scholarly journals DEVELOPMENT AND VALIDATION OF A SPECTROPHOTOMETRIC METHOD TO EVALUATE BIOSAFETY CAPACITY OF BARU (Dipteryx alata) PEELS

2018 ◽  
Vol 15 (30) ◽  
pp. 221-240
Author(s):  
E. C. CESARINO ◽  
D. S. MULHOLLAND ◽  
W. FRANCISCO
Keyword(s):  
Contact Time ◽  
Limit Of Detection ◽  
Copper Ions ◽  
Maximum Adsorption Capacity ◽  
Limit Of Quantification ◽  
Experimental Conditions ◽  
Inorganic Matter ◽  
Pseudo Second Order ◽  
Development And Validation ◽  
Dipteryx Alata

This study developed a new analytical method using Molecular Absorption Spectroscopy (MAS) to track the ion cover in adsorption solution per peel (mesocarp) of Baru (Dipteryx alata). The adsorption study was conducted at different pH and contact time (kinetic), encountering 4.0 as the best pH for adsorption experimental conditions. The variation of contact time showed a pseudo-second-order adsorption kinetic behavior. The interpretation of the isotherms allowed to approach the Langmuir model with R² of 0.918 and to determine the maximum adsorption capacity (qmáx) as 11.481 mg.g⁻¹. The characterization of biomass by MAS in the Infrared (FT-IR) identified the possible functional groups belonging to protein, fatty acids and lipids, while thermal analysis (TG-DSC) showed a greater removal of inorganic matter by the biomass washed with water. The method underwent analytical validation, being classified as specific, sensitive, linear, robust, precise and accurate, with LD (limit of detection) and LQ (limit of quantification) equal to 3.873 and 12.912 mg.L⁻¹, respectively. The results obtained demonstrated the potential use of mesocarp Baru as a natural adsorbent for copper ions in solution, opening power for future expansion and improvement of the method.

scholarly journals The nature and kinetics of 2,4-dimethylphenol adsorption in aqueous solution on biochar derived from Sargassum boveanum macroalgae

2020 ◽  
Vol 69 (5) ◽  
pp. 438-452 ◽  
Author(s):  
Mazen K. Nazal ◽  
Durga Rao ◽  
Nabeel Abuzaid
Keyword(s):  
Aqueous Solution ◽  
Contact Time ◽  
Maximum Adsorption Capacity ◽  
Solution Ph ◽  
Experimental Conditions ◽  
Freundlich Model ◽  
Adsorptive Removal ◽  
Adsorbate Concentration ◽  
Pseudo Second Order ◽  
Kinetics Of

Abstract Many industries produce 2,4-dimethylphenol (DMP) compound in the wastewater which is persistent, toxic, and carcinogenic. Therefore, an adsorbent was prepared by carbonizing a dried Sargassum boveanum macroalgae. The prepared biosorbent was investigated for adsorptive removal of DMP from aqueous solution. After carbonization, the biochar derived from S. boveanum macroalgae (BCM) removed almost 100% of DMP adsorbate. Effects of contact time, solution pH, adsorbate concentration, adsorbent mass, and temperature have been studied. It has been found that, within the experimental conditions, the maximum adsorption capacity is 17 mg/g, rate of adsorption follows pseudo-second order kinetics and the adsorption isotherm experimental data fit the Freundlich model. The thermodynamic parameters were calculated and it has been found that the adsorption of DMP on BCM is endothermic and thermodynamically favorable, and in addition the surface of BCM adsorbent shows affinity to the DMP molecules. The BCM adsorbent has the capability to remove around 65% of DMP from high saline seawater contaminated with DMP. Moreover, the prepared BCM adsorbent was reusable for at least four times in seawater for removal of DMP contaminant.

