scholarly journals Development and validation of analytical methodology with focus on the qualification of powder mixers

2015 ◽  
Vol 51 (2) ◽  
pp. 273-284 ◽  
Author(s):  
Pedro de Freitas Fiorante ◽  
Rodrigo Dias Martins ◽  
Mauri Sergio Alves Palma
Keyword(s):  
Hydrochloric Acid ◽  
Ferric Oxide ◽  
Analytical Procedure ◽  
Maximum Deviation ◽  
Hydrochloric Acid Concentration ◽  
Intermediate Precision ◽  
Analytical Methodology ◽  
Relative Standard ◽  
Performance Qualification ◽  
The Stability

<p>This study aims at developing an analytical procedure capable of quantifying the ferric oxide present in the mixture of ferric oxide/lactose monohydrate (0.4% w/w). The analytical procedure was checked for specificity, linearity, precision (system repeatability, procedure repeatability and intermediate precision), accuracy, stability of solutions and robustness of the procedure. The concentration of Fe (III) was determined by spectrophotometry at 480 nm based on calibration curves. The specificity was verified. The linearity was obtained in the range of 11.2 to 16.8 µg of ferric oxide/mL. The relative standard deviation (RSD) of the system repeatability, procedure repeatability and intermediate precision, were not more than 2%. The RSD of the accuracy values were less than 0.75%. The stability of the samples was checked over a 24 hours assay. In the robustness evaluation, the wavelength and the concentration of hydrochloric acid varied. The maximum absorbance deviation due to wavelength variation was 0.14 percent, and the maximum deviation due to the hydrochloric acid concentration variation was 2.4%, indicating that the concentration of hydrochloric acid is critical to the analysis of ferric oxide. The procedure developed was validated and is suitable to the performance qualification of powder mixers.</p>

scholarly journals An assessment of methanolysis and other factors used in the analysis of carbohydrate-containing materials

1971 ◽  
Vol 125 (4) ◽  
pp. 1009-1018 ◽  
Author(s):  
R. E. Chambers ◽  
J. R. Clamp
Keyword(s):  
Hydrochloric Acid ◽  
Analytical Procedure ◽  
Internal Standard ◽  
Inorganic Contaminants ◽  
Rotary Evaporation ◽  
Silver Salts ◽  
Methanolic Hydrochloric Acid ◽  
Different Temperatures ◽  
The Stability ◽  
Analytical System

The stability of monosaccharides in methanolic hydrochloric acid of different strengths and at different temperatures was determined. They are generally stable for 24h in methanolic 1m- and 2m-hydrochloric acid at both 85°C and 100°C, but undergo considerable destruction in methanolic 4m- and 6m-hydrochloric acid at 100°C. Analysis of glycopeptides and oligosaccharides of known composition showed that release of carbohydrate was complete within 3h in methanolic 1m-hydrochloric acid at 85°C. Removal of methanolic hydrochloric acid by rotary evaporation resulted in considerable losses of monosaccharides, which could be prevented by prior neutralization. Methanolysis caused extensive de-N-acetylation of acetamidohexoses, so that a re-N-acetylation step is necessary in the analytical procedure. The addition of acetic anhydride for this purpose also prevented loss of internal standard by adsorption on the insoluble silver salts used in neutralization. Several trimethylsilylating agents were studied and suitable conditions are recommended. The effects on the analytical system of water and some common organic and inorganic contaminants are assessed.

scholarly journals RP-HPLC (STABILITY-INDICATING) BASED ASSAY METHOD FOR THE SIMULTANEOUS ESTIMATION OF DORAVIRINE, TENOFOVIR DISOPROXIL FUMARATE AND LAMIVUDINE

2021 ◽  
pp. 153-159
Author(s):  
V. L. N. BALAJI GUPTA TIRUVEEDHI ◽  
VENKATESWARA RAO BATTULA ◽  
KISHORE BABU BONIGE
Keyword(s):  
Tenofovir Disoproxil Fumarate ◽  
Uv Light ◽  
Volume Ratio ◽  
Assay Method ◽  
Simultaneous Estimation ◽  
Intermediate Precision ◽  
Stability Indicating ◽  
Rp Hplc ◽  
Relative Standard ◽  
The Stability

