scholarly journals MULTIVARIATE CALIBRATION TECHNIQUE FOR THE SPECTROPHOTOMETRIC QUANTIFICATION OF IVERMECTIN IN PHARMACEUTICAL FORMULATION

2019 ◽  
pp. 444-451
Author(s):  
MADHAN S ◽  
KAVITHA J ◽  
LAKSHMI KS
Keyword(s):  
Multivariate Calibration ◽  
Limit Of Detection ◽  
Pharmaceutical Formulation ◽  
Regression Equations ◽  
Calibration Technique ◽  
Experimental Conditions ◽  
Pharmaceutical Dosage Form ◽  
Ich Guidelines ◽  
Relative Standard ◽  
Interday Precision

Objective: The present abstract makes the use of multivariate calibration technique for the quantification of ivermectin in pharmaceutical dosage form. Methods: Multivariate calibration technique is based on the use of linear regression equations, by correlating the relation between concentration and absorbance at seven different selected wavelengths. The λmax of ivermectin was found to be 245 nm. The results were treated statistically. This statistical approach gives optimum results by eliminating the fluctuations arising from the instrumental or experimental conditions. Results: The developed method was validated as per the ICH guidelines and was found to be simple, linear, accurate, precise, and reproducible. The method was found to be linear over a concentration range of 5–15 μg/mL with a correlation coefficient (r2) value of about 0.9998. The limit of detection and quantification were found to be 0.029 and 0.087 μg/mL, respectively. The percentage relative standard deviation for intraday and interday precision was found to be in the range of 0.473–1.373 and 0.301–1.617, respectively. The percentage recovery was found within the range of 97.60–101.80% w/w. Conclusion: The results evidence that a simple, linear, precise, accurate, sensitive, and reproducible multivariate calibration technique has been developed and validated for the quantification of ivermectin in bulk and pharmaceutical formulation.

scholarly journals Development and Validation of UV Spectrophotometric Method of Mesalamine Using Hydrotropic Solubilizing Agents

2021 ◽  
Vol 12 (3) ◽  
pp. 2291-2296
Author(s):  
Bhavani N. L. D. ◽  
Gowtham Reddy Cheruku ◽  
Bhargava Sri Harsha Polina ◽  
Dheeraj Kotagiri ◽  
Jnanendra Kumar Korukollu
Keyword(s):  
Method Development ◽  
Limit Of Detection ◽  
Regression Equations ◽  
Limit Of Quantification ◽  
Pharmaceutical Dosage Form ◽  
Technical Requirements ◽  
Ich Guidelines ◽  
Relative Standard ◽  
Method Development And Validation ◽  
Development And Validation

The work was proposed to discuss method development and validation of the drug Mesalamine by using hydrotropic solubilizing agents. An uncomplicated, accurate, and precise method was developed for the drug Mesalamine in bulk as well as Pharmaceutical dosage form. 5M Urea was used as the hydrotropic solubilizing agent to enhance the solubility of the drug. The maximum wavelength (ʎ max) for Mesalamine was found to be 241nm. The validation was performed as per International Council for Harmonization of Technical Requirements for Pharmaceuticals for Human Use (ICH) guidelines for Accuracy, linearity, precision, Limit of detection (LOD) and Limit of quantification (LOQ). Percentage recovery (%) of Mesalamine was ascertained to be between 95 to 98%. Linearity for Mesalamine was observed between 2-10 µg/ml. Regression equation y=0.0571x-0.0186, regression coefficient (r²) is 0.9996 for Mesalamine. Inter day and intraday precision were checked, % relative standard deviation values were less than 2 for both the methods. Limit of detection (LOD) and Limit of quantification (LOQ) values were derived using regression equations. LOD value was found to be 0.55 µg/ml. LOQ value was found to be 1.67 µg/ml. The assay of the marketed formulation was performed and the results of the assay were obtained by the proposed method. The results are in between 98-102%. So, the method developed was simple and economical that can be adopted for routine tests.

scholarly journals A Stability Indicating Assay Method Development and Validation for the Frovatriptan Succinate Monohydrate by Using UV: A Spectrophotometric Technique