scholarly journals Cr6+ adsorption by modified vermiculite

2020 ◽  
Author(s):  
Valeria Medoro ◽  
Celia Marcos Pascual ◽  
Giacomo Ferretti ◽  
Giulio Galamini ◽  
Massimo Coltorti
Keyword(s):  
Earth Sciences ◽  
Inductively Coupled Plasma ◽  
Contact Time ◽  
Second Order ◽  
Isotherm Models ◽  
Maximum Adsorption Capacity ◽  
Order Kinetic ◽  
Experimental Conditions ◽  
X Ray ◽  
Pseudo Second Order

<p><strong>Abstract</strong>: <strong>Cr<sup>6+</sup> adsorption by modified vermiculite</strong></p><p><strong> </strong></p><p>Valeria Medoro- University of Ferrara , Department of Physics and Earth Sciences, Italy</p><p>Celia Marcos Pascual-University of Oviedo, Department of Geology, Spain</p><p>Giacomo Ferretti- University of Ferrara , Department of Physics and Earth Sciences, Italy</p><p>Giulio Galamini- University of Ferrara , Department of Physics and Earth Sciences, Italy</p><p>Massimo Coltorti- University of Ferrara , Department of Physics and Earth Sciences, Italy</p><p> </p><p>This work aimed at investigating the adsorption of Cr<sup>6+</sup> in water by exfoliated vermiculite. The adsorbant tested in this experiment was a vermiculite (from China) which has been subjected to heating at 1000 °C for 1 minute, resulting in an exfoliated vermiculite.</p><p>Three effects were studied: 1) contact time; 2) initial concentracion of Cr<sup>6+</sup>; 3) adsorbent mass. Samples were analysed by X Ray Fluorescence (XRF), X Ray Diffraction (XRD) and the solutions with Inductively Coupled Plasma Mass Spectrometry (ICP-MS) to quantify the adsorbed Cr<sup>6+</sup> by the vermiculite.</p><p>Results from XRD diffraction showed a conversion of vermiculite into flogopite  after heating at 1000°C for 1 minute because of: 1) high content of potassium, 2) dehydration and 3) structural re-ordering; after the contact of vermiculite with Cr<sup>6+</sup>, the mineral structure did not change. The adsorption of Cr<sup>6+</sup> was studied by Langmuir, Freundlich and Dubinin-Kaganer-Radushkevich (DKR) isotherm models. DKR model, indicative of a cooperative process, described adsorption equilibrium better than the other two models and the maximum adsorption capacity obtained was of 2.81 mol/g. Kinetic was studied using pseudo-first and pseudo-second order kinetic models, with a better description of the process by pseudo-second order model with correlation coefficient almost unitary (R<sup>2</sup>=0.9984; other kinetic parameters were k<sub>2</sub>=0.0015 and the absorption initial rate of 0.2x10<sup>-8</sup> mg g<sup>-1</sup> h<sup>-1</sup>). </p><p>The present study demonstrates the effectiveness of modified vermiculite adsorbents for the treatment of hexavalent chromium-contaminated waters and that its adsorption depends on the experimental conditions (such as contact time, initial concentracion of Cr<sup>6+</sup> and adsorbent mass).</p>

scholarly journals Enhanced removal of cationic dye by eco-friendly activated biochar derived from rice straw

2020 ◽  
Vol 10 (1) ◽  
Author(s):  
A. I. Abd-Elhamid ◽  
Mohamed Emran ◽  
M. H. El-Sadek ◽  
Ahmed A. El-Shanshory ◽  
Hesham M. A. Soliman ◽  
...  
Keyword(s):  
Rice Straw ◽  
Contact Time ◽  
Ph Value ◽  
Active Material ◽  
Maximum Adsorption Capacity ◽  
Time Data ◽  
Experimental Conditions ◽  
Activated Biochar ◽  
Highly Active ◽  
Pseudo Second Order

