scholarly journals Development and Validation of an Automated Zone Fluidics-Based Sensor for In Vitro Dissolution Studies of Captopril Using Total Error Concept

Molecules ◽  
2021 ◽  
Vol 26 (4) ◽  
pp. 824
Author(s):  
Theano D. Karakosta ◽  
Paraskevas D. Tzanavaras ◽  
Constantinos K. Zacharis
Keyword(s):  
Limit Of Detection ◽  
Total Error ◽  
In Vitro Dissolution ◽  
Flow Conditions ◽  
Limit Of Quantification ◽  
Intermediate Precision ◽  
Tolerance Intervals ◽  
Dissolution Tests ◽  
Development And Validation

In the present research, a zone fluidics-based automated sensor for the analysis of captopril in in vitro dissolution samples is reported. Captopril is reacted under flow conditions with Ni(II) (10 mmol L−1) in alkaline medium (0.15% v/v NH3) to form a stable derivate, which is monitored spectrophotometrically at 340 nm. The chemical and instrumental parameters were carefully investigated and optimized. The validation of the developed method was performed in the range of 5 to 120% of the expected maximum concentration using the accuracy profiles as a graphical decision-making tool. The β-expectation tolerance intervals did not exceed the acceptance criteria of ±10%, which means that 95% of future results will be encompassed in the defined bias limits. The variation of the relative bias ranged between −2.3% and 3.5% and the RSD values for repeatability and intermediate precision were lower than 2.3% in all cases. The limit of detection (LOD), and the lower and the upper limit of quantification (LLOQ, ULOQ) were satisfactory and found to be 1%, 5% and 120% (corresponding to 0.6, 2.78 and 66.67 μg mL−1 in dissolution medium). The developed method was successfully applied for the analysis of captopril in dissolution tests of two commercially available batches.

scholarly journals Development and Validation of an Eco-friendly HPLC-UV-DAD Method for the Determination of Allopurinol in Pharmaceuticals with Application to In vitro Dissolution Studies

2021 ◽  
Vol 11 (5) ◽  
pp. 13089-13101
Keyword(s):  
Factorial Design ◽  
Matrix Effects ◽  
Dissolution Kinetics ◽  
In Vitro Dissolution ◽  
Dissolution Test ◽  
Dissolution Studies ◽  
Dissolution Tests ◽  
Development And Validation

In this study, a sustainable HPLC-UV-DAD method was developed and validated for the determination of allopurinol in tablets and optimization of the dissolution test using factorial design. The separation of the analyte from the sample matrix was achieved in 3.01 minutes in a C8 column (4.6 mm X 150 mm X 5 μm), using mobile phase 0.1 mol L-1 HCl (25%) + ethanol (50%) + ultrapure water (25%) by UV detection at 249 nm. The method presented satisfactory analytical parameters of validation (specificity, selectivity, linearity, stability, precision, accuracy, and robustness), showing no matrix effects. The dissolution test was optimized by complete factorial design 23 and, the optimal conditions were: HCl 0.001 mol L-1, apparatus II (paddle) and 75 rpm. The analytical procedures and dissolution tests were applied to allopurinol tablets marketed in Bahia, Brazil, to evaluate the dissolution studies. The pharmaceuticals had similar dissolution profiles and first-order dissolution kinetics. This new and sustainable HPLC-UV-DAD method is friendly to the environment and can be used for the routine pharmaceutical analysis of allopurinol in fixed dosage forms.

scholarly journals DEVELOPMENT AND EVALUATION OF NOVEL ESTIMATION TECHNIQUES FOR IN VITRO DISSOLUTION STUDY AND VALIDATION PROTOCOL FOR ESCITALOPRAM AS ANTIDEPRESSANT DRUG AND THEIR FORMULATION

2020 ◽  
pp. 55-61
Author(s):  
SHRIRAM H. BAIRAGI ◽  
R. S. GHOSH
Keyword(s):  
Limit Of Detection ◽  
Antidepressant Drug ◽  
Correlation Factor ◽  
In Vitro Dissolution ◽  
Linear Calibration ◽  
Limit Of Quantification ◽  
Minimum Concentration ◽  
Dissolution Study ◽  
Relative Standard

