scholarly journals Spectrofluorimetric determination of Bisoprolol fumarate and Rosuvastatin calcium in a novel combined formulation and in human spiked plasma

2018 ◽  
Vol 9 (4) ◽  
pp. 331-337 ◽  
Author(s):  
Nada Sayed Abdelwahab ◽  
Nouruddin Wageh Ali ◽  
Marco Mounir Zaki ◽  
Adel Ahmed Ali ◽  
Mohamed Mohamed Abdelkawy
Keyword(s):  
Simultaneous Determination ◽  
High Sensitivity ◽  
Emission Wavelength ◽  
Bioanalytical Method Validation ◽  
Spiked Plasma ◽  
Spectrofluorimetric Method ◽  
Significant Difference ◽  
Spectrofluorimetric Determination ◽  
Rosuvastatin Calcium

Sensitive, simple and rapid spectrofluorimetric method was developed for simultaneous determination of bisoprolol fumarate (BIS) and rosuvastatin calcium (ROS) in novel formulated tablets and in human spiked plasma depending on measuring their native fluorescence. The fluorescence intensity of BIS and ROS were measured in methanol at emission wavelength of 297 and 485 nm upon excitation at 227 and 242 nm, respectively. The emission spectrum of each drug reveals zero value at the emission wavelength of the other drug, thus allowing their simultaneous determination without any interference and without using any tedious derivatization steps. Excellent linearity was obtained over the range of 10-500 and 20-1000 ng/mL for BIS and ROS, respectively. The developed method was evaluated by applying to laboratory prepared mixtures and pharmaceutical formulation. The high sensitivity of the method was the motivation to its application for analysis of the cited drugs in spiked human plasma. Likewise, analytical and bioanalytical method validation was carried out following International Conference on Harmonisation guidelines and also statistical analysis with the reported methods was carried out and no significant difference was found. The developed method is the first developed spectrofluorimetric method for simultaneous determination of the newly formulated drugs.

scholarly journals Simultaneous Determination of Amlodipine Besylate and Atorvastatin Calcium in Binary Mixture by Spectrofluorimetry and HPLC Coupled with Fluorescence Detection

2013 ◽  
Vol 8 ◽  
pp. ACI.S12921 ◽  
Author(s):  
Bahia A. Moussa ◽  
Asmaa A. El-Zaher ◽  
Marianne A. Mahrouse ◽  
Maha S. Ahmed
Keyword(s):  
Simultaneous Determination ◽  
Fluorescence Detection ◽  
High Sensitivity ◽  
Hplc Method ◽  
Detection Methods ◽  
Amlodipine Besylate ◽  
Atorvastatin Calcium ◽  
New Methods ◽  
Spectrofluorimetric Method

Caduet tablets are novel prescription drug that combines amlodipine besylate (AM) with atorvastatin calcium (AT). A spectrofluorimetric and an HPLC-fluorescence detection methods were developed for simultaneous determination of both drugs in tablets. In the spectrofluorimetric method, native fluorescence of AM and AT were measured in methanol at 442 and 369 nm upon excitation at 361 and 274 nm, respectively. The emission spectrum of each drug reveals zero value at the emission wavelength of the other drug, thus allowing their simultaneous determination without interference. In the HPLC method, separation of AM and AT was achieved within 8 minutes on a C18 column using acetonitrile:phosphate buffer (0.015 M, pH 3) (45:55, v/v) as the mobile phase. Fluorescence detection was carried out using excitation wavelengths 361 and 274 nm and emission wavelengths 442 and 378 nm for AM and AT, respectively. Excellent linearity was observed. Careful validation proved advantages of the new methods: high sensitivity, accuracy, selectivity and suitability for quality control laboratories.

scholarly journals Novel Spectrophotometric Methods for Simultaneous Determination of Rosuvastatin Calcium, Timolol Maleate and Diclofenac Sodium in Pharmaceutical Ternary Mixture and Spiked Human Plasma

