery of tadalafil from the human plasma suggests no interference of any debris present into human plasma. This method can be used to deter-mine plasma tadalafil concentration in drug monitoring or pharmacokinetic investigation.

HPTLC Separation of a Hepatoprotective Combination in Pharmaceutical Formulation and Human Plasma

2020 ◽  
Vol 58 (5) ◽  
pp. 411-417
Author(s):  
Maimana A Magdy ◽  
Rehab M Abdelfatah
Keyword(s):  
Human Plasma ◽  
High Performance ◽  
Limit Of Detection ◽  
Pharmaceutical Formulation ◽  
Limit Of Quantification ◽  
Ich Guidelines ◽  
Spiked Plasma ◽  
Significant Difference ◽  
Developing System

Abstract A binary mixture of Silymarin (SR) and Vitamin E (VE) acetate, of an antioxidant and a hepatoprotective effect, has been analyzed using a sensitive, selective and economic high performance thin layer chromatographic (HPTLC) method in their pure forms, pharmaceutical formulation and spiked human plasma. SR and VE were separated on 60F254 silica gel plates using hexane:acetone:formic acid (7:3:0.15, v/v/v) as a developing system with UV detection at 215 nm. The method was evaluated for linearity, accuracy, precision, selectivity, limit of detection (LOD) and limit of quantification (LOQ). SR and VE were detected in the linear range of 0.2–2.5 and 0.2–4.5 μg/band, respectively. Method validation was done as per ICH guidelines and acceptable results of accuracy of 99.86 ± 1.190 and 100.22 ± 1.609 for SR and VE, respectively were obtained. The method has been successfully applied for determination of the studied drugs in their pharmaceutical formulation without any interference from excipients, and in spiked plasma samples. Results obtained by the developed HPTLC-densitometric method were statistically compared to those obtained by the reported HPLC methods and no significant difference was found between them.

scholarly journals Micellar Enhanced Spectrofluorimetric Method for the Determination of Ponatinib in Human Plasma and Urine via Cremophor RH 40 as Sensing Agent

2015 ◽  
Vol 2015 ◽  
pp. 1-9 ◽  
Author(s):  
Hany W. Darwish ◽  
Ahmed H. Bakheit ◽  
Ali Saber Abdelhameed ◽  
Amer S. AlKhairallah
Keyword(s):  
Human Plasma ◽  
Fluorescence Intensity ◽  
Limit Of Detection ◽  
Biological Fluids ◽  
Great Success ◽  
Limit Of Quantification ◽  
Human Plasma And Urine ◽  
Spectrofluorimetric Method ◽  
Fluorescence Characteristics

An impressively simple and precise spectrofluorimetric procedure was established and validated for ponatinib (PTB) quantitation in biological fluids such as human plasma and human urine. This method depends on examining the fluorescence characteristics of PTB in a micellar system of Cremophor RH 40 (Cr RH 40). Cr RH 40 enhanced the intrinsic fluorescence of PTB distinctly in aqueous water. The fluorescence spectra of PTB was recorded at 457 nm following its excitation at 305 nm. Maximum fluorescence intensity was attained by addition of 0.7 mL of Cr RH 40 and one mL of phosphate buffer to PTB aliquots and then dilution with distilled water. There is a linear relationship between the fluorescence intensity of PTB and its concentration over the range 5–120 ngmL−1, with limit of detection and limit of quantification equal to 0.905 ngmL−1and 2.742 ngmL−1, respectively. The accuracy and the precisions of the proposed method were checked and gave adequate results. The adopted method was applied with a great success for PTB quantitation in different biological matrices (spiked human plasma and urine) giving high recovery values.

scholarly journals Determination of Ranitidine in Human Plasma by SPE and ESI-LC-MS/MS for Use in Bioequivalence Studies

2013 ◽  
Vol 2013 ◽  
pp. 1-7
Author(s):  
Karini B. Bellorio ◽  
Maria Isabel R. Alves ◽  
Nelson R. Antoniosi Filho
Keyword(s):  
Solid Phase Extraction ◽  
Human Plasma ◽  
Extraction Method ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Internal Standard ◽  
Phase Extraction ◽  
Good Separation ◽  
Limit Of Quantification