Objective: In this study, a RP-HPLC (stability-indicating) based assay method for the estimation of doravirine (DRV), tenofovir disoproxil fumarate (TFF) and lamivudine (LMV) simultaneously in the tablets was described. Methods: The simultaneous analysis of DRV, TFF and LMV was done with HPLC system (Agilent 1100 series) and Luna Phenomenex C18 (250 mm × 4.6 mm × 5 μ) column with isocratic mobile phase (35% volume ratio of methanol and 65% volume ratio of 20 mmol ammonium formate, pH 5). Validation of assay method was done on sensitivity, linearity, accuracy, selectivity, precision, robustness and specificity. Results: The calibration curves were linear through the range of 25-200 µg/ml for DRV and 75-600 µg/ml for TFF and LMV. The percent relative standard deviation for intraday variation/precision, interday variation/precision, intermediate precision/ruggedness and robustness were lower than 2%. The recovery of LMV (99.09-99.76%), TFF (99.10-99.41%) and DRV (98.65-99.28%) confirmed the good accuracy. The stability of LMV, TFF and DRV in 0.1N NaOH, 3% peroxide, 0.1 N HCl, UV light and dry heat of 60 °C was determined. Conclusion: The results have allowed the method to be implemented in the tablets to quantify DRV, TFF, and LMV.

Calcium/Copper alginate framework doped with CuO nano-particles as a novel adsorbent for micro-extraction of benzodiazepines from human serum

2020 ◽  
Vol 16 ◽  
Author(s):  
Nadereh Rahbar ◽  
Fatemeh Ahmadi ◽  
Zahra Ramezani ◽  
Masoumeh Nourani
Keyword(s):  
Human Serum ◽  
High Performance ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Nano Particles ◽  
Limit Of Quantification ◽  
Analytical Methodology ◽  
Fiber Fabrication ◽  
Relative Standard ◽  
Green Procedure

Background: Sample preparation is one of the most challenging phases in pharmaceutical analysis, especially in biological matrices, affecting the whole analytical methodology. Objective: In this study, a new Ca(II)/Cu(II)/alginate/CuO nanoparticles hydrogel fiber (CCACHF) was synthesized through a simple, green procedure and applied for fiber micro solid phase extraction (FMSPE) of diazepam (DIZ) and oxazepam (OXZ) as model drugs prior to high-performance liquid chromatography-UV detection (HPLC-UV). Methods: Composition and morphology of the prepared fiber were characterized and the effect of main parameters on the fiber fabrication and extraction efficiency have been studied and optimized. Results: In optimal conditions, calibration curves were linear ranging between 0.1–500 µg L−1 with regression coefficients of 0.9938 and 0.9968. Limit of detection (LOD) (S/N=3) and limit of quantification (LOQ) (S/N=10) of the technique for DIZ and OXZ were 0.03 to 0.1 µg L−1. Within-day and between-day relative standard deviations (RSDs) for DIZ and OXZ were 6.0–12.5% and 3.3–9.4%, respectively. Conclusion: The fabricated adsorbent has been substantially employed to extraction of selected benzo-diazepines (BZDs) from human serum real specimens and the obtained recoveries were also satisfactory (82.1-109.7%).

scholarly journals Development of TLC Chromatographic-Densitometric Procedure for Qualitative and Quantitative Analysis of Ceftobiprole

Processes ◽  
2021 ◽  
Vol 9 (4) ◽  
pp. 708
Author(s):  
Żaneta Binert-Kusztal ◽  
Małgorzata Starek ◽  
Joanna Żandarek ◽  
Monika Dąbrowska
Keyword(s):  
High Sensitivity ◽  
Biologically Active ◽  
Fifth Generation ◽  
Ich Guidelines ◽  
Relative Standard ◽  
Lipophilicity Parameter ◽  
Alkaline Environments ◽  
Acetic Acid Water ◽  
Cephalosporin Antibiotics ◽  
The Stability

Currently, there is still a need for broad-spectrum antibiotics. The new cephalosporin antibiotics include, among others, ceftobiprole, a fifth-generation gram-positive cephalosporin, active against Staphylococcus aureus methicillin agonist (MRSA). The main focus of the work was to optimize the conditions of ceftobiprole qualitative determination and to validate the developed procedure according to ICH guidelines. As a result of the optimization process, HPTLC Cellulose chromatographic plates as a stationary phase and a mixture consisting of ethanol:2-propanol: glacial acetic acid: water (4:4:1:3, v/v/v/v) as a mobile phase were chosen. The densitometric detection was carried out at maximum absorbance of ceftobiprole (λ = 232 nm). Next, the validation process of the developed procedure was carried out. The relative standard deviation (RSD) for precision was less than 1.65%, which proves the high compatibility of the results, as well as the LOD = 0.0257 µg/spot and LOQ = 0.0779 µg/spot values, which also confirm the high sensitivity of the procedure. The usefulness of the developed method for the stability studies of ceftobiprole was analyzed. Study was carried out under stress conditions, i.e., acid and alkaline environments, exposure to radiation imitating sunlight and high temperature (40–60 °C). It was found that cefotbiprole is unstable in an alkaline environment and during exposure to UV-VIS radiation. Moreover, the lipophilicity parameter, as a main physicochemical property of the biologically active compound, was determined using experimental and computational methods.