2019 ◽  
pp. 1-21 ◽  
Author(s):  
Mohamed E. M. Hassouna ◽  
Hafsa O. Salem
Keyword(s):  
Simultaneous Determination ◽  
Human Plasma ◽  
Limit Of Detection ◽  
Diclofenac Sodium ◽  
Correlation Coefficients ◽  
Timolol Maleate ◽  
Spiked Human Plasma ◽  
Significant Difference ◽  
Rosuvastatin Calcium

Three sensitive, times saving, precise and accurate spectrophotometric techniques have been established and confirmed for the simultaneous determination of ternary admixture of rosuvastatin calcium (ROSCa), timolol maleate (TIM) and diclofenac sodium (DICNa). Method A, first derivative of ratio spectra spectrophotometric (1st DD) which is the most simple simplest one. Using the spectrum of an aliquot of 5 μg/mL of DICNa as a divisor, ROSCa could be determined by measuring 1DD amplitudes at 239.5 and 266.5 nm for ROSCa, while TIM could be similarly determined at 307.7 and 331 nm. DICNa could be determined at 269.7 and 292 nm when 5 μg/mL aliquot of ROSCa was used as a divisor without interference. This method showed limit of detection of 0.556, 0.567 & 0.3 µg/mL and correlation coefficients of 0.9997, 0.9998 and 0.9995 for ROSCa, DICNa and TIM respectively. Method B, depends on subjecting the ratio spectra to mean centering (MCRS). The arithmetical description of this method was explained. The method was performed for the estimation of these drugs together in one run without preseparation in authentic laboratory prepared mixtures, bulk and spiked human plasma. The wave lengths 277.9, 313.1 and 333.12 nm were used for the quantitative estimation of each of the studied drugs with good correlation coefficients (0.9998, 0.997& 0.9999 and LOD of 0.297, 0.150 & 0.24 µg/mL for the studied drugs in the previously mentioned order. Method C, successive-ratio derivative spectra method (SRDS). The mathematical description of the method was explained. By using this method, ROSCa, TIM and DICNa could be determined at 264, 339 and 300 nm, respectively. Correlation coefficients were 0.9998, 0.9999 & 0.9995 and LOD values of 0.374, 0.258 & 0.769 µg/mL in the same order. The three methods were linear in the range 5-25 µg/mL. The obtained results has been statistically compared with those obtained by the published one, showing no significant difference regarding accuracy and precision at p = 0.05. The developed methods do not need sophisticated techniques or instruments, besides being sensitive, selective and eco-friendly.

scholarly journals Simultaneous determination of bisoprolol fumarate and rosuvastatin calcium in a new combined formulation by validated RP-HPLC

2019 ◽  
Vol 10 (1) ◽  
pp. 52-56
Author(s):  
Marco Mounir Zaki ◽  
Nada Sayed Abdelwahab ◽  
Adel Ahmed Ali ◽  
Souty Mounie Zaki Sharkawi
Keyword(s):  
Simultaneous Determination ◽  
Mobile Phase ◽  
Orthophosphoric Acid ◽  
Hplc Method ◽  
Factors Affecting ◽  
Bulk Powder ◽  
Rp Hplc ◽  
Significant Difference ◽  
Rosuvastatin Calcium

A simple, specific, and precise RP-HPLC method was developed and validated for simultaneous determination of Bisoprolol fumarate (BIS) and Rosuvastatin calcium (ROS) in new formulated tablets. The developed RP-HPLC method depended on chromatographic separation using C18 column (150×4.6 mm, 0.5 μm) with mobile phase consisted of acetonitrile and 0.05 aqueous solution of orthophosphoric acid at the ratio of 65:35 % (v:v) with a flow rate of 1 mL/min and UV detection was carried out at 230 nm. Factors affecting the developed methods were studied and optimized and the retention times for BIS and ROS were found to be 2.758 and 4.974 min, respectively. Linearity of the proposed method was observed over a concentration range 0.2-50 μg/mL for each of BIS (r = 0.9999) and ROS (r = 0.9998). The proposed method was successfully applied for the determination of the studied drugs in their bulk powder, laboratory prepared mixtures and in the formulated tablets. The developed method is the first chromatographic method for determination of those drugs and showed no significant difference when compared with the reported methods.

