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 Stability indicating RP-UPLC method for simultaneous quantification of bempedoic acid and ezetimibe in bulk and pharmaceutical formulations

2021 ◽  
Vol 7 (1) ◽  
Author(s):  
Uma Sai Teja Yarra ◽  
Sowjanya Gummadi
Keyword(s):  
Present Method ◽  
Limit Of Detection ◽  
Pharmaceutical Formulations ◽  
Simultaneous Estimation ◽  
Stability Studies ◽  
Uv Detector ◽  
Limit Of Quantification ◽  
Stability Indicating ◽  
Simultaneous Quantification ◽  
Ich Guidelines

Abstract Background Bempedoic acid and Ezetimibe acid are used in combination for treatment of hypercholesterolemia. The current work was undertaken to develop a simple and rapid stability-indicating RP-UPLC method for the simultaneous estimation of Bempedoic acid and Ezetimibe in tablets as no such method was available. The chromatographic separation was performed with Waters Acquity C18 [50 × 2.1 mm, 1.7 μ] column using methanol: acetonitrile: water [50: 30: 20, by volume] as mobile phase pumped at a flow rate 0.5 mL/min. The separated analytes were detected at 260 nm using UV detector. Results The separation of Bempedoic acid (BA) and Ezetimibe (EZ) was done at a retention time of 1.827 min. and 3.577 min. respectively. The validation and stability studies of the present method were carried out according to the ICH guidelines. The linearity of the proposed method was in the range of 30–130 μg/mL and 5–50 μg/mL for Bempedoic acid and Ezetimibe respectively. Limit of detection (LOD) and limit of quantification (LOQ) were found to be 0.1216 μg/mL and 0.3685 μg/mL for Bempedoic acid and 0.1189 μg/mL and 0.3602 μg/mL for Ezetimibe respectively. The recovery of the method was found to be in the range of 99.89—100.31% for Bempedoic acid and 98.14—99.94% for Ezetimibe while the % RSD for both drugs in the precision and robustness study was less than 2.0. The drugs did not show any major degradants in the exposed conditions. Conclusion The developed method was found to be simple, sensitive, accurate, precise, robust, rapid and yet stability indicating. The method can be adopted for simultaneous estimation of Bempedoic acid and Ezetimibe in the pharmaceutical formulation.

scholarly journals Determination of Clopidol Residues in Chicken Tissues by Liquid Chromatography: Part I. Optimization of Analytical Conditions and Comparison with AOAC Gas Chromatography Method

2001 ◽  
Vol 84 (5) ◽  
pp. 1337-1342 ◽  
Author(s):  
Guo-Fang Pang ◽  
Yan-Zhong Cao ◽  
Chun-Lin Fan ◽  
Jin-Jie Zhang ◽  
Xue-Min Li ◽  
...  
Keyword(s):  
Chromatographic Method ◽  
Limit Of Detection ◽  
Chromatography Method ◽  
Anion Exchange Column ◽  
Chicken Tissues ◽  
Relative Standard ◽  
Liver And Kidney ◽  
Gas Chromatographic Method ◽  
Liquid Chromatographic

Abstract A simple and specific liquid chromatographic method was developed for determination of clopidol in chicken tissues. Samples were extracted with acetonitrile. The extracts were cleaned up on an alumina column and an anion exchange column. The clopidol was separated on a column (30 cm × 3.9 mm) of μBondapak C18 (10 μm) by using acetonitrile–water (20 + 80, v/v) as mobile phase, and determined quantitatively at 270 nm. Recoveries were 86.0–97.6%, with relative standard deviations of 2.14–9.42% at 0.010–2.0 mg/kg from 4 spiked matrixes of chicken muscle, egg, liver, and kidney. The limit of detection was 0.005 mg/kg. Compared with the modified AOAC gas chromatographic method, the present method is simple and fast to operate. Its results are accurate and reliable, making it favorable for environmental protection and meeting requirements for human safety. Thus, it is suitable for routine analysis of large quantities of samples.

scholarly journals Rapid, Simple, and Sensitive Spectrofluorimetric Method for the Estimation of Ganciclovir in Bulk and Pharmaceutical Formulations