A method for determining ranitidine in human plasma by ESI-LC-MS/MS was validated, using propranolol as internal standard. The extraction method used was solid phase extraction (SPE). Chromatographic separation was performed in a Chromolith C18 (50 mm × 4.6 mm i.d.) analytical column, which provided good separation of ranitidine and propranolol peaks with an analysis time of 2.5 minutes. Extraction yields of 94.4% for ranitidine and 89.4% for the internal standard were obtained. The lower limit of quantification (LLOQ) was 3.00 ng/mL, and limit of detection (LOD) was 0.05 ng/mL, with linearity ranging from 3.00 to 500 ng/mL. The results, thus, showed that this method is suitable for application in bioequivalence studies of ranitidine in human plasma.

scholarly journals Method Development and Validation of Metformin Hydrochloride in Tablet Dosage Form

2011 ◽  
Vol 8 (3) ◽  
pp. 1309-1313 ◽  
Author(s):  
Kaushelendra Mishra ◽  
Himesh Soni ◽  
Govind Nayak ◽  
Sita Sharan Patel ◽  
A. K. Singhai
Keyword(s):  
Method Development ◽  
Limit Of Detection ◽  
Wave Length ◽  
Metformin Hydrochloride ◽  
Limit Of Quantification ◽  
System Suitability ◽  
Method Development And Validation ◽  
Development And Validation ◽  
Tablet Dosage

A simple, reproducible and efficient method for the determination of metformin hydrochloride (MET) was developed and validated. The analysis complied with Beer's law in the concentration range of 8-13 μg/mL at 233 nm for MET. In our study the validation of analytical method for determination of MET by UV in tablets formulation was performed in accordance the parameters including-system suitability, specificity, limit of quantification, limit of detection, linearity of response, accuracy, precision (reproducibility & repeatability), robustness (change of wave length±2 nm).

scholarly journals Development of a HPLC-UV method for determination of meloxicam in human plasma and pharmaceutical dosage forms

2014 ◽  
Vol 60 (4) ◽  
pp. 142-145 ◽  
Author(s):  
Csifo Enikő ◽  
Croitoru M. D. ◽  
Fülöp Ibolya ◽  
Muntean Daniela-Lucia
Keyword(s):  
Human Plasma ◽  
Limit Of Detection ◽  
Low Cost ◽  
Extraction Procedure ◽  
Dosage Forms ◽  
Composition Gradient ◽  
Range Limit ◽  
Limit Of Quantification ◽  
Pharmaceutical Dosage Forms

Abstract Objectives: A simple, quick and low cost HPLC-UV method for assay of meloxicam in plasma and pharmaceutical dosage forms was developed. Methods: Separation and assay of meloxicam, using a simple reverse phase HPLC-UV method was achieved using an Agilent Zorbax SB C18 column, with methanol and 1% aqueous solution of glacial acetic acid as mobile phase. Elution was performed with composition gradient, meloxicam being detected at 355 nm with a 5 minutes analysis time. The method was tested on human plasma and pharmaceutical dosage forms. Results: The retention time of the meloxicam was 3,7 minutes. Regression analysis showed good linearity, with correlation coefficient R= 0,9997; linear regression equation: y = 206,1x -77,5 over the 20-2000 ng/ml concentration range. Limit of detection was determined to be 5 ng/ml and limit of quantification was set at 15 ng/ml. The recovery of the analyte in human plasma was low: 30,50%, however it was reproducible, with a coefficient of variation of 4,83%. The analysis of the tablets resulted in a 85,82% of meloxicam compared to the declared concentration. Conclusions: The method proposed is quick, simple and adequate for detecting the meloxicam in human plasma. Although the recovery rate was low, it was reproducible, which leads to the fact, that improving extraction procedure can optimize the method.

scholarly journals Development and Validation of HPLC Method for Simultaneous Determination of Ceftriaxone and Cefaclor in Commercial Formulations and Biological Samples

2017 ◽  
Vol 57 (4) ◽  
Author(s):  
Jasmin Shah ◽  
M. Rasul Jan ◽  
Sultan Shah ◽  
M. Naeem Khan
Keyword(s):  
Simultaneous Determination ◽  
Human Plasma ◽  
High Performance ◽  
Limit Of Detection ◽  
High Performance Liquid Chromatographic ◽  
Reversed Phase ◽  
Hplc Method ◽  
Limit Of Quantification ◽  
Spiked Human Plasma