scholarly journals New Spectrofluorimetric Method with Enhanced Sensitivity for Determination of Paroxetine in Dosage Forms and Plasma

2008 ◽  
Vol 3 ◽  
pp. ACI.S1053 ◽  
Author(s):  
Ibrahim A. Darwish ◽  
Sawsan M. Amer ◽  
Heba H. Abdine ◽  
Lama I. Al-Rayes
Keyword(s):  
High Sensitivity ◽  
Dosage Forms ◽  
Official Method ◽  
Factors Affecting ◽  
Pharmaceutical Tablets ◽  
Enhanced Sensitivity ◽  
Spectrofluorimetric Method ◽  
Relative Standard ◽  
Optimized Conditions

New simple spectrofluorimetric method with enhanced sensitivity has been developed and validated for the determination of the antidepressant paroxetine (PXT) in its dosage forms and plasma. The method was based on nucleophilic substitution reaction of PXT with 4-chloro-7-nitrobenzo-2-oxa-1,3-diazole in an alkaline medium (pH 8) to form a highly fluorescent derivative that was measured at 545 nm after excitation at 490 nm. The factors affecting the reaction was carefully studied and optimized. The kinetics of the reaction was investigated, and the reaction mechanism was presented. Under the optimized conditions, linear relationship with good correlation coefficient (0.9993) was found between the fluorescence intensity and PXT concentration in the range of 80-800 ng ml-1. The limits of detection and quantitation for the method were 25 and 77 ng ml-1, respectively. The precision of the method was satisfactory; the values of relative standard deviations did not exceed 3%. The proposed method was successfully applied to the determination of PXT in its pharmaceutical tablets with good accuracy; the recovery values were 100.2 ± 1.61%. The results obtained by the proposed method were comparable with those obtained by the official method. The proposed method is superior to the previously reported spectrofluorimetric method for determination of PXT in terms of its higher sensitivity and wider linear range. The high sensitivity of the method allowed its successful application to the analysis of PXT in spiked human plasma. The proposed method is practical and valuable for its routine application in quality control and clinical laboratories for analysis of PXT.

Simultaneous determination of duloxetine and 4-hydroxy duloxetine glucuronide in human plasma and back-conversion study

Bioanalysis ◽  
2021 ◽  
Author(s):  
Gabriel Onn Kit Loh ◽  
Emily Yii Ling Wong ◽  
Yvonne Tze Fung Tan ◽  
Yi Lin Lee ◽  
Chun Keat Chew ◽  
...  
Keyword(s):  
Simultaneous Determination ◽  
Human Plasma ◽  
Method Validation ◽  
Bioequivalence Study ◽  
Stability Study ◽  
Bioanalytical Method Validation ◽  
Study Materials ◽  
Study Results ◽  
Back Conversion

Aim: To develop an LC-MS/MS method for simultaneous determination of duloxetine and its metabolite, 4-hydroxy duloxetine glucuronide (4HDG) in human plasma and to investigate the potential back-conversion of 4HDG to duloxetine using stability study. Materials & methods: The LC-MS/MS method was validated according to the EMA and USFDA Bioanalytical Method Validation Guidelines and applied to pilot bioequivalence study. Results & conclusion: The method validation results were within the acceptance limits. The stability study and incurred sample reanalysis results ruled out the occurrence of back-conversion. The study highlighted the conduct of back-conversion test and the advantages of LC-MS/MS method in terms of sensitivity, specificity and low consumption of organic solvents.

scholarly journals Spectrofluorimetric Determination of Vigabatrin and Gabapentin in Dosage Forms and Spiked Plasma Samples Through Derivatization with 4-Chloro-7-Nitrobenzo-2-Oxa-1,3-Diazole

