scholarly journals Spectrofluorimetric determination of benidipine in pharmaceutical preparation and spiked plasma samples using 7-?uoro-4-nitrobenzo-2-oxa-1,3-diazole

2019 ◽  
Vol 23 (6) ◽  
pp. 1060-1066
Author(s):  
Cem ÖNAL ◽  
Şerife Evrim KEPEKÇİ TEKKELİ
Keyword(s):  
Pharmaceutical Preparation ◽  
Plasma Samples ◽  
Spiked Plasma ◽  
Spectrofluorimetric Determination

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.

scholarly journals Combining derivative and synchronous approaches for simultaneous spectrofluorimetric determination of terbinafine and itraconazole

2020 ◽  
Vol 7 (8) ◽  
pp. 200571
Author(s):  
Heba Elmansi ◽  
Aya Roshdy ◽  
Shereen Shalan ◽  
Amina El-Brashy
Keyword(s):  
Biological Samples ◽  
Concentration Level ◽  
Detection Limits ◽  
Plasma Samples ◽  
International Conference ◽  
Spiked Plasma ◽  
Spectrofluorimetric Determination ◽  
Good Agreement

In this study, determination of terbinafine and itraconazole down to biological concentration level has been carried out. The determination is based on increasing the selectivity of the spectrofluorimetric technique by combining both derivative and synchronous spectrofluorometric approaches, which permits successful estimation of terbinafine at 257 nm and itraconazole at 319 nm in the presence of each other at Δ λ of 60 nm. International Conference on Harmonization validation guidelines were followed to fully validate the method, and linearity was obtained for the two drugs over the range of 0.1–0.7 µg ml −1 for terbinafine and 0.5–4.0 µg ml −1 for itraconazole. Application of the method was successfully carried out in the commercial tablets with good agreement with the comparison spectrofluorometric methods. As the detection limits were down to 0.013 and 0.1 µg ml −1 and quantitation limits were 0.04 and 0.032 µg ml −1 for terbinafine and itraconazole, respectively; the in vitro determination of terbinafine and itraconazole in spiked plasma samples was applicable. The percentage recoveries in biological samples were 97.17 ± 4.54 and 98.75 ± 2.25 for terbinafine and itraconazole, respectively. Water was used as the optimum diluting solvent in the proposed methodology which adds an eco-friendly merit.

scholarly journals Spectrofluorimetric Determination of Warfarin Sodium by Using N1-Methylnicotinamide Chloride as a Fluorigenic Agent

2005 ◽  
Vol 88 (2) ◽  
pp. 455-461 ◽  
Author(s):  
Mohamed A El Dawy ◽  
Mokhtar M Mabrouk ◽  
Riad A El Barbary
Keyword(s):  
Aqueous Solutions ◽  
Human Plasma ◽  
Plasma Samples ◽  
Spiked Human Plasma ◽  
Human Plasma Samples ◽  
Warfarin Sodium ◽  
Spectrofluorimetric Method ◽  
Spectrofluorimetric Determination ◽  
Methylene Groups

Abstract A spectrofluorimetric method is described for the determination of drugs containing active methylene groups adjacent to carbonyl groups. The method was applied successfully to the determination of warfarin sodium in laboratory-prepared mixtures, in commercial tablets, and in spiked human plasma samples. Finally, the method was applied to the determination of the steady-state concentration of warfarin sodium in the blood of a hospitalized patient. The method involves the reaction of warfarin sodium with 0.2 ml (0.4 × 10−3M) N1-methylnicotinamide chloride reagent in the presence of 3 mL 1.0N NaOH and cooling in ice for 8 min, followed by adjustment of the pH to 2.0, using formic acid and heating for 4 min, whereby a highly fluorescent reaction product is produced. The optimal wavelengths of excitation and emission were determined by using a synchronous wavelength search and found to be 284 and 354 nm, respectively. The standard curves were linear over a concentration range of 50–1500 ng/mL in both aqueous solutions and spiked human plasma samples. The mean recoveries (± standard deviation) were 101.157 (±1.33) and 95.73 (±1.88%) for aqueous solutions and spiked human plasma samples, respectively. The method showed good specificity and precision. The proposed method is simple and economical because of its minimal instrumentation and chemicals requirements. Nevertheless, it is highly sensitive, specific, and reproducible. Accordingly, it is suitable for quality-control applications, drug monitoring, and bioavailability and bioequivalency studies.

scholarly journals Quality by Design–Applied Liquid Chromatography-Tandem Mass Spectrometry Determination of Enzalutamide Anti-Prostate Cancer Therapy Drug in Spiked Plasma Samples

2017 ◽  
Vol 12 ◽  
pp. 117739011772677 ◽  
Author(s):  
ASK Sankar ◽  
Shanmugasundaram Palani ◽  
Ravichandiran Velayudham
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Quality By Design ◽  
Tandem Mass ◽  
Plasma Samples ◽  
Chromatography Tandem Mass Spectrometry ◽  
Spiked Plasma ◽  
Liquid Chromatography Tandem Mass

