scholarly journals MICELLAR ENHANCED SYNCHRONOUS FLUORESCENCE FOR THE ASSAY OF SUMATRIPTAN SUCCINATE IN PHARMACEUTICAL TABLETS

2019 ◽  
pp. 218-223
Author(s):  
SAFWAN M. FRAIHAT
Keyword(s):  
Limit Of Detection ◽  
Fluorescence Emission ◽  
Reference Method ◽  
Synchronous Fluorescence ◽  
Pharmaceutical Tablets ◽  
Sumatriptan Succinate ◽  
Accuracy And Precision ◽  
Relative Standard ◽  
Wide Range

Objective: To develop a sensitive, fast and selective method for the determination of sumatriptan succinate (SUM) in pharmaceutical samples. Methods: The method is based on measuring the synchronous fluorescence of SUM using ∆λ of (120 nm) and at a wavelength of excitation and emission of 230 and 325 nm respectively, using Agilent Technology, Cary eclipse, G9800AA model Luminescence spectrometer. Effect of variables on fluorescence emission intensities was studied such as solvent, surfactant, and pH. The proposed method was validated in term of linearity, limit of detection as per the international conference on harmonization guidelines ICH Q2 (R1). Results: The linearity of the method was obtained with a wide range of (50-150) ng/ml with a high value of correlation coefficient value of (0.992). Limits of detection (LOD) and limits of quantitation (LOQ) were found to be 16.3 and 49.5 ng/ml respectively, the mean recovery was found to be 99.1% with low relative standard deviation (% RSD). The method was also compared statistically with the reference method using t-test and f-test, the results show no difference either in pure or pharmaceutical tablets. Conclusion: The obtained results revealed that the developed method can be applied successfully for the determination of SUM in drug formulations samples with good accuracy and precision.

scholarly journals Determination of Pantothenic Acid in Foods by Optical Biosensor Immunoassay

2005 ◽  
Vol 88 (4) ◽  
pp. 1008-1014 ◽  
Author(s):  
Simon A Haughey ◽  
Anthony A O'Kane ◽  
G Andrew Baxter ◽  
Andras Kalman ◽  
Marie-José Trisconi ◽  
...  
Keyword(s):  
Limit Of Detection ◽  
Extraction Procedure ◽  
Pantothenic Acid ◽  
Optical Biosensor ◽  
Liquid Chromatography Mass Spectrometry ◽  
Relative Standard ◽  
Wide Range ◽  
Simple Extraction ◽  
Reference Samples

Abstract An optical biosensor inhibition immunoassay was developed using a specific pantothenic acid-binding protein for the quantitation of free pantothenic acid (vitamin B5) in foodstuffs. Samples were prepared by a simple extraction procedure in buffer, and vitamin content was estimated against authentic calibrants in the same buffer. Performance parameters included a working range of 10–5000 ng/mL, a limit of detection of 4.4 ng/mL, precision relative standard deviation of 5.4–7.1% over a range of concentrations, and recoveries >95% in the matrixes tested. A wide range of foodstuffs, including National Institute of Standards and Technology reference samples, were tested in 3 independent laboratories and the results were compared with microbiological assay and liquid chromatography/mass spectrometry (LC/MS) methods. The results indicate that the biosensor technique is appropriate for the estimation of pantothenic acid in a wide range of foodstuffs.

scholarly journals Spectrophotometric Method for the Determination of Drugs Containing Phenol Group by Using 2, 4- Dinitrophenylhydrazine

2010 ◽  
Vol 7 (2) ◽  
pp. 395-402
Author(s):  
Padmarajaiah Nagaraja ◽  
Ashwinee Kumar Shrestha
Keyword(s):  
Standard Deviation ◽  
Spectrophotometric Method ◽  
Limit Of Detection ◽  
Dosage Forms ◽  
Limit Of Quantification ◽  
Pharmaceutical Dosage Forms ◽  
Accuracy And Precision ◽  
Relative Standard ◽  
Phenolic Drugs

A spectrophotometric method has been proposed for the determination of four phenolic drugs; salbutamol, ritodrine, amoxicillin and isoxsuprine. The method is based on the oxidation of 2, 4- dinitrophenyl-hydrazine and coupling of the oxidized product with drugs to give intensely colored chromogen. Under the proposed optimum condition, beer’s law was obeyed in the concentration range of 2.5-17, 2-29, 4-33 and 5-30 μg/mL for salbutamol, ritodrine, amoxicillin and isoxsuprine respectively. The limit of detection (LOD) and limit of quantification (LOQ) were 0.2, 0.83, 0.09, 0.84 μg/mL and 0.66, 2.79, 0.3 and 2.81 μg/mL in the same order. No interference was observed from common pharmaceutical adjuvants. The ringbom plots and low relative standard deviation assert the applicability of this method. The suggested method was further applied for the determinations of drugs in commercial pharmaceutical dosage forms, which was compared statistically with reference methods by means oft- test andF- test and were found not to differ significantly at 95% confidence level. The procedure is characterized by its simplicity with accuracy and precision.