scholarly journals Quantitative analysis of doxorubicin hydrochloride and arterolane maleate by mid IR spectroscopy using transmission and reflectance modes

BMC Chemistry ◽  
2021 ◽  
Vol 15 (1) ◽  
Author(s):  
Ranju Bansal ◽  
Ranjit Singh ◽  
Khushpal Kaur
Keyword(s):  
Quantitative Analysis ◽  
Spectroscopic Methods ◽  
Doxorubicin Hydrochloride ◽  
Intermediate Precision ◽  
Solid Dosage ◽  
Ich Guidelines ◽  
Relative Standard ◽  
Ft Ir ◽  
Solid Bulk ◽  
Ir Spectroscopic

Abstract Background Environment-friendly fast and accurate mid-infrared spectroscopic methods have been developed for the quantitative analysis of doxorubicin hydrochloride (DOX) and arterolane maleate (ALM) in bulk and marketed formulations. Both transmittance and reflectance modes have been used for the analysis and a comparison has been drawn for better accuracy. The analytical methods were validated in accordance with International Council for Harmonisation (ICH) guidelines Results The proposed methods have been successfully developed and validated for the quantification of doxorubicin and arterolane maleate in solid bulk and dosage form. High recovery values in both the modes, while analysing DOX and ALM, indicated good accuracy of the methods. The methods showed excellent repeatability and intermediate precision [% RSD (Relative Standard Deviation < 2.0%]. The assay values of the drugs in solid dosage forms were also found close to the labelled claim. Conclusion The proposed Fourier transform infrared (FT-IR) spectroscopic methods were found to be specific, reproducible, valid and could be used as general methods for the quantification of most of the solid drug preparations such as tablets, capsules and powders.

Surface Morphology and the Adsorptive Behavior of Coconut Active Carbon

2013 ◽  
Vol 690-693 ◽  
pp. 1029-1032
Author(s):  
Xiao Qiang Li ◽  
Li Juan Lan
Keyword(s):  
Electron Microscopy ◽  
Scanning Electron Microscopy ◽  
Hydrochloric Acid ◽  
Active Carbon ◽  
Adsorption Process ◽  
Hydrochloric Acid Concentration ◽  
Impregnation Method ◽  
Adsorption Experiment ◽  
Adsorptive Behavior ◽  
Scanning Electron

Active carbon modified by hydrochloric acid was prepared with impregnation method. The synthesized material was characterized by scanning electron microscopy. It was proved that plenty of pores with diameter of about 5-10μm were exist on the surface of active carbon. The adsorption process with toluene was performed over the modified active carbon to investigate the adsorptive efficiency. For comparison, other porous materials were also performed the adsorption experiment. The results showed that active carbon modified by hydrochloric acid has high adsorptive efficiency for toluene. The results proved that adsorptive performance of active carbon increased with the hydrochloric acid concentration.

Experimental Study on Concentrating Scandium by Leaching from Associated Scandium Ore

2013 ◽  
Vol 734-737 ◽  
pp. 1033-1036
Author(s):  
Gui Fang Zhang ◽  
Peng Yan ◽  
Qing Rong Yang
Keyword(s):  
Experimental Study ◽  
Particle Size ◽  
Hydrochloric Acid ◽  
Acid Concentration ◽  
Hydrochloric Acid Concentration ◽  
Leaching Rate ◽  
Optimal Conditions ◽  
Research Results ◽  
Solid Ratio ◽  
Leaching Residue

Based on the benefication of the complex silicate ore containing scandium, the research about aid-leaching agent used in the leaching of the scandium concentrate was been conducted. And the suitable leaching agent and aid-leaching agent which the useful ions entered into leaching liquid and the harmful ions were kept in leaching residue were been found according to the experiment results. For the scandium of sample existed various complex silicate ore as isomorphism form, the research has adopted hydrochloric acid with aid-leaching agent to dissociate the silicate ore and make scandium entering into solution. The research results has shown that the scandium leaching rate could reach 92.06% under the optimal conditions which the hydrochloric acid concentration is 22.8%, the dosage of aid leaching agent is 6%, liquid solid ratio is 4:1, particle size of leaching material totally is less than 0.15mm and leaching time is 8h.