2013 ◽  
Vol 2013 ◽  
pp. 1-6 ◽  
Author(s):  
Hitesh Verma ◽  
Surajpal Verma ◽  
Harmanpreet Singh
Keyword(s):  
Method Development ◽  
Limit Of Detection ◽  
Assay Method ◽  
Forced Degradation ◽  
Solution Stability ◽  
Limit Of Quantification ◽  
Experimental Conditions ◽  
Stability Indicating ◽  
Ich Guidelines ◽  
Relative Standard

A new simple, reliable, inexpensive, and accurate method was developed for the quantification of Frovatriptan Succinate Monohydrate in different physiological media at 244 nm in bulk and in tablet dosage forms. The developed method is an attempt to surpass the disadvantages associated with the reported methods, namely, less sensitive and tedious in usage for routine purposes. Beer’s law was followed over the range of 1.0 µg/mL to 4.5 µg/mL. Stability indicating assay method was developed and validated as per the ICH guidelines using various parameters, for example, accuracy, precision, limit of quantification, limit of detection, robustness, ruggedness, solution stability, recovery, forced degradation (hydrolysis, photo degradation, thermal degradation, and oxidation), and so forth. Percent relative standard deviation associated with all the parameters was less than 2, showing compliance with the acceptance criteria of ICH guidelines. The developed method was very sensitive as limit of quantification and limit of detection were found to be 0.025 µg/mL and 0.00625 µg/mL, respectively. Forced degradation studies of drug reveal good stability under the chosen experimental conditions.

scholarly journals UV Spectrophotometric Method Development and Validation of Esomeprazole in Bulk and Pharmaceutical Dosage Forms

2021 ◽  
Vol 12 (3) ◽  
pp. 2286-2290
Author(s):  
Gowtham Reddy Cheruku ◽  
Sai Laasya Mithinti ◽  
Purushotham Saidu
Keyword(s):  
Method Development ◽  
Limit Of Detection ◽  
Regression Equations ◽  
Limit Of Quantification ◽  
Pharmaceutical Dosage Form ◽  
Pharmaceutical Dosage Forms ◽  
Technical Requirements ◽  
Relative Standard ◽  
Method Development And Validation ◽  
Development And Validation

The work discusses method development and validation. An uncomplicated, accurate, and straightforward method was developed for the drug Esomeprazole in bulk as well as Pharmaceutical dosage form. NaOH was used as the solvent. The maximum wavelength (ʎ max) for Esomeprazole was found to be 305nm. The validation was performed as per International Council for Harmonization of Technical Requirements for Pharmaceuticals for Human Use (ICH) guidelines for Accuracy linearity, precision, Limit of Detection (LOD) and Limit of Quantification (LOQ). Esomeprazole's recovery percentage (%) was 100.20%, respectively. Linearity for Esomeprazole was observed between 5-25µg/ml, respectively. Regression equation y=0.0407x-0.0122, regression coefficient (r²) is 0.9963 for Esomeprazole. Inter day and intraday precision were checked, % relative standard deviation values were less than 2. The regression equations were used to derive the Limit of Detection (LOD) and Limit of Quantification (LOQ) values. LOD value was found to be 0.734 µg/mL and LOQ value was 2.224 µg/mL for Esomeprazole. The assay of the marketed formulation was performed, which was between 98-102%.  So the method developed was simple and economical that can be adopted for routine tests. 

scholarly journals Stability-indicating HPLC-DAD assay for simultaneous quantification of hydrocortisone 21 acetate, dexamethasone, and fluocinolone acetonide in cosmetics

2020 ◽  
Vol 18 (1) ◽  
pp. 962-973
Author(s):  
Saira Arif ◽  
Sadia Ata
Keyword(s):  
Mobile Phase ◽  
Limit Of Detection ◽  
Fluocinolone Acetonide ◽  
Internal Diameter ◽  
Forced Degradation ◽  
Specific Method ◽  
Regression Equations ◽  
Limit Of Quantification ◽  
Simultaneous Quantification ◽  
Relative Standard