Objective: To develop and validate the RP-HPLC method and in vitro dissolution study for escitalopram as antidepressant drug and their formulation. Methods: The chromatographic separation was done by using a C-18, 150 mm column and a mobile phase consisting of phosphate buffer (40%) and acetonitrile HPLC grade (60%). Detection was carried out at 211 nm with a flow rate of 1 ml/min with an injection of 20 μl. The method was validated with different parameters such as linearity, precision, accuracy, robustness, and limit of detection (LOD), the limit of quantification (LOQ) according to ICH guidelines. Results: The linear calibration curve was obtained in the concentration range of 0-50 μg/ml and gave an average correlation factor 0.992. The retention time was observed at 2.96 min. The Minimum concentration level at which the analyte can be reliably detected (LOD) and quantified (LOQ) were found to be 0.03 and 0.09 µg/ml, respectively. The relative standard deviation of intra and the inter-day assay was found to be less than 2. The dissolution studies show moderate dissolution (23.4%) after 45 min, but it reaches a plateau after approximately 25 min. Conclusion: This method was found to be simple, rapid and economic with less run time. The validated parameters manifest the method is reliable, linear, accurate and precise as well as robust with minor variations in chromatographic parameters. Therefore, the developed method can be applied for both routine analysis and quality control assay and it could be a very powerful tool to investigate the stability of escitalopram.

scholarly journals Development and Validation of a Green Analytical Method for the Determination of Aspirin and Domperidone Bulk or Formulation Using UV and HPLC

2020 ◽  
Vol 10 (6) ◽  
pp. 49-56
Author(s):  
Sneha Jagnade ◽  
Pushpendra Soni ◽  
Lavakesh Kumar Omray
Keyword(s):  
Analytical Method ◽  
Method Development ◽  
Limit Of Detection ◽  
Research Work ◽  
Ultra Violet ◽  
Limit Of Quantification ◽  
Intermediate Precision ◽  
Rp Hplc ◽  
Development And Validation

The aim of present study was to investigate the development and validation of a green analytical method for the determination of aspirin and domperidone. Method Development and Validation for Estimation of Domperidone and Aspirin in bulk or formulation by using RP-HPLC. The RP-HPLC method was developed for estimation of Aspirin and Domperidone in synthetic mixture by isocratically using 10 mM KH2PO4: Acetonitrile (20:80) as mobile phase, Prontosil C-18 column (4.6 x 250 mm, 5μparticle size) column as stationary phase and chromatogram was recorded at 231 nm. Then developed method was validated by using various parameters such as, linearity, Range accuracy, precision repeatability, intermediate precision, robustness, limit of detection, limit of quantification. The proposed methods were found to be linear with correlation coefficient close to one. Precision was determined by repeatability, Intermediate precision and reproducibility of the drugs. The robustness of developed method was checked by changing in the deliberate variation in solvent. The result obtained shows the developed methods to be Cost effective, Rapid (Short retention time), Simple, Accurate (the value of SD and % RSD less than 2), Precise and can be successfully employed in the routine analysis of these drugs in bulk drug as well as in tablet dosage form. The Simplicity, Rapidly and Reproducibility of the proposed method completely fulfill the objective of this research work. Keywords: Asprin; Domperidone; HPLC; Ultra Violet; Validation

scholarly journals COMPARISON OF RP-HPLC AND UV SPECTROPHOTOMETRIC METHODS FOR ESTIMATION OF HALOPERIDOL IN PURE AND PHARMACEUTICAL FORMULATION

2018 ◽  
Vol 8 (5-s) ◽  
pp. 277-282 ◽  
Author(s):  
AK Jain ◽  
BK Dubey ◽  
D Basedia ◽  
S Dhakar ◽  
M Ahirwar ◽  
...  
Keyword(s):  
Limit Of Detection ◽  
Uv Spectroscopy ◽  
Pharmaceutical Formulation ◽  
In Vitro Dissolution ◽  
Uv Spectrophotometry ◽  
Limit Of Quantification ◽  
Spectrophotometric Methods ◽  
Rp Hplc ◽  
Relative Standard