2013 ◽  
Vol 2013 ◽  
pp. 1-5 ◽  
Author(s):  
Garima Balwani ◽  
Emil Joseph ◽  
Satish Reddi ◽  
Vibhu Nagpal ◽  
Ranendra N. Saha
Keyword(s):  
Standard Deviation ◽  
Limit Of Detection ◽  
Pharmaceutical Formulations ◽  
Calibration Graph ◽  
Limit Of Quantification ◽  
Average Percentage ◽  
Ich Guidelines ◽  
Spectrofluorimetric Method ◽  
Relative Standard

A new, simple, rapid, sensitive, accurate, and affordable spectrofluorimetric method was developed and validated for the estimation of ganciclovir in bulk as well as in marketed formulations. The method was based on measuring the native fluorescence of ganciclovir in 0.2 M hydrochloric acid buffer of pH 1.2 at 374 nm after excitation at 257 nm. The calibration graph was found to be rectilinear in the concentration range of 0.25–2.00 μg mL−1. The limit of quantification and limit of detection were found to be 0.029 μg mL−1and 0.010μg mL−1, respectively. The method was fully validated for various parameters according to ICH guidelines. The results demonstrated that the procedure is accurate, precise, and reproducible (relative standard deviation <2%) and can be successfully applied for the determination of ganciclovir in its commercial capsules with average percentage recovery of 101.31 ± 0.90.

scholarly journals Validation of an RPHPTLC-Densitometric Method Using Silica Gel 60 RP18WF254for Simultaneous Determination of Nicotinamide in Selected Pharmaceutical Formulations

2015 ◽  
Vol 2015 ◽  
pp. 1-9 ◽  
Author(s):  
Małgorzata Dołowy ◽  
Alina Pyka
Keyword(s):  
Silica Gel ◽  
Mobile Phase ◽  
Research Study ◽  
Limit Of Detection ◽  
Pharmaceutical Formulations ◽  
Limit Of Quantification ◽  
Ich Guidelines ◽  
Development And Validation ◽  
Simple Economic

This research study describes the applicability of silica gel 60 RPW18F254plates for the development and validation of new, simple, economic, accurate, and precise RPHPTLC-densitometric method suitable for the quantification of nicotinamide (asVitamin PP) in three marketed preparations. The mobile phase used was methanol-water in volume composition 3 : 7. Detection wavelength was 200 nm. The proposed method was validated according to ICH guidelines and also based on Ferenczi-Fodor and Konieczka reports. Results were found to be linear over a range of 1.00 to 2.00 μg/spot. Limit of detection (LOD) and limit of quantification (LOQ) were 0.15 μg/spot and 0.45 μg/spot, respectively. The percent content of nicotinamide in the investigated preparations was found to be 99.2% (Product 1), 99.3% (Product 2), and 99.4% (Product 3). Developed method is accurate and precise (CV<3%) and may be successfully applied for the quality control of pharmaceutical formulations containing nicotinamide in the presence of its derivatives, such as N,N-diethylnicotinamide, N-methylnicotinamide, and nicotinic acid.

Fast HPLC Method for the Determination of Piroxicam and its Application to Stability Study

2017 ◽  
Vol 68 (4) ◽  
pp. 701-706 ◽  
Author(s):  
Alina Diana Panainte ◽  
Madalina Vieriu ◽  
Gladiola Tantaru ◽  
Mihai Apostu ◽  
Nela Bibire
Keyword(s):  
Limit Of Detection ◽  
Pharmaceutical Formulations ◽  
Hplc Method ◽  
Calibration Graph ◽  
Stability Study ◽  
Limit Of Quantification ◽  
Ich Guidelines ◽  
System Suitability ◽  
Optimum Separation

A fast and robust RP-HPLC isocratic method was developed for determination of piroxicam in bulk materials and pharmaceutical formulations. Optimum separation of piroxicam and stress induced degradation a product was achieved using a SB-C18 Eclipse column (150x4.6; 5�m). The mobile phase was a mixture of water: acetonitrile (50:50) with a flow rate of 0.5mL/min. The UV detection was performed at 360nm. The method was validated in accordance with the current ICH guidelines in terms of linearity, limit of detection, limit of quantification, precision, accuracy, recovery and system suitability. The retention time for piroxicam was 2.55 min. The calibration graph was linear in the concentration range 5-90�g/mL. The assay proved to be sensitive, specific and reproducible. The method was applied for the determination of piroxicam in tablets.

scholarly journals DETERMINATION OF 10-GINGEROL IN INDIAN GINGER BY VALIDATED HPTLC METHOD OF SAMPLES COLLECTED ACROSS SUBCONTINENT OF INDIA