AbstractThis report deals with converting the agriculture waste (rice straw) to environmental cleaner materials (biochar) using airless pyrolysis followed by eco-friendly activation. The biochar (p-Biochar) obtained after pyrolysis step (poorly active material) was activated using wet attrition method to give m-Biochar (highly active materials). The both p-Biochar and m-Biochar were characterized in detail and utilized for MB and CV dye removal from aqueous solution. Various parameters affecting the adsorption process such as dye concentration, adsorbent dose, contact time, temperature, NaCl dose and pH were investigated. The adsorption isotherm was well fitted using Langmuir isotherm, and the maximum adsorption capacity is 90.91 and 44.64 mg/g, for MB and CV dyes, respectively. The contact time data obtained showed that the two dyes were poorly adsorbed over p-Biochar. The equilibrium was reached quickly in 15 min for MB dye and 20 min for CV dye using the m-Biochar, and removal percent was 94.45 and 92.70% for MB and CV dyes, respectively. Moreover, the kinetic isotherm presented very well fitted by pseudo-second-order model. In addition, the adsorption percent increases with further increasing the pH value. Finally, we observed that m-Biochar highly adsorbs the MB dye compared with the CV dye over all experimental conditions.

Removal of Methylene Blue and Orange-G from Waste Water Using Magnetic Biochar

2015 ◽  
Vol 14 (04) ◽  
pp. 1550009 ◽  
Author(s):  
N. M. Mubarak ◽  
Y. T. Fo ◽  
Hikmat Said Al-Salim ◽  
J. N. Sahu ◽  
E. C. Abdullah ◽  
...  
Keyword(s):  
Methylene Blue ◽  
Contact Time ◽  
Agitation Speed ◽  
Adsorption Kinetic ◽  
Maximum Adsorption Capacity ◽  
Optimum Conditions ◽  
Magnetic Biochar ◽  
Design Expert ◽  
Orange G ◽  
Pseudo Second Order

The study on the removal of methylene blue (MB) and orange-G dyes using magnetic biochar derived from the empty fruit bunch (EFB) was carried out. Process parameters such as pH, adsorbent dosage, agitation speed and contact time were optimized using Design-Expert Software v.6.0.8. The statistical analysis reveals that the optimum conditions for the maximum adsorption of MB are at pH 2 and pH 10, dosage 1.0 g, and agitation speed and contact time of 125 rpm and 120 min respectively. While for orange-G, at pH 2, dosage 1.0 g, and agitation speed and contact time of 125 rpm and 120 min respectively. The maximum adsorption capacity of 31.25 mg/g and 32.36 mg/g for MB and orange-G respectively. The adsorption kinetic for both dyes obeyed pseudo-second order.

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.

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.

Development and Validation of the Analytical method for the estimation of a combination of 5-fluorouracil and Imiquimod by RP-HPLC

2021 ◽  
pp. 3313-3318
Author(s):  
Bhupender Tomar ◽  
Ankita Sharma ◽  
Inder Kumar ◽  
Sandeep Jain ◽  
Pallavi Ahirrao
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
High Performance Liquid Chromatographic ◽  
Simultaneous Estimation ◽  
Limit Of Quantification ◽  
Pharmaceutical Ingredients ◽  
Rp Hplc ◽  
Ich Guidelines ◽  
Development And Validation ◽  
Liquid Chromatographic

A simple, precise, and accurate reverse phase high performance liquid chromatographic method (RP-HPLC) was developed and validated for the estimation of the combination of 5- Fluorouracil (5-FU) and Imiquimod in active pharmaceutical ingredients (APIs). The method was carried out on Phenomenex C18 (250 × 4.6mm I.D., 5𝜇m) using isocratic elution mode. The mobile phase was used as Acetonitrile: 10mM potassium dihydrogen orthophosphate: triethylamine (40:59.9:0.1, v/v, pH 4.5 with orthophosphoric acid) and Water: ACN (50:50 v/v) was used as a diluent. The concentration of solvents was 1-20µg/ml and the volume of injection was 20µl with the flow rate of 1.2ml/min. The retention times for 5-FU and Imiquimod were found to be 1.9±0.5 and 6.6±0.5 min respectively. The absorption maxima of 5FU and Imiquimod were found 267nm and 227nm respectively. The method was validated as per ICH guidelines. All the data were found within the specified limits. The limit of detection (LOD) and limit of quantification (LOQ) of 5- Fluorouracil were found to be 0.015μg/mL and 0.048 μg/mL, respectively, and Imiquimod was found to be 0.078μg/mL and 0.237μg/mL, respectively. The method developed in the present study was found to be sensitive, specific, and precise and can be applied for the simultaneous estimation of 5-FU and Imiquimod.

