scholarly journals Some validation aspects on the analytical method for assaying carcinogenic amines from textile dyes

2018 ◽  
Vol 69 (03) ◽  
pp. 249-256
Author(s):  
PERDUM ELENA ◽  
MEDVEDOVICI ANDREI VALENTIN ◽  
TACHE FLORENTIN ◽  
VISILEANU EMILIA ◽  
DUMITRESCU IULIANA ◽  
...  
Keyword(s):  
Azo Dyes ◽  
Aromatic Amines ◽  
Textile Industry ◽  
Limit Of Detection ◽  
Research Work ◽  
Negative Effects ◽  
Limit Of Quantification ◽  
Safety Control ◽  
Gas Chromatographic Method ◽  
Finishing Processes

Chemicals safety control and ecological properties have become a priority for the textile industry in order to avoid the negative effects on humans and environment. The increasing interest for toxicology of textiles is determined by the presence of dangerous compounds in clothes generated from dyeing and finishing processes. In order to protect human health, European Regulations as Oeko Tex Standard 100 and REACH Regulation limit the presence of dangerous chemicals, such as aromatic amines, generated by reductive cleavage of azo dyes, by no more than 30 mg/kg of textile material. The main goal of this research work was to develop and validate a HPLC/MWD method for precise and reliable identification and quantification of carcinogenic aromatic amines derived from banned azo dye specific to the textile industry. The simultaneous determination of 24 regulated aromatic amines has been conducted by two chromatographic methods according to SR EN ISO 14362-1:2017 in order to avoid matrix interferences and compounds misidentification due to the presence of structural isomers. Preliminary analyses to establish the maximum absorption wavelength of each standard solution of aromatic amine were performed simultaneously at four wavelengths, 240, 280, 305 and 380 nm. With the scope of demonstrating the consistency, reliability and accuracy of the analysed data, both liquid and gas chromatographic method were validated. Parameters as selectivity, precision, limit of detection and limit of quantification of the analytical methods were evaluated. The certainty of the determinations was also proved by the results of proficiency testing conducted by IIS Netherlands on azo dyes in textiles.

A NOVEL HPLC METHOD FOR ESTIMATION OF GENOTOXIC IMPURITY 3-ACETAMIDOBENZENE 1, 2 DICARBOXYLIC ACID IN KEY STARTING MATERIAL 3-ACETAMIDOPTHALIC ANHYDRIDE OF APREMILAST API

INDIAN DRUGS ◽  
2018 ◽  
Vol 55 (05) ◽  
pp. 42-46
Author(s):  
P. Shinde ◽  
◽  
S. Shirke ◽  
R. Dwivedi ◽  
U Dhuppad
Keyword(s):  
Dicarboxylic Acid ◽  
Mobile Phase ◽  
Limit Of Detection ◽  
Research Work ◽  
Hplc Method ◽  
Starting Material ◽  
Phase Method ◽  
Limit Of Quantification ◽  
Ich Guidelines ◽  
Normal Phase Hplc

3-Acetamidobenzene -1, 2-dicarboxylic acid is a potential genotoxic impurity which gets formed during synthesis of 3- acetamidopthalic anhydride, a Key Starting Material (KSM) for manufacturing of apremilast API. During handling upon exposure to moisture, the anhydride ring of KSM 3-acetamidopthalic anhydride opens to form the acid. Hence Reverse phase HPLC method is not a feasible and robust option for estimation of this impurity. To overcome these problems a normal phase HPLC method is developed and proposed in this research work. Immobilized Chiral pack IA column from Daicel is used for estimation. n-Hexane and isopropyl alcohol in 90:10 (v/v) ratio modified with 0.1% trifluroacetic acid is used as mobile phase. Method is validated as per ICH guidelines. Limit of Detection (LOD) and Limit of Quantification (LOQ) are found to be 0.47 ppm (0.0047%) and 1.42 ppm (0.0142%), respectively. The method is linear over LOQ to 150%. Recovery is within limits (80-120%). Method is robust for parameters like mobile phase composition, flow rate, wavelength changes and column oven temperature.