scholarly journals DEVELOPMENT AND VALIDATION OF RP-HPLC METHOD FOR THE ESTIMATION OF ESCITALOPRAM OXALATE AND FLUPENTIXOL DIHYDROCHLORIDE IN COMBINED DOSAGE FORM AND PLASMA

2021 ◽  
pp. 61-66
Author(s):  
MALATHI SELLAPPAN ◽  
DARTHI DEVAKUMAR
Keyword(s):  
Mobile Phase ◽  
Dosage Form ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Accuracy And Precision ◽  
Relative Standard ◽  
Photodiode Array ◽  
Development And Validation ◽  
Potassium Dihydrogen Orthophosphate

Objective: The objective of the study was to develop a simple and rapid chromatographic method for quantification of escitalopram oxalate and flupentixol dihydrochloride in combined dosage form and plasma. Methods: The separation was achieved with a sun fire C8 [150×4.6 mm] 3.5 µm column with an isocratic mobile phase containing a mixture of potassium dihydrogen orthophosphate buffer: methanol: acetonitrile [30:60:10 v/v/v] pH adjusted to 11. The flow rate of the mobile phase was 1.5 ml/min with a Photodiode array [PDA] detection at 230 nm. Results: The HPLC method was developed and validated with respective linearity, accuracy, and precision, detection of limit, robustness, and specificity. The precision of the results stated as the relative standard deviation was below 2 %. The calibration curve was linear over a concentration range from 10-50 µg/ml for escitalopram oxalate and 1-5 µg/ml for flupentixol dihydrochloride with a correlation co-efficient 0.994 and 0.977 respectively. The accuracy of the method was demonstrated at levels in the range of 100 % and 120 % of the specification limit. The recovery of escitalopram oxalate and flupentixol dihydrochloride was found to be in the range of 90 % to 88 %, respectively. The lowest detection limits were found to be 2 µg/ml for escitalopram oxalate and 0.1 µg/ml for flupentixol dihydrochloride. The lowest quantification limits were found to be 5 µg/ml of escitalopram oxalate and 0.5 µg/ml of flupentixol dihydrochloride. Conclusion: The developed method was validated for linearity, accuracy, precision, the limit of detection and quantification, specificity. The method was applied successfully for the determination of escitalopram oxalate and flupentixol dihydrochloride in the combined dosage form and plasma.

scholarly journals Sensitive and selective spectrophotometric assay of doxycycline hyclate in pharmaceuticals using Folin-Ciocalteu reagent

2010 ◽  
Vol 60 (4) ◽  
pp. 445-454 ◽  
Author(s):  
Pavagada Ramesh ◽  
Kanakapura Basavaiah ◽  
Nagaraju Rajendraprasad
Keyword(s):  
Molar Absorptivity ◽  
Spectrophotometric Assay ◽  
Doxycycline Hyclate ◽  
Limit Of Quantification ◽  
Pharmaceutical Tablets ◽  
Bulk Powder ◽  
Accuracy And Precision ◽  
Relative Standard ◽  
Significant Difference

Sensitive and selective spectrophotometric assay of doxycycline hyclate in pharmaceuticals using Folin-Ciocalteu reagentA spectrophotometric method for the determination of doxycycline (DOX) is described. The method is based on the formation of blue colored chromogen due to reduction of tungstate and/or molybdate in Folin-Ciocalteu (F-C) reagent by DOX in alkaline medium. The colored species has an absorption maximum at 770 nm and the system obeys Beer's law over the concentration range 0.75-12.0 μg mL-1DOX. The apparent molar absorptivity is 2.78 × 104L mol-1cm-1. The limit of quantification and detection values are reported to be 0.20 and 0.08 μg mL-1, respectively. Over the linear range applicable, the accuracy and precision of the method were evaluated on intra-day and inter-day basis. The reported mean accuracy value was 101.0 ± 1.7 %, the relative error was ≤ 2.7 % and the relative standard deviation was ≤ 2.5 %. Application of the proposed method to bulk powder and commercial pharmaceutical tablets is also presented. No significant difference was obtained between the results of the proposed method and the official BP method. The procedure described in this paper is simple, rapid, accurate and precise.

scholarly journals Simple and extraction-free spectrophotometric methods for risperidone in pure form and in dosage forms