This research article presents the Quality by Design (QbD)–finalised conditions for a method that uses liquid chromatography-tandem mass spectrometry for the determination of concentration of enzalutamide (ENZ), an atypical anticancer drug, in a drug formulation and in spiked plasma samples. Critical process attributes (CPA) considered to be the influential parameters in separation, identification, and quantification processes by ultrahigh-performance liquid chromatography-electrospray ionisation-tandem mass spectrometry (UHPLC-ESI-MS/MS) were organic content, buffer strength, pH modifier, flow rate, spray voltage, sheath gas, and auxiliary gas that alter critical analytical attributes, such as retention time (R1) and area (R2). These factors were evaluated first in a factorial design (Taguchi orthogonal array design) and then extensively in a central composite design (CCD) to zero-in on the mobile phase for the quantification of ENZ standard drug and along with its internal standard (ENZIS) in spiked plasma samples and in formulation. Pareto chart from initial factorial design (Taguchi orthogonal array design) model suggested which of the CPA factors should be given the weightage, that is, to be exhaustively analysed in the CCD and response surface analysis. The elaborated parameters proposed by World Health Organization were studied by method validation, ie, selectivity, linearity, accuracy, precision repeatability system-suitability tests, method robustness/ruggedness, sensitivity, and stability. The strategy followed gives an insight on the development of a robust QbD-compliant quantitative UHPLC-ESI-MS/MS method for ENZ drug containing plasma samples (spiked).

scholarly journals Spectrofluorimetric determination of amlodipine in human plasma without derivatization

2012 ◽  
Vol 48 (4) ◽  
pp. 719-725 ◽  
Author(s):  
Yucel Kadioglu ◽  
Murat Ozturk
Keyword(s):  
Channel Blocker ◽  
Limit Of Detection ◽  
Plasma Samples ◽  
Experimental Conditions ◽  
Spectrofluorimetric Method ◽  
Relative Standard ◽  
Limit Of Quantitation ◽  
Spectrofluorimetric Determination ◽  
Better Than

A rapid and sensitive spectrofluorimetric method was developed for the determination of amlodipine (AD), a calcium channel blocker, in the plasma. The type of solvent, the wavelength range, and the range of AD concentration were selected to optimize the experimental conditions. The calibration curves were linear (r² >0.997) in the concentration range of 0.1-12.5 ppm of AD. The limit of quantitation and limit of detection values for the method for plasma samples were 0.1 ppm and 0.07 ppm, respectively. The precision calculated as the relative standard deviation was less than 3.5%, and the accuracy (relative error) was better than 5.5% (n=6). The method developed in this study can be directly and easily applied for the determination of AD in the plasma without derivatization in plasma.

scholarly journals Spectrofluorimetric Determination of Acetaminophen with N-Bromosuccinimide

2005 ◽  
Vol 88 (6) ◽  
pp. 1626-1630 ◽  
Author(s):  
Hanaa M Abdel-Wadood ◽  
Niveen A Mohamed ◽  
Fardous A Mohamed
Keyword(s):  
Pharmaceutical Preparations ◽  
Interference Effects ◽  
Fluorescent Intensity ◽  
Selective Method ◽  
Average Recovery ◽  
Spiked Plasma ◽  
Spectrofluorimetric Determination ◽  
Lower Detection ◽  
Stability Time

Abstract A simple, sensitive, and selective method for determination of acetaminophen based on its oxidation using N-bromosuccinimide (NBS) to produce a highly fluorescent product. Optimization of reaction variables was carried out concerning NBS concentration, pH, temperature, reaction time, and stability time. Under optimal analytical conditions, the fluorescent intensity was measured at λemission. 442 nm (excitation at λ 330 nm). The linearity range is 120–800 ng/mL with lower detection limit of 33.6 ng/mL acetaminophen. The method was applied successfully to the determination of the compound in pharmaceutical preparations, with average recovery of 100.3 ± 2%. The method was also applied successfully to the determination of the drug in spiked plasma samples, with an average recovery of 101.2 ± 1%. Interference effects of some compounds, present in combination with acetaminophen, were studied and the tolerance limits of these compounds were determined.

scholarly journals Estimation of isatin in spiked plasma samples using high performance liquid chromatography

2013 ◽  
Vol 19 (4) ◽  
pp. 605-614
Author(s):  
Zeid Alothman ◽  
Masoom Siddiqui ◽  
Saikh Wabaidur
Keyword(s):  
High Performance ◽  
Degradation Products ◽  
Chromatographic Determination ◽  
Drug Formulation ◽  
Forced Degradation ◽  
Plasma Samples ◽  
Spiked Plasma ◽  
Forced Degradation Studies ◽  
Liquid Chromatographic

An isocratic analytical method based on liquid chromatographic determination with UV detection is described for the determination of isatin in spiked plasma and in its synthetic mixture. The separation of the isatin was achieved on betasil C-8 column using mobile phase consisting of a binary mixture of acetonitrile and buffer (Na2CO3 + NaHCO3). Linearity, accuracy and precision were found to be acceptable over the concentration range (5 - 150 mg/L). LOD and LOQ were found to be 1.09 mg/L and 3.3 mg/L, respectively. The developed LC method with UV-visible detection offers simplicity, selectivity, precision and accuracy. It produces a symmetric peak shape and reasonable retention time. No interference has been observed with the excipients found in the drug formulation. Forced degradation studies were also conducted on the isatin samples and the results shows that the newly developed method is able to determine the content of isatin in presence of its degradation products. The proposed method when applied to the determination of isatin in spiked plasma samples produced a recovery ranging from 96.0%-98.2%.

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