scholarly journals Determination of Pitavastatin Calcium by Analytical Spectrophotometry

2021 ◽  
Vol 18 ◽  
pp. 30-39
Author(s):  
Saad Antakli ◽  
Leon Nejem ◽  
Ahmad Kullah
Keyword(s):  
Limit Of Detection ◽  
Extraction Process ◽  
Pharmaceutical Formulation ◽  
Raw Material ◽  
Bromocresol Purple ◽  
Limit Of Quantification ◽  
Effect Of Solvents ◽  
Percent Recovery ◽  
Pitavastatin Calcium

Simple and rapid spectrophotometric method for the quantitative analysis of Pitavastatin calcium (PTV) in raw material and tablets pharmaceutical formulation has been described. The method is based on the formation of yellow ion-pair complex between Pitavastatin calcium and Bromocresol purple (BCP) in chloroform medium. Different parameters affecting the reaction such as: effect of solvents, stability, reagent concentration, correlation ratio, etc. were optimized. The formed complex was quantified spectrophotometrically at absorption maximum 405 nm. Linearity range was 2.20 - 35.23 µg/mL, regression analysis showed a good correlation coefficient R2 = 0.9991. The limit of detection (LOD) and limit of quantification (LOQ) were to be 0.367 µg/mL and 1.112 µg/mL respectively. The average percent recovery was found to be (100.62 – 101.14) % for Pitavastatin Calcium. This study was applied on Syrian pharmaceutical trademark: (PAVACRIUM 4 & Londalop). The method was successfully applied for the determination of Pitavastatin calcium in tablets pharmaceutical formulation. The proposed method is simple, direct, sensitive and do not require any extraction process. Thus, this method could be readily applicable for the quality control and routine analysis.

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.

Chlorobenzene. Determination in workplace air

2019 ◽  
Vol 35 (1(99)) ◽  
pp. 19-28
Author(s):  
Anna Jeżewska ◽  
Agnieszka Woźnica
Keyword(s):  
Occupational Exposure ◽  
Carbon Disulfide ◽  
Limit Of Detection ◽  
Skin Irritation ◽  
Raw Material ◽  
Good Precision ◽  
Limit Of Quantification ◽  
Selective Determination ◽  
Workplace Air

Chlorobenzene is a colorless, flammable liquid that has an almond-like odor. It is used in industry as a solvent: resins, paints and fats, raw material for the production of plastics, as well as for the production of phenol, aniline and nitrobenzene. Occupational exposure to chlorobenzene vapors can occur through inhalation, absorption through the skin or ingestion. Harmful if inhaled, causes skin irritation. Long-term exposure affects the central nervous system. The aim of this study was an amendment to the PN-Z-04022- 03:2001 withdrawn from the Polish set of standards, and validate method for determination concentrations of chlorobenzene in the workplace air in the range from 1/10 to 2 MAC values, in accordance with the requirements of the standard PN-EN 482. The study was performed using a gas chromatograph (GC) with a flame ionization detector (FID) equipped with a capillary column HP-5 (30 m x 0.32 mm, 0.25 μm). This method is based on the adsorption of chlorobenzene vapors on activated charcoal, desorption with carbon disulfide, and analyzed by GC-FID. Application of HP-5 column allows selective determination of chlorobenzene in a presence of carbon disulfide, aniline, phenol and nitrobenzene. The measurement range was 2.3 ÷ 46 mg/m3 for a 15 l air sample. Limit of detection: 6.75 ng/ml and limit of quantification: 20.25 ng/ml. Analytical method described in this paper enables selective determination of chlorobenzene in workplace atmosphere in presence of other solvents at concentrations from 2.3 mg/m3 (1/10 MAC value). The method is characterized by good precision and accuracy and meets the criteria for the performance of procedures for the measurement of chemical agents, listed in EN 482. The method may be used for the assessment of occupational exposure to chlorobenzene and the associated risk to workers’ health. The developed method of determining chlorobenzene has been recorded as an analytical procedure (see Appendix). This article discusses the problems of occupational safety and health, which are covered by health sciences and environmental engineering.