AbstractA rapid and specific method was developed for simultaneous quantification of hydrocortisone 21 acetate (HCA), dexamethasone (DEX), and fluocinolone acetonide (FCA) in whitening cream formulations using reversed-phase high-performance liquid chromatography. The effect of the composition of the mobile phase, analysis temperature, and detection wavelength was investigated to optimize the separation of studied components. The analytes were finally well separated using ACE Excel 2, C18 AR column having 150 mm length, 3 mm internal diameter, and 2 µm particle size at 35°C using methanol with 1% formic acid and double-distilled deionized water in the ratio of 60:40 (v/v), respectively, as the mobile phase in isocratic mode. Ten microliters of sample were injected with a flow rate of 0.5 mL/min. The specificity, linearity, accuracy, precision, recovery, limit of detection (LOD), limit of quantification (LOQ), and robustness were determined to validate the method as per International Conference on Harmonization guidelines. All the analytes were simultaneously separated within 8 min, and observed retention times of HCA, DEX, and FCA were 4.5, 5.5, and 6.9 min, respectively. The proposed method showed good linearity with the correlation coefficient, R2 = 0.999 over the range of 1–150 µg/mL for all standards. The linear regression equations were y = 12.7x + 118.7 (r = 0.999) for HCA, y = 12.9x + 106.8 (r = 0.999) for DEX, and y = 12.9x + 96.8 (r = 0.999) for FCA. The LOD was 0.25, 0.20, and 0.08 µg/mL for HCA, FCA, and DEX and LOQ was 2.06, 1.83, and 1.55 µg/mL for HCA, FCA, and DEX, respectively. The recovery values of HCA, DEX, and FCA ranged from 100.7–101.3, 102.0–102.6, and 100.2–102.0%, respectively, and the relative standard deviation for precision (intra- and interday) was less than 2, which indicated repeatability and reproducibility. The novelty of the method was described by forced degradation experimentation of all analytes in the combined form under acidic, basic, oxidative, and thermal stress. The proposed method was found to be simple, rapid, and reliable for the simultaneous determination of HCA, DEX, and FCA in cosmetics.

scholarly journals Determination of cobalt in water samples by atomic absorption spectrometry after pre-concentration with a simple ionic liquid-based dispersive liquid-liquid micro-extraction methodology

2010 ◽  
Vol 8 (3) ◽  
pp. 617-625 ◽  
Author(s):  
Hossein Abdolmohammad-Zadeh ◽  
Elnaz Ebrahimzadeh
Keyword(s):  
Ionic Liquid ◽  
Atomic Absorption Spectrometry ◽  
Atomic Absorption ◽  
Water Samples ◽  
Limit Of Detection ◽  
Absorption Spectrometry ◽  
Experimental Conditions ◽  
Flame Atomic Absorption ◽  
Relative Standard

AbstractA rapid dispersive liquid-liquid micro-extraction (DLLME) methodology based on the application of 1-hexylpyridinium hexafluorophosphate [C6py][PF6] ionic liquid (IL) as an extractant solvent was applied for the pre-concentration of trace levels of cobalt prior to determination by flame atomic absorption spectrometry (FAAS). 1-Phenyl-3-methyl-4-benzoyl-5-pyrazolone (PMBP) was employed as a chelator forming a Co-PMBP complex to extract cobalt ions from aqueous solution into the fine droplets of [C6py][PF6]. Some effective factors that influence the micro-extraction efficiency include the pH, the PMBP concentration, the amount of ionic liquid, the ionic strength, the temperature and the centrifugation time which were investigated and optimized. In the optimum experimental conditions, the limit of detection (3s) and the enrichment factor were 0.70 µg L−1 and 60, respectively. The relative standard deviation (RSD) for six replicate determinations of 50 µg L−1 Co was 2.36%. The calibration graph using the pre-concentration system was linear at levels 2–166 µg L−1 with a correlation coefficient of 0.9982. The applicability of the proposed method was evaluated by the determination of trace amounts of cobalt in several water samples.