2016 ◽  
Vol 8 (12) ◽  
pp. 190
Author(s):  
Kamran Ashraf ◽  
Syed Adnan Ali Shah ◽  
Mohd Mujeeb
Keyword(s):  
Thin Layer ◽  
Thin Layer Chromatography ◽  
High Performance ◽  
Limit Of Detection ◽  
Limit Of Quantification ◽  
Chromatography Method ◽  
Aluminum Plates ◽  
Layer Chromatography ◽  
Hptlc Method

<p><strong>Objective: </strong>A simple, sensitive, precise, and accurate stability indicating HPTLC (high-performance thin-layer chromatography) method for analysis of 10-gingerol in ginger has been developed and validated as perICH guidelines.</p><p><strong>Methods: </strong>The separation was achieved on TLC (thin layer chromatography) aluminum plates pre-coated with silica gel 60F<sub>254</sub> using n-hexane: ethyl acetate 55:45 (%, v/v) as a mobile phase. Densitometric analysis was performed at 569 nm.</p><p><strong>Results: </strong>This system was found to have a compact spot of 10-gingerol at <em>R</em><sub>F</sub> value of 0.57±0.03. For the proposed procedure, linearity (<em>r</em><sup>2</sup> = 0.998±0.02), limit of detection (18ng/spot), limit of quantification (42 ng/spot), recovery (ranging from 98.35%–100.68%), were found to be satisfactory.</p><p><strong>Conclusion: </strong>Statistical analysis reveals that the content of 10-gingerol in different geographical region varied significantly. The highest and lowest concentration of 10-gingerol in ginger was found to be present in a sample of Patna, Lucknow and Surat respectively which inferred that the variety of ginger found in Patna, Lucknow are much superior to other regions of India.</p>

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.

scholarly journals Oxytetracycline Residues in Honey Analyzed by Liquid Chromatography with UV Detection

2013 ◽  
Vol 57 (1) ◽  
pp. 25-32 ◽  
Author(s):  
Anna Gajda ◽  
Andrzej Posyniak ◽  
Andrzej Bober ◽  
Tomasz Błądek ◽  
Jan Żmudzki
Keyword(s):  
Liquid Chromatography ◽  
Oxalic Acid ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Experimental Treatment ◽  
Uv Detection ◽  
Limit Of Quantification ◽  
Chromatography Method ◽  
Liquid Chromatography Method

Summary A liquid chromatography method with UV detection for determination of oxytetracycline (OTC) in honey has been developed. The samples were extracted with the solution of oxalic acid. The clean-up procedure was performed by solid phase extraction (SPE) using polymeric Strata X and carboxylic acid cartridges. Chromatographic separation was carried out on the Luna C8 analytical column with mobile phase consisting of acetonitrile-0.02 M oxalic acid. The method has been successfully validated according to the requirements of the European Decision 2002/657/EC and this method is used in routine control of oxytetracycline in honey samples. The limit of detection (LOD) and limit of quantification (LOQ) of the presented method were 10 and 12.5 μg/kg, respectively. The developed method has also been verified in quantitative determination of oxytetracycline residues in honey after experimental treatment with this product in bee colonies.

scholarly journals Liquid Chromatographic Method for the Analysis of Brimonidine in Ophthalmic Formulations

2012 ◽  
Vol 9 (3) ◽  
pp. 1327-1331 ◽  
Author(s):  
A. Narendra ◽  
D. Deepika ◽  
M. Mathrusri Annapurna
Keyword(s):  
Limit Of Detection ◽  
Detector Response ◽  
Eye Drops ◽  
Reverse Phase ◽  
Limit Of Quantification ◽  
Ich Guidelines ◽  
Acid Sodium Salt ◽  
Liquid Chromatographic Method ◽  
Liquid Chromatographic

A reverse phase LC method was developed for the determination of Brimonidine in eye drops. Chromatography was carried on an Inertsil ODS 3V column (C18) using a mixture of Octane 1- sulfonic acid sodium salt (0.02M) (pH 3.5 ± 0.05) and acetonitrile (64:36 v/v) as mobile phase at a flow rate of 1 mL/min with UV detection at 254 nm. The drug was eluted at 4.636 min. The detector response was linear in the concentration range of 0.4–72 μg/mL. The limit of detection and limit of quantification were found to be 0.0561 and 0.1848 μg/mL respectively. The proposed method was validated as per the ICH guidelines and can be applied for the routine analysis of Brimonidine in eye drops.

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.

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