scholarly journals A Terbium Sensitized Luminescence Method for the Assay of Flubiprofen in Pharmaceutical Formulations

2014 ◽  
Vol 19 (1) ◽  
pp. 54
Author(s):  
Salma M.Z. Al-Kindy ◽  
Arwa Al-Ghazali ◽  
Fakhr Eldin O. Suliman ◽  
Haidar A.J. Al-Lawati
Keyword(s):  
Limit Of Detection ◽  
Tap Water ◽  
Pharmaceutical Formulations ◽  
Aqueous System ◽  
Tween 20 ◽  
Luminescence Method ◽  
Time Resolved ◽  
Relative Standard ◽  
Excellent Reproducibility

A sensitive time-resolved luminescence method for the determination of flubiprofen (FLP) in methanol and in aqueous solution is described. The method is based on the luminescence sensitization of terbium (Tb3+ ) by the formation of a ternary complex with FLP in the presence of 4,7 diphenyl 1,10 phenanthroline (DPP) as co-ligand, and Tween-20 as surfactant. The signal for Tb-FLP-DPP was monitored at λex  = 285 nm and λem  = 552 nm. Optimum conditions for the formation of the complex in an aqueous system were TRIS buffer, pH 8.0, DPP (2.5Å~10−7  M), Tween-20 (0.30%) and 4Å~10-5  mol L-1  of Tb3+  which allowed the determination of 20–1000 ng mL-1  of FLP with a limit of detection (LOD) of 10 ng mL-1 . The relative standard deviations of the method ranged between 0.6 and 1.4% indicating excellent reproducibility of the method. The proposed method was successfully applied for the assays of FLP in pharmaceutical formulations and spiked tap water samples with average recoveries of 87% – 95%. 

scholarly journals DEVELOPMENT AND VALIDATION OF ULTRAVIOLET-SPECTROPHOTOMETRIC METHOD FOR DETERMINATION OF FEBUXOSTAT FOR CONDUCTING IN-VITRO QUALITY CONTROL TESTS IN BULK AND PHARMACEUTICAL DOSAGE FORMS

2018 ◽  
Vol 11 (9) ◽  
pp. 115
Author(s):  
Jaspreet Kaur ◽  
Daljit Kaur ◽  
Sukhmeet Singh
Keyword(s):  
Spectrophotometric Method ◽  
Limit Of Detection ◽  
Pharmaceutical Formulations ◽  
Dosage Forms ◽  
Pharmaceutical Dosage Forms ◽  
Relative Standard ◽  
Limit Of Quantitation ◽  
Development And Validation

Objective: A simple, accurate, and selective ultraviolet-spectrophotometric method has been developed for the estimation of febuxostat in the bulk and pharmaceutical dosage forms.Method: The method was developed and validated according to International Conference on Harmonization (ICH Q2 R1) guidelines. The developed method was validated statistically with respect to linearity, range, precision, accuracy, ruggedness, limit of detection (LOD), limit of quantitation (LOQ), and recovery. Specificity of the method was demonstrated by applying different stressed conditions to drug samples such as acid hydrolysis, alkaline hydrolysis, oxidative, photolytic, and thermal degradation.Results: The study was conducted using phosphate buffer pH 6.8 and λmax was found to be 312 nm. Standard plot having a concentration range of 1–10 μg/ml showed a good linear relationship with R2=0.999. The LOD and LOQ were found to be 0.118 μg/ml and 0.595 μg/ml, respectively. Recovery and percentage relative standard deviations were found to be 100.157±0.332% and <2%, respectively.Conclusion: Proposed method was successfully applicable to the pharmaceutical formulations containing febuxostat. Thus, the developed method is found to be simple, sensitive, accurate, precise, reproducible, and economical for the determination of febuxostat in pharmaceutical dosage forms.

scholarly journals Sensitive Determination of Terazosin in Pharmaceutical Formulations and Biological Samples by Ionic-Liquid Microextraction Prior to Spectrofluorimetry