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 Wasteful Azo Dyes as a Source of Biologically Active Building Blocks

2021 ◽  
Vol 9 ◽  
Author(s):  
Ana Fernandes ◽  
Bruna Pinto ◽  
Lorenzo Bonardo ◽  
Beatriz Royo ◽  
M. Paula Robalo ◽  
...  
Keyword(s):  
Azo Dyes ◽  
Aromatic Amines ◽  
Textile Industry ◽  
Building Blocks ◽  
Biologically Active ◽  
One Pot ◽  
Whole Cells ◽  
Cota Laccase ◽  
Immobilised Cells ◽  
Set Up

In this work, an environment-friendly enzymatic strategy was developed for the valorisation of dye-containing wastewaters. We set up biocatalytic processes for the conversion of azo dyes representative of the main classes used in the textile industry into valuable aromatic compounds: aromatic amines, phenoxazinones, phenazines, and naphthoquinones. First, purified preparations of PpAzoR azoreductase efficiently reduced mordant, acid, reactive, and direct azo dyes into aromatic amines, and CotA-laccase oxidised these compounds into phenazines, phenoxazinones, and naphthoquinones. Second, whole cells containing the overproduced enzymes were utilised in the two-step enzymatic conversion of the model mordant black 9 dye into sodium 2-amino-3-oxo-3H-phenoxazine-8-sulphonate, allowing to overcome the drawbacks associated with the use of expensive purified enzymes, co-factors, or exquisite reaction conditions. Third, cells immobilised in sodium alginate allowed recycling the biocatalysts and achieving very good to excellent final phenoxazine product yields (up to 80%) in water and with less impurities in the final reaction mixtures. Finally, one-pot systems using recycled immobilised cells co-producing both enzymes resulted in the highest phenoxazinone yields (90%) through the sequential use of static and stirring conditions, controlling the oxygenation of reaction mixtures and the successive activity of azoreductase (anaerobic) and laccase (aerobic).

2,2-Bis(4-hydroxyphenyl)propane – inhalation fraction. Determination method in workplace air

2017 ◽  
Vol 33 (3(93)) ◽  
pp. 141-150
Author(s):  
Marzena Bonczarowska ◽  
Sławomir Brzeźnicki
Keyword(s):  
Flame Retardants ◽  
Limit Of Detection ◽  
Upper Respiratory Tract ◽  
Negative Effects ◽  
Limit Of Quantification ◽  
Liquid Chromatograph ◽  
Selective Determination ◽  
Human Fertility ◽  
Workplace Air ◽  
Air Sample

2,2-Bis(4-hydroxyphenyl)propane (bisphenol A BPA) is a substance in a form of a solid crystals or flakes with a mild phenolic odor. BPA is commonly used in the production of epoxide, polycarbonate or polysulfone resins, glues, breaks fluids or as a flame retardants and fungicides. Exposure to BPA can cause irritation of skin, BPA can also act as a nefro or hepatotoxic factor and upper respiratory tract or mucous membranes of the eye. BPA has a negative effects on human fertility. The aim of this study was to develop and validate a sensitive method for determining BPA concentrations in workplace air in the range from 1/10 to 2 MAC values, in accordance with the requirements of Standard No. PN-EN 482. The study was performed using a liquid chromatograph with spectrophotometric (UV-VIS) and spectrofluorimetric (FLD) detection. All chromatographic analyses were performed with Supelcosil LC 18 (150 × 3 mm) analytical column, which was eluted with mixture of acetonitrile and water (1:1). This method was based on collecting BPA on glass fiber filter, extracting with acetonitrile, and chromatographic determining resulted solution with HPLC technique. The average extraction efficiency of BPA from filters was 90%. The method was linear (r = 0.9996) within the investigated working range 0.125–5 mg/m3 for a 720-L air sample. The calculated limit of detection (LOD) and the limit of quantification (LOQ) was to 0.02 μg/ml (UV-VIS) and 0.013 μg/ml (FLD), and 0.068 μg/ml (UV-VIS) and 0.042 μg/ml (FLD), respectively. The analytical method described in this paper enables specific and selective determination of BPA in workplace air in presence of other compounds. The method is precise, accurate and it meets the criteria for measuring chemical agents listed in Standard No. PN-EN 482+A1:2016-01. The method can be used for assessing occupational exposure to BPA and associated risk to workers’ health. The developed method of determining BPA has been recorded as an analytical procedure (see appendix).