A reversed phase high performance liquid chromatographic method has been developed for the simultaneous determination of cefaclor and ceftriaxone cephalosporin antibiotic. The developed method has been validated and applied to mixtures of the commercial formulation and spiked human plasma. A mediterranea C<sub>18</sub> column (4.6 × 250 mm) was used with isocratic solvent delivery system and UV-visible detector. Different experimental parameters like solvent composition (acetonitrile: methanol: triethyl amine buffer 1:1:2 (v/v), flow rate of mobile phase (0.6 mLmin<sup>-1</sup>), pH of the buffer (7), and wavelength (260 nm) were optimized for effective separation and esolution of the analyte peaks. The separation was achieved in 6 min with retention times of 4.94 ± 0.056 min and 3.39 ± 0.022 min for cefaclor and ceftriaxone respectively. The linear range for both the studied drugs was found to be 0.5-250 μgmL<sup>-1</sup> with r<sup>2</sup> of 0.9987 (cefaclor) and 0.9997 (ceftriaxone). The limit of detection (3.3 σ/S) was found to be 2.34 × 10<sup>-2</sup> μgmL−1 and 1.70 × 10−2 μgmL<sup>-1</sup>, respectively, for cefaclor and ceftriaxone. Similarly limit of quantification (10σ/S) was 7.10 × 10−2 μgmL<sup>-1</sup> for cefaclor and 5.15 × 10−2 μgmL<sup>-1</sup> for ceftriaxone. The chromatographic procedure was applied to commercial formulations and spiked human plasma and the results were compared with literature HPLC method.

scholarly journals Utilization of 4-Chloro-7-Nittobenzo-2-Oxa-1, 3-Diazol (NBD-CL) as Chromogenic Reagent for Determination of Metformin hydrochloride (MET) in Pharmaceutical Formulation

2019 ◽  
Vol 7 (1) ◽  
pp. 19-23
Author(s):  
Abdalla Ahmed Elbashir ◽  
Omnia Mohamed Abdallah alfaki
Keyword(s):  
Quality Control ◽  
Limit Of Detection ◽  
Wave Length ◽  
Pharmaceutical Formulation ◽  
Metformin Hydrochloride ◽  
Linear Regression Equation ◽  
Reaction Conditions ◽  
Medium Ph ◽  
Limit Of Quantification

A new, simple, selective, precise and accurate spectrophotometric method for the determination of metformin in pharmaceutical formulation was developed and validated. The method was based on the reaction between metformin and 4-chloro-7-nitrobenzo-2-oxa-1,3-diazole (NBD-Cl) at alkaline medium (pH 12.0) to form brown adduct.  Beer’s law was obeyed in the concentration range of 20-100 μg mL-1  of  metformin at maximum wave length 465 nm . Under the optimized reaction conditions, the linear regression equation of the calibration curve was found to be y=0.003x +0.156 with a linear correlation coefficient (r=0.999). The limit of detection (LOD) and limit of quantification (LOQ) were found to be 5.8, 17.5 μg mL-1 respectively. The method is useful for routine analysis of metformin in quality control laboratories.

Spectrophotometeric Determination of Trifluoperazine HCL in Pure Forms and Pharmaceutical Preperations

2017 ◽  
Vol 9 (5) ◽  
Author(s):  
Mohammad Hamzah Hamzah ◽  
Rawa M M Taqi ◽  
Muna M. Hasan ◽  
Raid J. M. Al-Timimi
Keyword(s):  
Standard Method ◽  
Limit Of Detection ◽  
Molar Absorptivity ◽  
Dosage Forms ◽  
Oxidizing Agent ◽  
Optimum Conditions ◽  
Limit Of Quantification ◽  
Cerium Ion ◽  
Blank Solution

A simple and accurate spectrophotometric method for the determination of Trifluoperazine HCl in pure and dosage forms was developed. The method is based on the reaction between Trifluoperazine HCl and p-chloroaniline in the presence of cerium ion as oxidizing agent which lead to the formation of violate color product that absorbed at a maximum wavelength 570nm while the blank solution was pink. Under the optimum conditions a linear relationship between the intensity and concentration of TRF in the range 4-50μg/ml was obtained . The molar absorptivity 3.74×103 L.mol-1.cm-1 , Limit of detection (2.21μg/ml), while limit of quantification was 7.39μg/ml. The proposed analytical method was compared with standard method using t-test and F-test , the obtained results shows there is no significant differences between proposed method and standard method. Based on that the proposed method can be used as an alternative method for the determination of TRF in pure and dosage forms.