2012 ◽  
Vol 2012 ◽  
pp. 1-7 ◽  
Author(s):  
Mohsen Zeeb ◽  
Mahdi Sadeghi
Keyword(s):  
Ionic Liquid ◽  
Ionic Strength ◽  
Biological Samples ◽  
Limit Of Detection ◽  
Pharmaceutical Formulations ◽  
Experimental Conditions ◽  
Relative Standard ◽  
Common Ion ◽  
Liquid Microextraction

An efficient and environmentally friendly sample preparation method based on the application of hydrophobic 1-Hexylpyridinium hexafluorophosphate [Hpy][PF6] ionic liquid (IL) as a microextraction solvent was proposed to preconcentrate terazosin. The performance of the microextraction method was improved by introducing a common ion of pyridinium IL into the sample solution. Due to the presence of the common ion, the solubility of IL significantly decreased. As a result, the phase separation successfully occurred even at high ionic strength, and the volume of the settled IL-phase was not influenced by variations in the ionic strength (up to 30% w/v). After preconcentration step, the enriched phase was introduced to the spectrofluorimeter for the determination of terazosin. The obtained results revealed that this system did not suffer from the limitations of that in conventional ionic-liquid microextraction. Under optimum experimental conditions, the proposed method provided a limit of detection (LOD) of 0.027 μg L−1and a relative standard deviation (R.S.D.) of 2.4%. The present method was successfully applied to terazosin determination in actual pharmaceutical formulations and biological samples. Considering the large variety of ionic liquids, the proposed microextraction method earns many merits, and will present a wide application in the future.

scholarly journals Rapid, Simple, and Sensitive Spectrofluorimetric Method for the Estimation of Ganciclovir in Bulk and Pharmaceutical Formulations

2013 ◽  
Vol 2013 ◽  
pp. 1-5 ◽  
Author(s):  
Garima Balwani ◽  
Emil Joseph ◽  
Satish Reddi ◽  
Vibhu Nagpal ◽  
Ranendra N. Saha
Keyword(s):  
Standard Deviation ◽  
Limit Of Detection ◽  
Pharmaceutical Formulations ◽  
Calibration Graph ◽  
Limit Of Quantification ◽  
Average Percentage ◽  
Ich Guidelines ◽  
Spectrofluorimetric Method ◽  
Relative Standard

A new, simple, rapid, sensitive, accurate, and affordable spectrofluorimetric method was developed and validated for the estimation of ganciclovir in bulk as well as in marketed formulations. The method was based on measuring the native fluorescence of ganciclovir in 0.2 M hydrochloric acid buffer of pH 1.2 at 374 nm after excitation at 257 nm. The calibration graph was found to be rectilinear in the concentration range of 0.25–2.00 μg mL−1. The limit of quantification and limit of detection were found to be 0.029 μg mL−1and 0.010μg mL−1, respectively. The method was fully validated for various parameters according to ICH guidelines. The results demonstrated that the procedure is accurate, precise, and reproducible (relative standard deviation <2%) and can be successfully applied for the determination of ganciclovir in its commercial capsules with average percentage recovery of 101.31 ± 0.90.

scholarly journals Simultaneous Determination of Aspirin and Rosuvastatin Calcium in Capsules by Using RP-HPLC Coupled with Photo Diode Array Detection

2014 ◽  
Vol 33 ◽  
pp. 218-230
Author(s):  
Ankita Panchal ◽  
Gaurav Sanghvi ◽  
Ashish Vachhani ◽  
Navin Sheth ◽  
Devendra Vaishnav
Keyword(s):  
Quality Control ◽  
Simultaneous Determination ◽  
Lower Limit ◽  
Limit Of Detection ◽  
Pharmaceutical Formulations ◽  
Coefficient Of Determination ◽  
Limit Of Quantification ◽  
Relative Standard ◽  
Rosuvastatin Calcium

