scholarly journals Development and Validation of Estimation of Genotoxic Impurity (Triethyl orthoformate content) in 5-methyl-4-isoxazole carboxylic acid (5-MIA) by using GC Technique

2021 ◽  
Vol 37 (2) ◽  
pp. 348-353
Author(s):  
Mohan bhatale ◽  
Neelakandan kaliyaperumal ◽  
Gopalakrishnan Mannathusamy ◽  
Gurunathan ramalingam
Keyword(s):  
Method Development ◽  
Limit Of Detection ◽  
Fused Silica ◽  
Triethyl Orthoformate ◽  
Concentration Limit ◽  
Simultaneous Estimation ◽  
Validation Parameters ◽  
Limit Of Quantitation ◽  
Gas Chromatographic Method ◽  
Development And Validation

A simple, selective, precise and accurate Gas chromatographic method for determination of Triethyl orthoformate content (Genotoxic impurity) in 5-MIA is reported. The GC method development and validation as per the International Council for Harmonisation (ICH) guidelines Q2(R1). The effective chromatographic separations were achieved on DB-624, 60 m × 0.53 mm ID, with film thickness of 3.0 μm (Fused silica capillary column), Capillary injector temperature of 150°C, and Nitrogen Carrier gas. This method is unique as there is no UV response; hence GC Method was developed for Triethyl orthoformate. The elution was accomplished with the flow rate of 5.0 mL/min and Split Flow of 10 mL/minute. Detection was performed with FID detector (temp. 260°C) and with column oven temperature program. Methods range from limit of quantitation (LOQ) to 150% level with respect to specification concentration limit of impurity is linear and correlation coefficient of impurity is > 0.99. The linearity of Triethyl orthoformate covered from LOQ to 113 ppm (ie. LOQ to 150% of specification limit) and LOQ to 19 ppm wrt standard concentration. The limit of detection (LOD)values were observed were 2.5 ppm and limit of quantitation (LOQ) were 7.7 ppm, respectively. The parameters selected for the method validated were from international conference on harmonization guidelines, Indian pharmacopeia, USP. The percentage recovery from LOQ, 50% ,100% to 150% level of content were 87.70%, 98.60%, 102.25 and 96.59% respectively. The %RSD values were for LOQ to 150% were from 1.64%, 0.89%, 1.78 % and 1.49%. The range was covered from LOQ to 150% of standard concentration. The results of validation parameters were found in the acceptance range. Standard and sample were stable up to 30 h at when stored at room temperature. Also it was quite robust for the small change in method parameter like, change in column oven temperature(± 5 degree). Hence from the above parameter it was concluded that the GC method with FID detector is selective, precise, linear, and robust for simultaneous estimation of Triethyl orthoformate in Drug Substances.

scholarly journals Measurement of HDO Products Using GC-TCD: Towards Obtaining Reliable Analytical Data

2018 ◽  
Vol 5 (1) ◽  
pp. 1-11 ◽  
Author(s):  
Oman Zuas ◽  
Harry Budiman ◽  
Dieni Mansur ◽  
Muhammad Rizky Mulyana
Keyword(s):  
Method Development ◽  
Limit Of Detection ◽  
Analytical Data ◽  
Sample Treatment ◽  
Gaseous Products ◽  
Relative Standard ◽  
Validation Parameters ◽  
Limit Of Quantitation ◽  
Method Development And Validation ◽  
Development And Validation

Abstract This paper reported the method development and validation of a gas chromatography with thermal conductivity detector (GC-TCD) method for the measurement of the gaseous products of hydrodeoxygenation (HDO). The method validation parameters include selectivity, precision (repeatability and reproducibility), accuracy, linearity, limit of detection (LoD), limit of quantitation (LoQ), and robustness. The results showed that the developed method was able to separate the target components (H2, CO2, CH4 and CO) from their mixtures without any special sample treatment. The validated method was selective, precise, accurate, and robust. Application of the developed and validated GC-TCD method to the measurement of by-product components of HDO of bio-oil revealed a good performance with relative standard deviation (RSD) less than 1.0% for all target components, implying that the process of method development and validation provides a trustworthy way of obtaining reliable analytical data.

scholarly journals A REVIEW ON ANALYTICAL METHOD DEVELOPMENT AND VALIDATION

2018 ◽  
Vol 10 (6) ◽  
pp. 8 ◽  
Author(s):  
Shivani Sharma ◽  
Swapnil Goyal ◽  
Kalindi Chauhan
Keyword(s):  
Method Development ◽  
Limit Of Detection ◽  
Cost Effective ◽  
Good Manufacturing Practice ◽  
Raw Material ◽  
Analytical Technique ◽  
Effective Manner ◽  
Validation Parameters ◽  
Limit Of Quantitation ◽  
Development And Validation