scholarly journals Stability-indicating RP-UPLC Method for Determination of Vildagliptin in Drug Substance and Its Tablet Dosage Form

2021 ◽  
pp. 139-146
Author(s):  
Kalyani Peluri ◽  
S. Rajasekaran
Keyword(s):  
Limit Of Detection ◽  
Research Work ◽  
Cost Effective ◽  
Drug Substance ◽  
Forced Degradation ◽  
Limit Of Quantification ◽  
Average Percentage ◽  
Stability Indicating ◽  
Degradation Studies

Aim: The foremost purpose of this research work is to diminish the analysis time and to establish cost effective method for estimation of Vildagliptin by RP-UPLC. Study Design: UPLC based Quantification studies. Place and Duration of Study: Department of Pharmacy, Bhagwant University, Ajmer, Rajasthan, Indiabetween June 2020 and August 2020. Methodology: A simple, responsive and precised RP-UPLC method with good robustness was developed and validated as per ICH for the analysis of Vildagliptin in drug substance and separation of degradants generated by different forced degradation conditions. Productive separation of Vildagliptin was attained by the use of Luna C18 column (100x2.6mm and 1.6µm) with a mobile phase composition of 0.1% v/v Trifluoroacetic acid and Acetonitrile in 80:20 v/v, which was pumped with 0.5 ml/min flow rate. The eluted substances were examined with PDA detector at 239nm. Stressed degradation studies were performed with proposed method to determine the percentage degradation of Vildagliptin. Results: The RT of Vildagliptin was observed at 1.56 min. The developed method was validated as per ICHQ2B and proved that the method was precise, sensitive, specific and accurate.The lowest concentration of limit of detection (0.05µg/ml) and limit of quantification(0.5µg/ml) of Vildagliptin make obvious about the sensitivity of the method. The correlation coefficient found to be 0.9997 for given range of linear concentrations. The calculated average percentage recoveries of Vildagliptin in spiked solutions were found to be in the range of 99.1-100.5. The calculated % RSD was determined to be less than 2. Determination of degradation of amount of Vildagliptin by forced degradation studies representing the stability indicating nature of the proposed method. Conclusion: The developed method said to be highly sensitive, accurate, specific and robust, therefore this method has high probability to adopt in pharmaceutical industry for regular analysis of Vildagliptin.

scholarly journals Determination of Ethanol Content in Kombucha Using Headspace Gas Chromatography with Mass Spectrometry Detection: Single-Laboratory Validation

2020 ◽  
Author(s):  
Michael Chan ◽  
Hong Sy ◽  
Jamie Finley ◽  
Jake Robertson ◽  
Paula N Brown
Keyword(s):  
Dynamic Range ◽  
Limit Of Detection ◽  
Alcoholic Beverage ◽  
The United States ◽  
Limit Of Quantification ◽  
Method Performance ◽  
Potential Health ◽  
Headspace Gas ◽  
Gas Chromatographic Method