An accurate, precise, sensitive and reproducible High-performance liquid chromatographic (HPLC) and UV spectrophotometric methods were developed and validated for the quantitative determination of haloperidol (HPD) in bulk drug and pharmaceutical formulation. Different analytical performance parameters such as linearity, precision, accuracy, specificity, limit of detection (LOD) and limit of quantification (LOQ) were determined according to International Conference on Harmonization ICH Q2B guidelines. The RP-HPLC method was developed by the isocratic technique on a reversed-phase Thermo C18 (250 × 4.6 mm, 5µm) column with mobile phase consisting of Methanol: Acetonitrile (50:50v/v) at flow rate of 1.0 ml/min. The retention time for HPD was 2.238±0.3min. The UV spectrophotometric determinations were performed at 244 nm using 80% methanol as a solvent. The linearity range for HPD was 5-25 μg/ml for both HPLC and UV method. The linearity of the calibration curves for each analyte in the desired concentration range was good (r2 >0.999) by both the HPLC and UV methods. The method showed good reproducibility and recovery with percent relative standard deviation less than 2%. Moreover, the accuracy and precision obtained with HPLC co-related well with the UV method which implied that UV spectroscopy can be a cheap, reliable and less time consuming alternative for chromatographic analysis. The proposed methods are highly sensitive, precise and accurate and hence successfully applied for determining the assay and in vitro dissolution of a marketed formulation. Keywords: HPLC, UV Spectrophotometry, Haloperidol, Pharmaceutical formulation, Method validation, Quantitative analysis

scholarly journals DEVELOPMENT AND VALIDATION OF AN RP-HPLC METHOD FOR THE DETERMINATION OF ULIPRISTAL ACETATE IN BULK AND PHARMACEUTICAL DOSAGE FORM

2021 ◽  
pp. 83-89
Author(s):  
SANATHOIBA SINGHA S ◽  
SREENIVAS RAO T
Keyword(s):  
Dosage Form ◽  
Limit Of Detection ◽  
Limit Of Quantification ◽  
Intermediate Precision ◽  
Pharmaceutical Dosage Form ◽  
Pharmaceutical Dosage Forms ◽  
Ulipristal Acetate ◽  
Relative Standard ◽  
Development And Validation

Objective: This work makes an attempt to establish a sensitive and accurate method for the development and validation of an analytical method for estimation of ulipristal acetate (UPA) in bulk and pharmaceutical dosage form. Methods: A mixture of 20 mM acetate buffer pH 3.7 and methanol in the ratio of 70:30 (v/v %) was used as the mobile phase. An xBridge™ C18 column (250 mm × 4.6 mm, 5μ) was used for the analysis at a flow rate of 1 ml/min, injection volume of 20 μl, run time of 15 min, and detection wavelength of 309 nm. The repeatability (within-day in triplicates) and intermediate precision (for 2 days) were carried out by six injections and the obtained results within and between the days of trials were expressed as percent relative standard deviation (% RSD). The linearity of the method was determined by the analysis of analyte concentration across a range of 10 μg/ml–60 μg/ml. Results: The % RSD values of precision studies were found to be below the accepted limit of 2%. The method was found to be linear with a correlation coefficient (R2) of 0.98. The method was also found to be accurate and robust with suitable values. Limit of detection (LOD) and limit of quantification (LOQ) of the method were found to be 0.371 μg/ml and 1.23 μg/ml, respectively. Conclusion: The results of analysis prove that this method can be used for the routine determination of UPA in bulk drug and in pharmaceutical dosage forms.

scholarly journals Development and Validation of RP-HPLC-PDA Method for the Analysis of Diclofenac Sodium in the In Vitro Transdermal Permeation Samples

2019 ◽  
Vol 9 (2) ◽  
pp. 212-216 ◽  
Author(s):  
Saisrianusha Valluru ◽  
Buchi N Nalluri
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
Skin Permeation ◽  
Diclofenac Sodium ◽  
Hplc Method ◽  
Limit Of Quantification ◽  
Validation Parameters ◽  
In Vitro Skin Permeation ◽  
Development And Validation

A new analytical method using high-performance liquid chromatography coupled with photo diode array detection was developed and validated for the quantification of Diclofenac (DIC) from in vitro skin permeation samples. Analysis was performed using a Phenomenex C18 column (150 x 4.6mm, 5µm) with 10mM ammonium acetate: Acetonitrile (62:38% v/v) as the mobile phase in isocratic mode and eluents were monitored at 276nm. DIC was eluted at 3.1min and showed a good linearity in the concentration range of 0.2-3µg/mL with a correlation coefficient >0.999. The validation parameters, such as specificity, linearity, accuracy and limit of detection, limit of quantification, precision, robustness fulfilled the regulatory requirements. The developed HPLC method was successfully used for the analysis of DIC in samples obtained from transdermal diffusate samples.

scholarly journals Development and Validation of UV Spectrophotometric Method For Determination of Bisoprolol Fumarate in Bulk and Pharmaceutical Dosage Forms