A simple, sensitive, specific, and cost effective method for simultaneous determination of Aspirin and Rosuvastatin calcium was developed and validated in single dosage formulation. The sample solution of ASP and RSTC was prepared using methanol as a solvent. Separation of ASP and RSTC was achieved with a mobile phase consisting of 20 mM KH2PO4 : Methanol (30:70 v/v) at a flow rate of 1.0 ml/min. Separations were performed on Merck hibar 250-4.6 RP18 (5 µm) column (150 mm X 3.0 mm), using a Shimadzu Prominence HPLC system equipped with a Shimadzu SPD-20A detector, Rhenodyne 7725i injector with 20 μL loop, LC-20 AD pump, CBM-20 Alite controller and LC Solution software. Retention times of ASP and RSTC were 3.747 and 5.969 minutes respectively. Absolute recovery of ASP and RSTC was 100.3 and 100.03 % respectively. The lower limit of quantification (LLOQ) of ASP and RSTC was 0.3097 and 0.1063 ppm and lower limit of detection (LLOD) of ASP and RSTC was 0.01535 and 0.01358 ppm respectively. Linearity was established for the range of concentrations 15.00-90.0 μg/ml and 2.0-12.0 μg/ml for ASP and RSTC respectively with the coefficient of determination (R2) of 0.994 and 0.999 for both the compounds. The inter- and intra-day precision in the measurement of ASP quality control (QC) sample 75 μg/ml, were in the range 0.1-0.2 % relative standard deviation (R.S.D.) and 0.2-0.3 % R.S.D., respectively. The inter- and intra-day precision in the measurement of RST quality control (QC) sample 10 μg/ml, were in the range 0.1-0.2 % R.S.D., and 0.0-0.3 % R.S.D., respectively. The developed method would be applicable for routine quality control of ASP And RSTC in bulk as well as in pharmaceutical formulations

scholarly journals Voltammetric Determination of Captopril Using Chlorpromazine as a Homogeneous Mediator

2011 ◽  
Vol 2011 ◽  
pp. 1-6 ◽  
Author(s):  
Hossein Bahramipur ◽  
Fahimeh Jalali
Keyword(s):  
Electron Transfer ◽  
Limit Of Detection ◽  
Linear Sweep Voltammetry ◽  
Pharmaceutical Formulations ◽  
Electron Transfer Reaction ◽  
Linear Calibration ◽  
Serum Samples ◽  
Catalytic Rate Constant ◽  
Relative Standard

Chlorpromazine was used as a homogeneous electrocatalyst in the oxidation of captopril. The anodic peak current of chlorpromazine was increased substantially in the presence of low concentrations of captopril (pH 4). Cyclic voltammetry and chronoamperometry were used to study the kinetics of the catalytic electron transfer reaction. The values of electron transfer coefficient () and catalytic rate constant () were estimated to be 0.34 and , respectively. Linear sweep voltammetry was used for the determination of captopril in the presence of chlorpromazine. A linear calibration curve was obtained in the concentration range of captopril of 10.0–300.0 μM, with a limit of detection of 3.65 μM. The relative standard deviation (RSD%) for 5 replicate measurements of captopril (100 μM) was 1.96%. The method was applied to the determination of captopril in pharmaceutical formulations and blood serum samples with satisfactory results.

scholarly journals Direct Spectrophotometric Determination of Glimepiride in Pure Form And Pharmaceutical Formulations Using Bromocresol Purple

2018 ◽  
Vol 15 (2) ◽  
pp. 6186-6198
Author(s):  
Abdul Aziz Ramadan ◽  
Souad Zeino
Keyword(s):  
Limit Of Detection ◽  
Reference Method ◽  
Pharmaceutical Formulations ◽  
Molar Absorptivity ◽  
Bromocresol Purple ◽  
Reaction Conditions ◽  
Reagent Blank ◽  
Limit Of Quantification ◽  
Relative Standard