Abstract Background Kombucha is a fermented beverage made with tea, sugar, and a symbiotic colony of bacteria and yeast that is usually marketed as a non-alcoholic beverage. Products must contain <0.5% and <1.1% alcohol by volume in the United States and Canada respectively to be classified as non-alcoholic products. Prior studies have found that Kombucha beverages can become very acidic and may contain levels of alcohol above 1% which can be a potential health risk to children and the developing fetus during pregnancy. Objective Given the public safety concerns and legal requirements associated with the level of alcohol within Kombucha beverages, there is a need for accurate and reliable methods. Herein we describe the validation of a sensitive, rapid, and simple Headspace Gas Chromatographic method with mass spectrometric detection for determining ethanol in Kombucha. Methods Method performance characteristics measured included linearity, accuracy, precision, limit of detection (LOD), and limit of quantification (LOQ) as per AOAC International guideline Appendix K Part 1. Performance was evaluated against the AOAC Standard Method Performance Requirements 2016.001 for determination of ethanol in Kombucha. Results The linear dynamic range for this method was confirmed over the range of 0.025 to 2.47% ABV. The LOD and LOQ were determined to be 0.0002% and 0.002% ABV, respectively. With a spike recovery of 102% for accuracy and precision of RSDr ≤ 4% the method met the SMPR requirements within the analytical range. Conclusions The results of this validation study demonstrated the method is fit for the purpose of quantifying ethanol in Kombucha and is suitable for rapid and easy integration by laboratories to ensure that regulatory requirements are met.

Development and Validation of Teneligliptin Stereoisomers by HPLC Using Cellulose Based Immobilized Polysaccharide Chiral Stationary Phase

2020 ◽  
Vol 17 ◽  
Author(s):  
Gunnam Srinivasu ◽  
Ch Thirupathia ◽  
Ch Lakshmi Narayanaa ◽  
Ch Parameswara Murthy ◽  
Sarah Imam Siddiqui
Keyword(s):  
Stationary Phase ◽  
High Performance ◽  
Chiral Stationary Phase ◽  
Limit Of Detection ◽  
Research Work ◽  
Hplc Method ◽  
Limit Of Quantification ◽  
Bulk Drug ◽  
Development And Validation ◽  
Isocratic Mode

Background:: There is no single chiral method for the quantitation of teneligliptin stereoisomers by high performance liquid chromatography (HPLC). Hence, there is a need for the quantification of teneligliptin (TNGP) and its stereoisomers. Objective:: The main aim of the research work is to develop a novel simple, selective, precise and accurate HPLC method for separation of TNGP and its stereoisomers. Methods:: Different screening trials were executed by changing the mobile phase compositions to normal phase and polar mode and also by utilizing the different immobilized polysaccharide chiral columns like CHIRALPAK IA, IC, ID, IE, IF and IG. All the stereoisomers were eluted with high resolution, on CHIRALPAK IC-3 (4.6×250 mm), 3 μm chiral stationary phase (CSP) with flow rate of 0.7 mL/min. The chromatographic system was processed with isocratic mode comprising ethanol: acetonitrile: ethanolamine in the proportion of 90:10:0.1% v/v/v with column oven temperature of 15 °C and detection wavelength of 250 nm. Results:: The limit of detection (LOD) and limit of quantification (LOQ) values of TNGP(API), R,S-isomer, S,R-isomer and R,R-isomer were found to be 0.036/0.11, 0.029/0.09, 0.038/0.011 and 0.020/0.06 μg/mL, respectively. The method was found to be precise, accurate and linear (R2 > 0.999). Conclusion:: The developed method also successfully applied for the quantification of bulk drug without any interference with the extraneous components. Hence, the method can be utilized successfully in the pharmaceutical organizations for the separation and quantification of TNGP isomers.

scholarly journals Quantitative determination and validation of ethylhexylglycerin using Gas chromatography method

2018 ◽  
Vol 9 (1) ◽  
pp. 30
Author(s):  
Rambabu Arla ◽  
Srinivasa Rao J ◽  
Kailasam Koumaravelou
Keyword(s):  
Chromatographic Method ◽  
Limit Of Detection ◽  
Pharmaceutical Formulations ◽  
Stability Studies ◽  
Limit Of Quantification ◽  
Chromatography Method ◽  
Ich Guidelines ◽  
Clear Peak ◽  
Gas Chromatographic Method