A VALIDATED SPECTROFLUORIMETRIC METHOD FOR DETERMINATION OF POLYSORBATE 80 FROM PHARMACEUTICAL FORMULATION

INDIAN DRUGS ◽  
2019 ◽  
Vol 56 (05) ◽  
pp. 24-29
Author(s):  
V. K Parmar ◽  
◽  
H. R. Brahmbhatt
Keyword(s):  
Fluorescence Intensity ◽  
Limit Of Detection ◽  
Ophthalmic Solution ◽  
Pharmaceutical Formulation ◽  
Ionic Surfactant ◽  
Polysorbate 80 ◽  
Limit Of Quantification ◽  
Spectrofluorimetric Method ◽  
Eosin B

A simple, rapid and sensitive spectrofluorimetric method has been developed and validated for the determination of the non-ionic surfactant, polysorbate 80, from pharmaceutical formulation. The proposed method is based on a fluorescence enhancement of the probe (eosin B dye) with addition of polysorbate 80. The eosin B concentration was optimised and found to be 4μg/mL. The fluorescence intensity was measured in a diluting solvent, citric acid buffer (pH 4.0) using excitation and emission wavelengths, 545 nm and 580 nm, respectively. The fluorescence intensity was found to be liner over a concentration range of 16-80 μg/mL of polysorbate 80 with a high correlation coefficient (r = 0.9990). The developed method was validated in terms of linearity, precision, accuracy, limit of detection and limit of quantification and specificity. The limit of detection and limit of quantification for polysorbate 80 were found to be 2 μg/mL and 16 μg/mL, respectively. The developed method was successfully applied for the determination of polysorbate 80 in ophthalmic solution and micro emulsion.

Application of a ternary complex of tungsten(VI) with 4-nitrocatechol and thiazolyl blue for extraction-spectrophotometric determination of tungsten

2006 ◽  
Vol 60 (4) ◽  
Author(s):  
V. Lekova ◽  
K. Gavazov ◽  
A. Dimitrov
Keyword(s):  
Limit Of Detection ◽  
Ion Association ◽  
Extraction Process ◽  
Chloroform Extract ◽  
Molar Absorptivity ◽  
Limit Of Quantification ◽  
Diphenyltetrazolium Bromide ◽  
Optimum Ph ◽  
Association Complex

AbstractA new ternary ion-association complex of tungsten(VI), 4-nitrocatechol (NC), and 3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyltetrazolium bromide (Thiazolyl Blue, MTT) was obtained and studied using an extraction-spectrophotometric method. The optimum pH, reagent concentrations, and extraction time were determined. The composition of the complex was found to be W(VI): NC: MTT = 1: 2: 2. The extraction process was investigated quantitatively and the key constants were calculated. The molar absorptivity of the chloroform extract at λmax = 415 nm was 2.8 × 104 dm3 mol−1 cm−1, and the Beer’s law was obeyed up to 8.8 μg cm−3 tungsten(IV). The limit of detection and limit of quantification were calculated to be 0.27 μg cm−3 and 0.92 μg cm−3, respectively. The effect of foreign ions and reagents was studied and a competitive method for determination of tungsten in products from ferrous metallurgy was developed. The residual standard deviation and the relative error were 0.53 % and 0.2 %, respectively.

scholarly journals A Validated HPTLC Densitometric Method for Quantitative Determination of Zanamivir in Bulk and Pharmaceutical Formulation

2018 ◽  
Vol 9 (2) ◽  
pp. 115-120 ◽  
Author(s):  
Mohammed Al Bratty ◽  
Safaa Fathy Saleh ◽  
Hassan Ahmad Alhazmi ◽  
Sadique Akhtar Javed ◽  
Adel Mohammed Ahmed ◽  
...  
Keyword(s):  
Quantitative Determination ◽  
High Performance ◽  
Limit Of Detection ◽  
Antiviral Agent ◽  
Pharmaceutical Formulation ◽  
Limit Of Quantification ◽  
Tlc Plates ◽  
Pure Drug ◽  
Hptlc Method