2013 ◽  
Vol 19 (1) ◽  
pp. 121-128 ◽  
Author(s):  
Hemavathi Deepakumari ◽  
Shiramahally Mallegowda ◽  
Kanakapura Vinay ◽  
Hosakere Revanasiddappa
Keyword(s):  
Limit Of Detection ◽  
Ion Pairs ◽  
Pharmaceutical Preparations ◽  
Reference Method ◽  
Standard Addition ◽  
Bromophenol Blue ◽  
Phenol Red ◽  
Spectrophotometric Methods ◽  
Accuracy And Precision

Two simple, sensitive and extraction-free spectrophotometric methods are described for the estimation of risperidone (RSP) in both pure and in pharmaceutical preparations. The proposed methods are based on the formation of ion-pair complex between RSP and the dyes, bromophenol blue (BPB) in method A and Phenol red (PR) in method B at room temperature to form yellow colored products which show maximum absorbance at 410 and at 400 nm in methods A and B, respectively. Beer's law was obeyed in the concentration range of 0.5-10 and 0.5-25 ?g mL-1 in methods A and B with apparent molar absorptivities of 3.43 ? 104 and 0.85 ? 104 L moL-1 cm-1, respectively. The limit of detection for method A is found to be 0.0056 and for method B is 0.132 ?g mL-1. The composition of the ion-pairs was established by Job?s method and it was found to be 1:1 for both the methods A and B. The proposed methods have been applied successfully to the determination of RSP in pharmaceutical preparations. The results were statistically compared with those of a reference method by applying the Student?s t-test and F-test. The methods developed were validated for accuracy and precision by performing recovery experiments via standard addition technique.

scholarly journals Improvements to a laser-induced fluorescence instrument for measuring SO<sub>2</sub> – impact on accuracy and precision

2021 ◽  
Vol 14 (3) ◽  
pp. 2429-2439
Author(s):  
Pamela S. Rickly ◽  
Lu Xu ◽  
John D. Crounse ◽  
Paul O. Wennberg ◽  
Andrew W. Rollins
Keyword(s):  
Limit Of Detection ◽  
Laser System ◽  
Fluorescence Emission ◽  
Laser Induced Fluorescence ◽  
Fluorescence Signal ◽  
Fluorescence Emission Spectrum ◽  
Signal Ratio ◽  
Accuracy And Precision ◽  
Aromatic Species

Abstract. This work describes key improvements made to the in situ laser-induced fluorescence instrument for measuring sulfur dioxide (SO2) that was originally described by Rollins et al. (2016). Here, we report measurements of the SO2 fluorescence emission spectrum. These measurements allow for the determination of the most appropriate bandpass filters to optimize the fluorescence signal, while reducing the instrumental background. Because many aromatic species fluoresce in the same spectral region as SO2, fluorescence spectra were also measured for naphthalene and anisole to determine if ambient SO2 measurements could be biased in the presence of such species. Improvement in the laser system resulted in better tunability, and a significant reduction in the 216.9 nm laser linewidth. This increases the online/offline signal ratio which, in turn, improves the precision and specificity of the measurement. The effects of these improvements on the instrumental sensitivity were determined by analyzing the signal and background of the instrument, using varying optical bandpass filter ranges and cell pressures and calculating the resulting limit of detection. As a result, we report an improvement to the instrumental sensitivity by as much as 50 %.

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 A Sensitive Spectrophotometric Estimation of Nimodipine in Tablets and Injection Using Phloroglucinol

2013 ◽  
Vol 2013 ◽  
pp. 1-7
Author(s):  
Hemavathi N. Deepakumari ◽  
Hosakere D. Revanasiddappa
Keyword(s):  
Azo Dye ◽  
Absorption Maximum ◽  
Reference Method ◽  
Molar Absorptivity ◽  
Ratio Test ◽  
Reaction Sequence ◽  
Accuracy And Precision ◽  
Relative Standard ◽  
Bulk Drug

A rapid, simple, and sensitive spectrophotometric method has been described for the determination of nimodipine in bulk drug, tablets, and injection. The proposed method is based on the diazotization of reduced nimodipine with nitrous acid followed by coupling with phloroglucinol to form colored azo dye and showing absorption maximum () at 410 nm. The formed colored azo dye is stable for about more than 2 h. The method obeyed Beer’s law over the concentration range of 0–25 μg/mL and the corresponding molar absorptivity value is  L/moL/cm. The Sandell sensitivity values limits of detection (LOD) and quantification (LOQ) values have also been reported for the developed method. The accuracy and precision of the method was evaluated on intra- and interday basis; the relative error (%RE) and the relative standard deviation (RSD) were <2.0%. All variables have been optimized and the presented reaction sequence was applied to the analysis of nimodipine in bulk drug, tablets, and injections. The performance of this method was evaluated in terms of Student’s -test and variance ratio -test to find out the significance of proposed method over the reference method.