Method Development and Validation of Spectrophotometric Methods for The Estimation of Rizatriptan Benzoate in Pure and Pharmaceutical Dosage Form

2021 ◽  
pp. 6003-6006
Author(s):  
Pushpa Latha E. ◽  
Sailaja B.
Keyword(s):  
Dosage Form ◽  
Method Development ◽  
Limit Of Detection ◽  
Limit Of Quantification ◽  
Pharmaceutical Dosage Form ◽  
Rizatriptan Benzoate ◽  
Spectrophotometric Methods ◽  
Ich Guidelines ◽  
Development And Validation ◽  
Tablet Dosage

Analytical UV derivative spectrophotometric method was developed and validated to quantify Rizatriptan Benzoate in pure drug and tablet dosage form. Based on the spectrophotometric characteristics of Rizatriptan Benzoate, a signal of zero (225nm), first (216nm), second (237nm), third (233nm), fourth (231nm) order derivative spectra were found to be adequate for quantification. The methods obeyed Beer's law in the concentration range of (0.1-360µg/ml) with square correlation coefficient (r2) of 0.999. The mean percentage recovery was found to be 100.01 ± 0.075. As per ICH guidelines the results of the analysis were validated in terms of linearity, precision, accuracy, limit of detection and limit of quantification, and were found to be satisfactory.

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 Development and validation of novel RP-UPLC method for estimation of atropine sulphate in pharmaceutical dosage form

2013 ◽  
Vol 19 (3) ◽  
pp. 333-337 ◽  
Author(s):  
A.C. Arvadiya ◽  
P.P. Dahivelker
Keyword(s):  
Mobile Phase ◽  
Dosage Form ◽  
Limit Of Detection ◽  
Atropine Sulphate ◽  
Limit Of Quantification ◽  
Pharmaceutical Dosage Form ◽  
Column Temperature ◽  
Ich Guidelines ◽  
Development And Validation

A simple, precise, accurate, sensitive and repeatable RP-UPLC method was developed for quantitative determination of atropine sulphate in pharmaceutical dosage form. The method was developed by using C18 column Hiber HR Purospher Star (100mm?2.1mm id, 2?m particle size) as stationary phase with Phosphate Buffer: Acetonitrile (87:13, %v/v) as a mobile phase, pH was adjusted to 3.5 by ortho-phosphoric acid at a flow rate of 0.5 mL/min and column temperature maintained at 30?C. Quantification of eluted compound was achieved with PDA detector at 210 nm. Atropine sulphate followed linearity in concentration range of 2.5-17.5 ?g/mL with r2=0.9998 (n=6). Limit of detection (LOD) and limit of quantification (LOQ) values were 0.0033 and 0.0102 ?g/mL for atropine sulphate. The validation study is carried out as per International Conference on Harmonization (ICH) guidelines. This method was successfully applied for estimation of atropine sulphate in pharmaceutical formulation.

scholarly journals Use of Dispersive Liquid-Liquid Microextraction and UV-Vis Spectrophotometry for the Determination of Cadmium in Water Samples

2014 ◽  
Vol 2014 ◽  
pp. 1-4 ◽  
Author(s):  
J. Pérez-Outeiral ◽  
E. Millán ◽  
R. Garcia-Arrona
Keyword(s):  
Water Samples ◽  
Limit Of Detection ◽  
Experimental Conditions ◽  
Cadmium Determination ◽  
A Value ◽  
Relative Standard ◽  
Potential Applicability ◽  
Dispersive Liquid Liquid Microextraction ◽  
Liquid Microextraction

A simple and inexpensive method for cadmium determination in water using dispersive liquid-liquid microextraction and ultraviolet-visible spectrophotometry was developed. In order to obtain the best experimental conditions, experimental design was applied. Calibration was made in the range of 10–100 μg/L, obtaining good linearity (R2 = 0.9947). The obtained limit of detection based on calibration curve was 8.5 μg/L. Intra- and interday repeatability were checked at two levels, obtaining relative standard deviation values from 9.0 to 13.3%. The enrichment factor had a value of 73. Metal interferences were also checked and tolerable limits were evaluated. Finally, the method was applied to cadmium determination in real spiked water samples. Therefore, the method showed potential applicability for cadmium determination in highly contaminated liquid samples.

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