High performance liquid chromatography (HPLC) method development and validation for the determination of flunixin: Animal plasma based study

2021 ◽  
pp. 1-11
Author(s):  
Sultan M. Alshahrani ◽  
John Mark Christensen
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Method Development ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Limit Of Quantification ◽  
Mobile Phases ◽  
Hplc Method Development ◽  
Development And Validation

This study was designed to develop and validate a simple and efficient high performance liquid chromatography (HPLC) method to determine flunixin concentrations in Asian elephant’s (Elephas maximus) plasma. Flunixin was administered orally at a dose of 0.8 mg/kg, and blood samples were collected. Flunixin extraction was performed by adding an equal amount of acetonitrile to plasma and centrifuging at 4500 rpm for 25 minutes. The supernatant was removed, and flunixin was analyzed using HPLC-UV detection. Two methods were developed and tested utilizing two different mobile phases either with or without adding methanol (ACN: H2O vs. ACN: H2O: MeOH). Both methods showed excellent linearity and reproducibility. The limit of detection was 0.05 ug/ml and limit of quantification was 0.1 ug/ml. the efficiency of flunixin recovery was maximized by the addition of methanol to mobile phase (ACN: H2O: MeOH as 50:30:20) at 95% in comparison to 23% without methanol. In conclusion, adding methanol to HPLC methods for extraction of flunixin from elephants’ plasma yielded higher recovery rate than without methanol.

scholarly journals DEVELOPMENT AND VALIDATION OF UV-SPECTROPHOTOMETRIC METHOD FOR ESTIMATION OF HYDROQUINONE IN BULK, MARKETED CREAM AND PREAPARED NLC FORMULATION

2017 ◽  
Vol 9 (5) ◽  
pp. 102
Author(s):  
Sukhjinder Kaur ◽  
Taranjit Kaur ◽  
Gurdeep Kaur ◽  
Shivani Verma
Keyword(s):  
Spectrophotometric Method ◽  
Limit Of Detection ◽  
Pharmaceutical Formulations ◽  
Pure Form ◽  
Nanostructured Lipid Carrier ◽  
Limit Of Quantification ◽  
Double Beam ◽  
Uv Visible ◽  
Development And Validation

Objective: The aim of the present work was to develop a simple, rapid, accurate and economical UV-visible spectrophotometric method for the determination of hydroquinone (HQ) in its pure form, marketed formulation as well as in the prepared nanostructured lipid carrier (NLC) systems and to validate the developed method.Methods: HQ was estimated at UV maxima of 289.6 nm in pH 5.5 phosphate buffer using UV-Visible double beam spectrophotometer. Following the guidelines of the International Conference on Harmonization (ICH), the method was validated for various analytical parameters like linearity, precision, and accuracy robustness, ruggedness, limit of detection, quantification limit, and formulation analysis.Results: The obtained results of the analysis were validated statistically. Recovery studies were performed to confirm the accuracy of the proposed method. In the developed method, linearity over the concentration range of 5-40 μg/ml of HQ was observed with the correlation coefficient of 0.998 and found in good agreement with Beer Lambert’s law. The precision (intra-day and inter-day) of the method was found within official RCD limits (RSD<2%).Conclusion: The sensitivity of the method was assessed by determining the limit of detection and limit of quantification. It could be concluded from the results obtained that the purposed method for estimation of HQ in pure form, in the marketed ointment and in the prepared NLC-formulation was simple, rapid, accurate, precise and economical. It can be used successfully in the quality control of pharmaceutical formulations and for the routine laboratory analysis.

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