2017 ◽  
Vol 6 (5) ◽  
pp. 196-199 ◽  
Author(s):  
Shahinaz Mohammed ◽  
Mohammed Adam ◽  
Shaza Shantier
Keyword(s):  
Spectrophotometric Method ◽  
Limit Of Detection ◽  
Limit Of Quantification ◽  
Intermediate Precision ◽  
Pharmaceutical Dosage Forms ◽  
Ich Guidelines ◽  
Recovery Percentage ◽  
Development And Validation ◽  
Tablet Dosage

In this study a simple, accurate and precise UV- spectrophotometric method was developed for the estimation of bisoprolol fumarate (BF) in bulk and tablet dosage form. The method was based on measurement of absorbance of BF aqueous solution at 271nm. Validation was conducted in accordance to ICH guidelines. The calibration curve was linear in the concentration range 5-25 µg/mL with correlation coefficient not less than 0.9986. The limit of detection and limit of quantification were 0.22 μg/ml and 0.66 μg/ml, respectively. Intraday and intermediate precision of the developed method were reflected by the low RSD% values (1.19 and 0.854, respectively). The recovery percentage was 105.0 ± 1.3%, n=3. The proposed method was applied for the assay of BF in three different brands

scholarly journals Method Development and Validation for the Trace Level Quantification of Genotoxic Impurity Oseltamivir Phosphate Related Compound-a in Oseltamivir Phosphate Using LC-MS

2021 ◽  
Vol 37 (5) ◽  
pp. 1192-1198
Author(s):  
Pikkili Viswanath ◽  
Doddipalli Venkata Ramana Reddy ◽  
Nagaraju Chamarthi
Keyword(s):  
Method Development ◽  
Concentration Level ◽  
Limit Of Detection ◽  
Signal To Noise Ratio ◽  
Mass Analyzer ◽  
Limit Of Quantification ◽  
Intermediate Precision ◽  
Single Mass ◽  
Development And Validation ◽  
Oseltamivir Phosphate

A selective and sensitive method has been developed for the determination of ethyl-(3S,4R,5S)-4-acetamido-5-amino-2-azido-3-(pentan-3-yloxy)cyclohexanecarboxylate (OSPRC-A) by using liquid chromatography coupled with mass spectrometer with single mass analyzer (LC-MS).The method was developed by using column DEVELOSIL ODS-UG-5, (50×3.0 mm, 5.0 µm) with linearity range of 0.005% to 0.0151% which meets to quantification level of 150% range. The column oven temperature was maintained at 40ºC. The flow rate was set as 1.5 mL/min. Injection volume was 10 µL and the detection wavelength was 215 nm. The signal to noise ratio values obtained were found to be 4.79 at concentration level of 0.00015% for the limit of detection (LOD) and 13.46 at concentration level of 0.0005% for the limit of quantification (LOQ). The % recovery was found to be in between the range 80.0% to 101.32% at LOQ to 150% level. The result obtained in method precision and intermediate precision are found to be within the specification limit. The percentage RSD for the content of OSPRC-A of method precision was 4.26. The percentage RSD for the content of OSPRC-A for intermediate precision was 4.00. The sample prepared in analytical solution was found to be stable for 24 h. This method can be used for the identification of impurity, OSPRC-A in Oseltamivir phosphate drug substances in its manufacturing.

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.

scholarly journals Development and Validation of a Rapid RP-HPLC Method for the Estimation of Esmolol Hydrochloride in Bulk and Pharmaceutical Dosage Forms

2010 ◽  
Vol 7 (3) ◽  
pp. 807-812 ◽  
Author(s):  
Vanita Somasekhar ◽  
D. Gowri Sankar
Keyword(s):  
Limit Of Detection ◽  
Hplc Method ◽  
Detector Response ◽  
Reverse Phase Hplc ◽  
Limit Of Quantification ◽  
Pharmaceutical Dosage Forms ◽  
Rp Hplc ◽  
Accuracy And Precision ◽  
Development And Validation

A reverse phase HPLC method is described for the determination of esmolol hydrochloride in bulk and injections. Chromatography was carried on a C18column using a mixture of acetonitrile, 0.05 M sodium acetate buffer and glacial acetic acid (35:65:3 v/v/v) as the mobile phase at a flow rate of 1 mL/min with detection at 275 nm. The retention time of the drug was 4.76 min. The detector response was linear in the concentration of 1-50 μg/mL. The limit of detection and limit of quantification was 0.614 and 1.86 μg/mL respectively. The method was validated by determining its sensitivity, linearity, accuracy and precision. The proposed method is simple, economical, fast, accurate and precise and hence can be applied for routine quality control of esmolol hydrochloride in bulk and injections.

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