2001 ◽  
Vol 84 (4) ◽  
pp. 1017-1024 ◽  
Author(s):  
Ekram M Hassan ◽  
Fathalla Belal ◽  
Omar A Al-Deeb ◽  
Nasr Y Khalil
Keyword(s):  
Reaction Pathway ◽  
Dosage Forms ◽  
Specific Method ◽  
Plasma Samples ◽  
Spiked Plasma ◽  
Highly Sensitive ◽  
Percent Recovery ◽  
Spectrofluorimetric Determination ◽  
Label Claim

Abstract A highly sensitive and specific method is proposed for the determination of vigabatrin (I) and gabapentin (II) in their dosage forms and spiked human plasma. The method is based on coupling the drugs with 4-chloro-7-nitrobenzo-2-oxa-1,3-diazole in borate buffer at pH 7.1 and measuring the resulting fluorescence at 532 nm after excitation at 465 nm. The fluorescence intensity was a linear function of the concentration of the drugs over the ranges of 1.3–6.5 and 1.7–8.5 μg/mL for I and II, respectively. Minimum detectability values were 0.54 μg/mL (4.2 × 10−6M) and 0.97 μg/mL (5.7 × 10−6M) for I and II, respectively, under the described conditions. The proposed method was successfully applied to the determination of the 2 drugs in their dosage forms, and the percent recoveries ± standard deviation (SD) were 104.53 ± 1.2 and 100.00 ± 1.32 of the label claim for I and II, respectively. The method was further applied to the determination of vigabatrin in spiked plasma samples. The percent recovery ± SD was 101.58 ± 2.68. Interference from endogenous α-amino acids was overcome through selective complexation with freshly prepared Cu(OH)2. The interference likely to be encountered from co-administered drugs, such as carbamazepine, cimetidine, clonazepam, clopazam, phenobarbital, valproic acid, and lamotrigine, was also studied. A reaction pathway is suggested.

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 Simultaneous Determination of Sitagliptin and Metformin in Pharmaceutical Preparations by Capillary Zone Electrophoresis and its Application to Human Plasma Analysis

2012 ◽  
Vol 7 ◽  
pp. ACI.S9940 ◽  
Author(s):  
Mohamed Salim ◽  
Nahed El-Enany ◽  
Fathallah Belal ◽  
Mohamed Walash ◽  
Gabor Patonay
Keyword(s):  
Simultaneous Determination ◽  
Human Plasma ◽  
Capillary Zone Electrophoresis ◽  
Pharmaceutical Preparations ◽  
Effective Length ◽  
Relative Standard ◽  
Significant Difference ◽  
Zone Electrophoresis ◽  
Capillary Zone

A novel, quick, reliable and simple capillary zone electrophoresis CZE method was developed and validated for the simultaneous determination of sitagliptin (SG) and metformin (MF) in pharmaceutical preparations. Separation was carried out in fused silica capillary (50.0 cm total length and 43.0 cm effective length, 49 μm i.d.) by applying a potential of 15 KV (positive polarity) and a running buffer containing 60 mM phosphate buffer at pH 4.0 with UV detection at 203 nm. The samples were injected hydrodynamically for 3 s at 0.5 psi and the temperature of the capillary cartridge was kept at 25 °C. Phenformin was used as internal standard (IS). The method was suitably validated with respect to specificity, linearity, limit of detection and quantitation, accuracy, precision, and robustness. The method showed good linearity in the ranges of 10-100 μg/mL and 50-500 μg/mL with limits of detection of 0.49, 2.11 μm/mL and limits of quantification of 1.48, 6.39 μg/mL for SG and MF, respectively. The proposed method was successfully applied for the analysis of the studied drugs in their synthetic mixtures and co-formulated tablets without interfering peaks due to the excipients present in the pharmaceutical tablets. The method was further extended to the in-vitro determination of the two drugs in spiked human plasma. The estimated amounts of SG/MF were almost identical with the certified values, and their percentage relative standard deviation values (% R.S.D.) were found to be ≤1.50% (n = 3). The results were compared to a reference method reported in the literature and no significant difference was found statistically.

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