A simple, direct and accurate spectrophotometric method has been developed for the determination of Glimepiride (GLM) in pure and pharmaceutical formulations by complex formation with bromocresol purple (BCP). The method involves the formation of a yellow ion-pair complex between BCP with glimepiride at pH<3,8; after reacting GLM with Na2CO3 to give C24H33N4H+O5NaS which is extracted by chloroform. The formed complex [GLM]:[ BCP] was measured at lmax 418 nm against the reagent blank prepared in the same manner. Variables were studied in order to optimize the reaction conditions. Molar absorptivity (e) for complex was  20600  L.mol-1.cm-1. Beer’s law was obeyed in the concentration range of  1.226 – 46.608   mg.mL-1 in present of 5.0x10-4 mol/l of BCP with good correlation coefficient (R2= 0.9997). The relative standard deviation did not exceed 3.6%. The limit of detection (LOD) and the limit of quantification (LOQ) were 0.15 and 0.46 mg.mL-1, respectively. The proposed method was validated for specificity, linearity, precision and accuracy, repeatability, sensitivity (LOD and LOQ)  and robustness. The developed method is applicable for the determination of GLM in  pure and different dosage forms with average assay of 98.8 to 102.0% and the results are in good agreement with those obtained by the  RP-HPLC reference method.  

scholarly journals Ionophore-based potentiometric PVC membrane sensors for determination of phenobarbitone in pharmaceutical formulations

2016 ◽  
Vol 66 (4) ◽  
pp. 503-514 ◽  
Author(s):  
Haitham Alrabiah ◽  
Abdulrahman Al-Majed ◽  
Mohammed Abounassif ◽  
Gamal A.E. Mostafa
Keyword(s):  
Limit Of Detection ◽  
Pharmaceutical Formulations ◽  
Dioctyl Phthalate ◽  
Pvc Membrane ◽  
Relative Standard ◽  
The Mean ◽  
Ph Range ◽  
Foreign Species ◽  
Good Agreement

Abstract The fabrication and development of two polyvinyl chloride (PVC) membrane sensors for assaying phenobarbitone sodium are described. Sensors 1 and 2 were fabricated utilizing β- or γ-cyclodextrin as ionophore in the presence of tridodecylmethylammonium chloride as a membrane additive, and PVC and dioctyl phthalate as plasticizer. The analytical parameters of both sensors were evaluated according to the IUPAC guidelines. The proposed sensors showed rapid, stable anionic response (-59.1 and -62.0 mV per decade) over a relatively wide phenobarbitone concentration range (5.0 × 10-6-1 × 10-2 and 8 × 10-6-1 × 10-2 mol L-1) in the pH range of 9-11. The limit of detection was 3.5 × 10-6 and 7.0 × 10-6 mol L-1 for sensors 1 and 2, respectively. The fabricated sensors showed high selectivity for phenobarbitone over the investigated foreign species. An average recovery of 2.54 μg mL-1 phenobarbitone sodium was 97.4 and 101.1 %, while the mean relative standard deviation was 3.0 and 2.1 %, for sensors 1 and 2, respectively. The results acquired for determination of phenobarbitone in its dosage forms utilizing the proposed sensors are in good agreement with those obtained by the British Pharmacopoeial method.

scholarly journals Determination of the fenvalerate insecticide in natural waters by a photochemically-induced fluorescence method

2015 ◽  
Vol 34 (2) ◽  
pp. 245 ◽  
Author(s):  
Diène Diégane Thiaré ◽  
Atanasse Coly ◽  
Diégane Sarr ◽  
Abdourakhmane Khonté ◽  
Amadou Diop ◽  
...  
Keyword(s):  
Natural Waters ◽  
Sea Water ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Irradiation Time ◽  
Tap Water ◽  
Analytical Sensitivity ◽  
Photochemically Induced Fluorescence ◽  
Relative Standard