The main purpose of the present study was to develop and validate a high performance thin layer chromatographic (HPTLC) method for quantitative determination of an antiviral agent, zanamivir in pure drug and diskhaler powder formulation. Chromatography was performed on aluminum TLC plates pre-coated with silica gel 60F254, employing a mixture of chloroform:methanol:ammonia (9.5:3.2:0.2,v:v:v) as mobile phase. The TLC scanner was operated in the absorbance mode at a wavelength of 230 nm for evaluation of chromatograms. The system has given well resolved peak of zanamivir (Rf = 0.56). The linearity of the method was established in the range of 20-300 ng/spot; correlation coefficient (r) was 0.9995. The low values of limit of detection and limit of quantification (12.4 and 37.5 ng/spot, respectively) have demonstrated the sensitivity of the developed method. The reported method was precise in both intra-day as well as inter-day analysis; % RSD of peak area was found to be less than 2%, and has an accuracy within 100 ± 2%. The developed method has a potential to quantify zanamivir from its diskhaler formulation without any interference from other components. The applicability of the method was demonstrated by excellent recovery of analyte (99.8%) from diskhaler formulation. The current analytical method can be applied for routine analysis of zanamivir in pure form and pharmaceutical formulation in quality control laboratories. 

Development and Validation of UV-Spectrophotometric Methods for the Determination of Berberine in Polymeric Nanoparticles

2019 ◽  
Vol 11 (12) ◽  
pp. 1273-1278
Author(s):  
Md Ali Mujtaba
Keyword(s):  
Phosphate Buffer ◽  
Limit Of Detection ◽  
Polymeric Nanoparticles ◽  
Uv Spectroscopy ◽  
Pharmaceutical Formulation ◽  
Limit Of Quantification ◽  
Spectrophotometric Methods ◽  
Relative Standard ◽  
Development And Validation

A simple, specific, economic, accurate, and reproducible UV-spectrophotometric methods were developed and validated for the estimation of berberine (BRC) in bulk and pharmaceutical formulation. The λmax of BRC in 0.1 N hydrochloric acid (pH 1.2), phosphate buffer (pH 6.8), and water was found to be 346 nm, 343 nm and 260 nm respectively. Beer's law was obeyed in the concentration range of 5–30 μg/ml (R2 = 0.9698) in water, 5–25 μg/ml (R2 = 0.9991) in 0.1 N HCl buffer (pH 1.2) and 5–35 μg/ml (R2 = 0.9935) in phosphate buffer (pH 6.8). These methods were tested, and validated for various parameters such as linearity, precision, accuracy, specificity, limit of detection (LOD), and limit of quantification (LOQ) according to ICH guidelines. The method showed good reproducibility and recovery with percent relative standard deviation less than 2%. Moreover, the accuracy and precision obtained implied that UV spectroscopy can be a cheap, reliable, and less time consuming alternative for chromatographic analysis. The proposed methods were successfully applied for the determination of BRC in pharmaceutical formulation. The BRC estimated from the formulation was found to be well within limits (±5% of the labelled content of the formulations). The proposed methods are highly sensitive, precise, accurate, and can be employed for the routine analysis of berberine in bulks as well as in the commercial formulations.

scholarly journals Determination of Glibenclamide By Analytical Spectrophotometry

2021 ◽  
Vol 18 ◽  
pp. 40-48
Author(s):  
Saad Antakli ◽  
Leon Nejem ◽  
Monzer Alraii
Keyword(s):  
Quality Control ◽  
Regression Analysis ◽  
Spectrophotometric Method ◽  
Limit Of Detection ◽  
Correlation Coefficients ◽  
Extraction Process ◽  
Metformin Hydrochloride ◽  
Limit Of Quantification ◽  
First Derivative