Determination of patulin and hydroxymethylfurfural in beverages by UPLC-PDA

2020 ◽  
pp. 1-8
Author(s):  
M. Pernica ◽  
J. Martiník ◽  
R. Boško ◽  
V. Zušťáková ◽  
K. Benešová ◽  
...  
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
Penicillium Expansum ◽  
Limit Of Quantification ◽  
Accuracy And Precision ◽  
Relative Standard ◽  
Validation Parameters ◽  
Photodiode Array ◽  
Quantification Accuracy

The present study describes using molecularly imprinted polymer (MIP) technology for determination of patulin (PAT) and 5-hydroxymethylfurfural (5-HMF) in beverages by ultra-high performance liquid chromatography coupled to photodiode array (UPLC-PDA). PAT (4-hydroxy-4H-furo[3,2-c]pyran-2(6H)-one) is a mycotoxin produced by Penicillium fungi and Penicillium expansum is probably the most commonly encountered species that infects apples during their growth, harvest, storage or processing. The occurrence of PAT as a natural contaminant of apples is a worldwide problem. 5-HMF (also known as 5-(hydroxymethyl) furan-2-carbaldehyde), is formed in the Maillard reaction as well as during caramelisation. It is a good storage time-temperature marker and flavour indicator, especially in beverages such as wine, beer, but also cider and apple juice which may contain PAT. PAT and 5-HMF were separated within 2 min using a Luna Omega C18 column and the PDA detector wavelength was set to 276 nm. The validation parameters of the analytical method such as linearity, limit of detection, limit of quantification, accuracy and precision were tested. The calibration curves were linear at least in the range 50-1000 ng/ml with a good linearity (R2>0.999) for both analytes, the limit of detection and the limit of quantification for PAT and 5-HMF were in the range 4.9-6.6 and 16.1-21.8 μg/l, respectively. The recoveries of the selected analyte were in the range 61.9-109.0% with a precision of <8.2% (relative standard deviation (RSD)) for PAT and in the range 50.8-98.0% with a precision of <10.0% (RSD) for 5-HMF. The validated procedure was successfully applied for the analysis of PAT and 5-HMF in beverages from retail shops.

scholarly journals DEVELOPMENT AND VALIDATION OF DIFFERENTIAL PULSE POLAROGRAPHIC ANALYSIS OF FENOFIBRATE IN PURE AND PHARMACEUTICAL DOSAGE FORMS USING DROPPING MERCURY ELECTRODE

2016 ◽  
Vol 8 (10) ◽  
pp. 284
Author(s):  
Abdul Aziz Ramadan ◽  
Hasna Mandil ◽  
Reham Abu-saleh
Keyword(s):  
Limit Of Detection ◽  
Mercury Electrode ◽  
Reference Method ◽  
Differential Pulse ◽  
Dosage Forms ◽  
Pharmaceutical Dosage Forms ◽  
Polarographic Analysis ◽  
Relative Standard ◽  
Dropping Mercury Electrode

<p><strong>Objective: </strong>An easy, fast, accurate and sensitive differential pulse polarographic analysis for determination of fenofibrate (FEN) in pure and pharmaceutical dosage forms using dropping mercury electrode (DME) was applied.</p><p><strong>Methods: </strong>The method involves the electrochemical reduction of fenofibrate at DME by differential pulse polarographic analysis (DPPA). Different buffer solutions were used over a wide pH range (1.0–10.0). The best definition of the analytical signals was found in lithium perchlorate trihydrate buffer at pH 6.0 containing 24% (v/v) acetonitrile at-994 to-1025mV (versus Ag/AgCl).</p><p><strong>Results: </strong>Under optimized conditions the peak current (I<sub>p</sub>) is linear over the range 0.0361-3.608 μg/ml. The DPPA was used successfully for the determination of FEN in pure and pharmaceutical dosage forms. The relative standard deviation did not exceed 2.1% for the concentration of FEN 0.0361 μg/ml. Regression analysis showed a good correlation coefficient (R<sup>2</sup>= 0.9994) between Ip and concentration at the mentioned range. The limit of detection (LOD) and the limit of quantification (LOQ) was to be 0.0025 and 0.0076 μg/ml, respectively. The proposed method was validated for linearity, precision and accuracy, repeatability, sensitivity (LOD and LOQ), robustness and specificity with an average recovery of 99.8-100.6%.</p><p><strong>Conclusion: </strong>The developed method is applicable for the determination of FEN in pure and different dosage forms with the assay of marketed formulations 99.8-104.0% and the results are in good agreement with those obtained by square-wave voltammetry (SWV) reference method.</p><p><strong>Keywords: </strong>Differential pulse polarographic analysis, Fenofibrate, Pharmaceutical formulations</p>

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