<p>The fenvalerate pyrethroid insecticide was determined in various types of natural waters of Senegal by means of a newly-developed, simple, rapid and very sensitive photochemically-induced fluorescence (PIF) method. The PIF method was optimized with respect to the irradiation time, solvent and pH. The obtained calibration curves yielded correlation coefficients very close to unity. The limit of detection (LOD) and of quantification (LOQ) values were very low (LOD = 0.01–0.66 ng/ml and LOQ = 0.04–2.20 ng/ml, according to the solvent), and the relative standard deviation (RSD) values were small, ranging between 0.1 and 1.5 %, which indicated a very good analytical sensitivity and a great repeatability of PIF. Recovery studies were performed on spiked distilled water, tap water, sea water, well water, river water and draining water samples of Senegal, using the liquid-liquid extraction (LLE), solid phase extraction (SPE), and standard addition procedures. Satisfactory recovery results (about 85–121%) were obtained for the determination of fenvalerate in an aquatic environment.</p>

Determination of musks and other fragrance compounds at ng/L levels using CLSA (closed loop stripping analysis) and GC/MS detection

2004 ◽  
Vol 50 (5) ◽  
pp. 119-123 ◽  
Author(s):  
D. Mitjans ◽  
F. Ventura
Keyword(s):  
Closed Loop ◽  
Matrix Effects ◽  
Limit Of Detection ◽  
Tap Water ◽  
Quality Parameters ◽  
Stripping Analysis ◽  
Polycyclic Musks ◽  
Relative Standard ◽  
High Resolution Gas Chromatography

Closed loop stripping analysis (CLSA), a suitable tool for the determination of volatile and semivolatile compounds at low trace levels (ng/l), has been used to determine and quantify seven selected musks and two fragrances (Acetyl cedrene and Amberonne). The obtained extracts are analyzed by high resolution gas chromatography coupled to mass spectrometry (GC/MS) operating in the SIM mode. Quality parameters such as limit of detection; matrix effects; precision expressed as repeatability and reproducibility relative standard deviations of the method and an estimation of the uncertainty have been evaluated. The method has been applied to the analysis of wastewater effluents, surface water and tap water from different places in Europe. All samples contained differents musks at ng/l levels with the polycyclic musks Galaxolide and Tonalide and both fragrances, Amberonne and Acetyl cedrene, being the most abundant. These results suggest the importance of studying and controlling the presence of these ubiquitous environmental compounds in water systems.

scholarly journals Simple UV Spectrophotometric Method for the Determination of Fluvastatin Sodium in Bulk and Pharmaceutical Formulations

2009 ◽  
Vol 6 (4) ◽  
pp. 1233-1239 ◽  
Author(s):  
J. Saminathan ◽  
A. S. Sankar ◽  
K. Anandakumar ◽  
T. Vetrichelvan
Keyword(s):  
Spectrophotometric Method ◽  
Limit Of Detection ◽  
Regression Line ◽  
Cost Effective ◽  
Pharmaceutical Formulations ◽  
Molar Absorptivity ◽  
Good Precision ◽  
Limit Of Quantification ◽  
Relative Standard

A simple and cost effective spectrophotometric method is described for the determination of fluvastatin sodium in pure form and in pharmaceutical formulations. When the drug reacts with sodium hydroxide shows absorption maximum at 304 nm and obeys beer's law in the concentration range 5-25 µg mL-1. The absorbance was found to increase linearly with increasing concentration of FVS, which is corroborated by the calculated correlation coefficient value of 0.9999 (n=5). The apparent molar absorptivity and sandell sensitivity were 1.1905×104and 0.0368844 µg cm-2cm respectively. The slope and intercept of the equation of the regression line are 0.027112 and 0.003539 respectively. The limit of detection and limit of quantification was found to be 0.0811 µg mL-1& 0.2460 µg mL-1. The validity of the described procedure was assessed. Statistical analysis of the result has been carried out revealing high accuracy and good precision. The proposed method was successfully applied to the determination of FVS in pharmaceutical formulations without any interference from common excipients. The relative standard deviations were ≤ 0.937%, with recoveries of 98.60% -101.70%.

Sign in / Sign up

Export Citation Format

Share Document