Simple and rapid spectrophotometric method was developed and applied to determine Glibenclamide (GB) by zero spectrophotometric method and first derivative spectrophotometric method for determining of (GB) in the presence of Metformin hydrochloride (MET). Zero spectrophotometric (ZS) method was applied for the determination of (GB) at λmax = 300 nm. Linearity range was (4 – 360) μg/mL. Regression analysis showed a good correlation coefficients R2 = 0.99993. The limit of detection (LOD) and limit of quantification (LOQ) were to be 0.65 μg/mL and 2.31 μg/mL, respectively.  First derivative spectrophotometric (1DS) method was applied for the determination of (GB) in the presence (MET). (GB) was determined at 317 nm (1D317). Linearity ranges were (4 – 240) μg/mL for (GB). Regression analysis showed a good correlation coefficients R2 = 0.999914. The limit of detection (LOD) and limit of quantification (LOQ) were to be 0.60 μg/mL and 1.83 μg/mL for (GB). The proposed zero spectrophotometry method was applied to analysis individual (GB), and the derivative (1D317) method was applied to analysis (GB) individually or combined with (MET) in Syrian trademark drugs. The proposed method is simple, direct, sensitive and do not require any extraction process. Thus, this method could be readily applicable for the quality control and routine analysis.

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 Spectrophotometric determination of ranitidine hydrochloride (RNH) in pharmaceutical formulation using 9-fluorenylmethyl chloroformate (FMOC-Cl)

2018 ◽  
Vol 6 (6) ◽  
pp. 7-14
Author(s):  
Abdalla Ahmed Elbashir ◽  
Shahd Moutasim Merghani
Keyword(s):  
Quality Control ◽  
Absorption Maximum ◽  
Limit Of Detection ◽  
Pharmaceutical Formulation ◽  
Reaction Conditions ◽  
Limit Of Quantification ◽  
Ranitidine Hydrochloride ◽  
Ich Guidelines ◽  
Sensitive Spectrophotometric Method

A new, simple and sensitive spectrophotometric method is developed for the determination of ranitidine hydrochloride (RNH). The proposed method is based upon reaction of RNH with 9-fluorenylmethyl chloroformate (FMOC-Cl) in borate buffer of pH 8.0 producing an absorption maximum at 255 nm. All parameters required for the reaction conditions are investigated. Linearity is verified with a range of 2-16 μg/mL and is described by the regression equation y = 61129 x + 0.0354 with a correlation coefficient of 0.9998 (n = 7). The limit of detection (LOD) and the limit of quantification (LOQ) were calculated as per ICH guidelines and were found to be 0.2219 and 0.6724 μg/mL, respectively. The method was successfully applied for the determination of RNH in pharmaceutical formulation. Therefore, the method can be used for routine analysis of RNH in quality control laboratories.

scholarly journals Method Validation & Determination of Contamination (Pesticides) Scenario of Surface & Wastewater

2020 ◽  
Vol 2 (1) ◽  
pp. 17
Keyword(s):  
Surface Water ◽  
Method Validation ◽  
Limit Of Detection ◽  
Extraction Process ◽  
Treated Wastewater ◽  
Synthetic Pyrethroids ◽  
Limit Of Quantification ◽  
Validation Parameters ◽  
Wastewater Samples

Un-treated wastewater can contaminate surface water and harm huge amounts of life. Toxic compounds like pesticides in the wastewater can seriously disrupt aquatic ecosystems also, so there is a necessity to monitor their components. It is very important to determine these pesticides at trace levels in wastewater with an updated method. A modified liquid-liquid extraction process for micro-quantitative determination of multiclass multi-residues in surface wastewater samples of organo-chlorine (OCPs), organo-phosphorus (OPPs), synthetic pyrethroids and other pesticides by using GC-MS and GC-ECD has been established. The important method validation parameters, like the limit of detection and limit of quantification, linearity, accuracy, precision, specificity, were evaluated as per standard guidelines. The percent recovery ranged from 84.3 to 111, with an acceptable coefficient of variation (RSD) of 1.8 to 15.4%. The linearity showed a reliable range (0.995–0.999). Validated methods have been finally applied to field wastewater samples, and a significant number of water samples found to be contaminated with targeted pesticides. So, surface water pollution with special reference to pesticides has to be monitored on a regular basis has been discussed.

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