Development and Validation of a New Method for the Determination of Anti-hepatitis C Agent Simeprevir in Human Plasma using HPLC with Fluorescence Detection

2020 ◽  
Vol 16 (4) ◽  
pp. 428-435
Author(s):  
Ahmed F.A. Youssef ◽  
Yousry M. Issa ◽  
Kareem M. Nabil
Keyword(s):  
Hepatitis C ◽  
Human Plasma ◽  
Fluorescence Detection ◽  
Internal Standard ◽  
Protein Precipitation ◽  
Assay Method ◽  
Fluorescence Detector ◽  
Limit Of Quantification ◽  
Relative Standard

Background: Simeprevir is one of the recently discovered drugs for treating hepatitis C which is one of the major diseases across the globe. Objective: The present study involves the development of a new and unique High-Performance Liquid Chromatography (HPLC) method using fluorescence detection for the determination of simeprevir (SIM) in human plasma. Methods: Two methods of extractions were tested, protein precipitation using acetonitrile and liquidliquid extraction. A 25 mM dipotassium hydrogen orthophosphate (pH 7.0)/ACN (50/50; v/v), was used as mobile phase and C18 reversed phase column as the stationary phase. The chromatographic conditions were optimized and the concentration of simeprevir was determined by using the fluorescence detector. Cyclobenzaprine was used as an internal standard. Results: Recovery of the assay method based on protein precipitation was up to 100%. Intra-day and inter-day accuracies range from 92.30 to 107.80%, with Relative Standard Deviation (RSD) range 1.65-8.02%. The present method was successfully applied to a pharmacokinetic study where SIM was administered as a single dose of 150 mg SIM/capsule (Olysio®) to healthy individuals. Conclusion: This method exhibits high sensitivity with a low limit of quantification 10 ng mL-1, good selectivity using fluorescence detection, wide linear application range 10-3000 ng mL-1, good recovery and highly precise and validation results. The developed method can be applied in routine analysis for real samples.

scholarly journals A novel LC-MS method development and validation for the determination of phenyl vinyl sulfone in eletriptan hydrobromide

2021 ◽  
Vol 7 (1) ◽  
Author(s):  
Indhu Priya Mabbu ◽  
G. Sumathi ◽  
N. Devanna
Keyword(s):  
Method Development ◽  
Limit Of Detection ◽  
Vinyl Sulfone ◽  
Limit Of Quantification ◽  
Relative Standard ◽  
Pressure Chemical Ionization ◽  
Pressure Chemical ◽  
Development And Validation ◽  
Phenyl Vinyl

Abstract Background The aim of the present method is to develop and validate a specific, sensitive, precise, and accurate liquid chromatography-mass spectrometry (LC-MS) method for the estimation of the phenyl vinyl sulfone in the eletriptan hydrobromide. The effective separation of the phenyl vinyl sulfone was achieved by the Symmetry C18 (50 × 4.6 mm, 3.5 μm) column and a mobile phase composition of 0.1%v/v ammonia buffer to methanol (5:95 v/v), using 0.45 ml/min flow rate and 20 μl of injection volume, with methanol used as diluent. The phenyl vinyl sulfone was monitored on atomic pressure chemical ionization mode mass spectrometer with positive polarity mode. Results The retention time of phenyl vinyl sulfone was found at 2.13 min. The limit of detection (LOD) and limit of quantification (LOQ) were observed at 1.43 ppm and 4.77 ppm concentration respectively; the linear range was found in the concentration ranges from 4.77 to 27.00 ppm with regression coefficient of 0.9990 and accuracy in the range of 97.50–102.10%. The percentage relative standard deviation (% RSD) for six replicates said to be injections were less than 10%. Conclusion The proposed method was validated successfully as per ICH guidelines. Hence, this is employed for the determination of phenyl vinyl sulfone in the eletriptan hydrobromide.

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