Effects of high hydrochloric acid concentration on aniline chemical polymerization

Polymer ◽  
1997 ◽  
Vol 38 (20) ◽  
pp. 5247-5250 ◽  
Author(s):  
Gustavo M. Morales ◽  
Marcos Llusa ◽  
Maria C. Miras ◽  
Cesar Barbero
Keyword(s):  
Hydrochloric Acid ◽  
Acid Concentration ◽  
Hydrochloric Acid Concentration ◽  
Chemical Polymerization

scholarly journals Analysis of Mercury in Skin Lightening Cream by Microwave Plasma Atomic Emission Spectroscopy (MP-AES)

Molecules ◽  
2021 ◽  
Vol 26 (11) ◽  
pp. 3130
Author(s):  
Hardoko I. Qudus ◽  
Purwadi Purwadi ◽  
Iis Holilah ◽  
Sutopo Hadi
Keyword(s):  
Emission Spectroscopy ◽  
Microwave Plasma ◽  
Atomic Emission ◽  
Atomic Emission Spectroscopy ◽  
Solution Stability ◽  
Analysis Method ◽  
Plasma Atomic Emission ◽  
Relative Standard ◽  
The Stability ◽  
Skin Lightening

This research aimed at developing an analysis method, which was optimized and validated to determine the content of mercury in skin lightening cream discovered in the market in Bandar Lampung, Indonesia, through the use of microwave plasma atomic emission spectroscopy (MP-AES). The optimization on the analysis method was conducted on pump rate, viewing position, and reductant concentration in order to obtain the highest mercury emission intensity, while the solution stability was optimized to know the stability of mercury in the solution. The result showed that the method developed had precision with a relative standard deviation of 2.67%, recovery value of 92.78%, and linearity with an r value of 0.993, respectively. The sensitivity of the instrument detection had a limit of analysis method detection and quantification of 0.59 and 1.98 µg/L, respectively. The results of the test of the lightening cream (8 of 16 samples) positively contained mercury in the range of 422.61–44,960.79 ng/g. Therefore the method of analysis developed may be used for routine analysis of chemicals in any cosmetics products.

scholarly journals Spectrofluorometric determination of L-tryptophan in canary (Canarium indicum L.) seed protein hydrolysate

2019 ◽  
Vol 10 (1) ◽  
pp. 4780-4785
Keyword(s):  
Protein Hydrolysate ◽  
Intermediate Precision ◽  
North Sulawesi ◽  
Accuracy Test ◽  
Spectrofluorometric Determination ◽  
Relative Standard ◽  
Indigenous Plant ◽  
Assay Precision ◽  
Specific Reagent

Canary (Canarium indicum L.) is an indigenous plant of Indonesia, which mainly grows in the eastern part of Indonesia, especially in the Maluku, North Sulawesi, and Seram islands. We believe that no scientific reports have been conducted about L-tryptophan content in Canarium indicum. Therefore, this study was conducted to determine the presence and quantitate the aromatic amino acid (L-tryptophan) in the canary protein hydrolysate by the spectrofluorometric method. The protein hydrolysate was prepared by two hydrolysis methods, enzymatic and alkaline hydrolysis. L-tryptophan can be differentiated from tyrosine directly without using any reagent by excitation of the sample at 295 nm in order to avoid tyrosine emission. The equation of calibration curve correlation using standard in the range 0.5-5 ppm was y = 6632.3x - 845.42 and correlation coefficient of 0.9997, while the coefficient of variance in linear regression was 1.29%. The detection limit and quantification limit obtained were 0.116 ppm and 0.35 ppm respectively. The recoveries of the accuracy test were obtained in the range of 95-96%. The relative standard deviation of intra-assay precision tests were obtained in the range of 0.5-1.8%, while the intermediate precision in the range of 2.18-3.74%. L-tryptophan was detected in all samples (papain, pepsin, and alkaline hydrolysate), with concentrations 5.6, 5 and 1.53 mg/100mg of protein respectively. The used fluorometric method complied with the validation requirements and can be used to analyze L-tryptophan in samples containing tyrosine without overlapping of spectra and without the use of any specific reagent.

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