Ethylhexylglycerin, an alkyl glyceryl ether, used in various cosmetics and deodorants is also known to have anti-microbial activity and hence used as an adjuvant along with other preservatives to produce synergistic effect. In the present study, a gas chromatographic method has been employed and validated to determine the presence of impurities along with ethylhexylglycerin. A column having the dimension of DB-1 30m x 0.32mm; 0.25µm with acetone as solvent was found to be optimal for the ideal separation of ethylhexylglycerin from its impurities. Injection volume was set to 1 µl and temperature was maintained at 240°C. A clear peak was observed with the retention time of 8.002 minutes. As per ICH guidelines, the developed method was validated with respect to specificity, sensitivity, Limit of detection, Limit of quantification, linearity, precision, and also stability studies. As per the method, it shows a good correlation co-efficient (R2) value of 0.999 within the concentration range of 0.1- 0.75µg. Therefore, a gas chromatographic method was proposed which can be precise, specific and can be employed for the determination of ethylhexylglycerin in various pharmaceutical formulations. Keywords: Ethylhexylglycerin; Adjuvant; ICH guidelines; Validation; Stability studies

scholarly journals “Robust and Rapid” UV Spectroscopic Method for Estimation of Luliconazoleand Clobetasol Propionate Drug Combination

2021 ◽  
pp. 313-320
Author(s):  
Binal Solanki ◽  
Hirak Joshi
Keyword(s):  
Method Development ◽  
Limit Of Detection ◽  
Spectroscopic Method ◽  
Research Work ◽  
Clobetasol Propionate ◽  
New Combination ◽  
Simultaneous Estimation ◽  
Statistical Validation ◽  
Limit Of Quantification ◽  
Laboratory Procedure

Objective: The new combination for Luliconazole and Clobetasol Propionate was approved for the treatment of variety of skin disease. The main objective of this research is development and validation of novel, simple, fast and responsive derivative spectroscopic process for simultaneous estimation of newly approved combination Luliconazole (LLZ) and Clobetasol Propionate (CLP). Methodology: Here in this first derivative spectroscopic method, the absorbance of LLZ and CLP was taken at 312nm (ZCP of CLP) and 249nm (ZCP of LLZ) respectively. Establishment of linearity was in a concentration varies from 10-50 µg/ml for Luliconazole and 5-25µg/ml for Clobetasole Propionate. Results: From the method developed above the R2 value observed for LLZ and CLP is 0.9988 and 0.9961. Statistical validation of accuracy and reproducibility was done for planned procedure with the help of recovery studies. The mean % recovery of Luliconazole and Clobetasol Propionate was found to be 99.45 % and 99.43% respectively. For LLZ the Limit of detection is 0.0054 µg/ml and limit of quantification is 0.0164 µg/ml and for CLP the Limit of detection is 0.0009µg/ml and limit of quantification 0.0027µg/ml. Conclusion: From research work the method development was done and shows fast, precise, exact and easily accessible laboratory procedure for routine evaluation of combination drugs.

Spectrophotometeric Determination of Trifluoperazine HCL in Pure Forms and Pharmaceutical Preperations

2017 ◽  
Vol 9 (5) ◽  
Author(s):  
Mohammad Hamzah Hamzah ◽  
Rawa M M Taqi ◽  
Muna M. Hasan ◽  
Raid J. M. Al-Timimi
Keyword(s):  
Standard Method ◽  
Limit Of Detection ◽  
Molar Absorptivity ◽  
Dosage Forms ◽  
Oxidizing Agent ◽  
Optimum Conditions ◽  
Limit Of Quantification ◽  
Cerium Ion ◽  
Blank Solution

A simple and accurate spectrophotometric method for the determination of Trifluoperazine HCl in pure and dosage forms was developed. The method is based on the reaction between Trifluoperazine HCl and p-chloroaniline in the presence of cerium ion as oxidizing agent which lead to the formation of violate color product that absorbed at a maximum wavelength 570nm while the blank solution was pink. Under the optimum conditions a linear relationship between the intensity and concentration of TRF in the range 4-50μg/ml was obtained . The molar absorptivity 3.74×103 L.mol-1.cm-1 , Limit of detection (2.21μg/ml), while limit of quantification was 7.39μg/ml. The proposed analytical method was compared with standard method using t-test and F-test , the obtained results shows there is no significant differences between proposed method and standard method. Based on that the proposed method can be used as an alternative method for the determination of TRF in pure and dosage forms.

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