The top objective of any pharmaceutical industry is to produce products of necessary characteristic and quality reliably, in a cost-effective manner. Development of a method is essential for discovery, development, and evaluation of medicines in the pharmaceutical formulation. The main aim of this review article was to check the development and validation of the procedure employed for the medication from the starting of the formulation to the complete commercial batch of product. At the point when an analytical technique is applied to produce outcomes for the quality of medicine associated samples, it is necessary that the outcomes are reliable. In the pharma industry, validation policy is documented for how to perform validation, types of validation and validation policy are complied with the necessities of good manufacturing practice (GMP) regulations. Validation is very important for the effective running of the pharmaceutical firms. At every stage from raw material to the finished, stability, everywhere validation was performed. The method was developed properly, and validation parameters are explained in terms of accuracy, specificity, precision, limit of detection (LOD), limit of quantitation (LOQ), ruggedness, robustness, and system suitability testing with the example of certain drugs. All validation parameters are used in the routine and stability analysis.

scholarly journals Analytical Method Development and Validation of Rp-Hplc Method for Simultaneous Estimation of Pyridoxamine Dihydrochloride and Acetylcysteine in Tablet Dosage Form.

2021 ◽  
Vol 23 (06) ◽  
pp. 992-1000
Author(s):  
Sneha S. Ghule ◽  
◽  
Ashpak M. Tamboli ◽  
Snehal D. Patil ◽  
◽  
...  
Keyword(s):  
High Performance ◽  
Method Development ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Rp Hplc ◽  
System Suitability ◽  
Validation Parameters ◽  
Method Development And Validation ◽  
Development And Validation ◽  
Tablet Dosage

A reverse-phase high-performance liquid chromatography (RP-HPLC) method for the simultaneous estimation of Pyridoxamine dihydrochloride and Acetylcysteine in the marketed formulation is developed. Chromatography carried out at 30oc temperature on Agilent Zorbax Bonus-RP (250 x 4.6 mm, 5 µ) coloum. Coloum using a mobile phase 0.1% trifluroacetic acid in water: acetonitrile (80:20v/v) with flow rate 1ml/min (DAD scan at 210nm). Validation parameters such as system suitability, linearity, precision, accuracy are considered as reported International Conference on Harmonization guidelines. The retention times for Pyridoxamine dihydrochloride and Acetylcysteine are 2 min and 3.4 min. The linearity range for Pyridoxamine dihydrochloride and Acetylcysteine is 30-70 µg/ml and 180-420 µg/ml. The %RSD for accuracy was found to be less than 2%. Hence the proposed method was found to be accurate, precise, reproducible, and specific and can be used for simultaneous analysis of these drugs in tablet formulation.

METHOD DEVELOPMENT AND VALIDATION FOR THE SIMULTANEOUS ESTIMATION OF THYMOL AND EUGENOL BY USING RP-HPLC IN PURE AND IN EMULGEL FORMULATION

INDIAN DRUGS ◽  
2021 ◽  
Vol 58 (07) ◽  
pp. 59-65
Author(s):  
Vinita C. Patole ◽  
Shilpa P. Chaudhari ◽  
Keyword(s):  
High Performance ◽  
Method Development ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Limit Of Quantification ◽  
Relative Standard ◽  
Peak Areas ◽  
80 A 20 ◽  
Development And Validation

An attempt was made to develop a simple, selective, rapid and precise high-performance liquid chromatography (HPLC) method for simultaneous estimation of thymol and eugenol. Analysis was performed on a C18 column with the mobile phase consisting of solvent %A (water) and solvent %B (acetonitrile) with the following gradient: 0–1 min, 80 % A, 20 % B; 1–7 min, 40 % A and 60 % B; 7–12 min, 10 % A and 90 % B; and 12–15min, 80 % A and 20 % B at a flow rate of 0.6 mL/min. The compounds were well separated on a Thermo Scientific Hypersil BDS RP C18 column (4.6 mm × 150 mm, dp = 5 µm) and ultraviolet detection at 280 nm. The retention times of eugenol and thymol were 10.5 min and 11.6 min, respectively. Validation of the proposed method was carried out according to the guidelines of the International Council on Harmonization (ICH). The linearity of the method is good for thymol and eugenol over the concentration range of 1–50 ppm, and the r 2 values were 0.9996 for both thymol and eugenol. The calculated limit of detection (LOD) value was 0.5ppm and the limit of quantification (LOQ) value was 1ppm for both the analytes. The intra and interday relative standard deviation (RSD) of the retention time and peak areas was less than 3 %.The established method was appropriate, and the two markers were well resolved, enabling efficient quantitative analysis of thymol and eugenol.

scholarly journals Reversed phase HPLC for strontium ranelate: Method development and validation applying experimental design

2018 ◽  
Vol 68 (2) ◽  
pp. 171-183
Author(s):  
Béla Kovács ◽  
Lajos Kristóf Kántor ◽  
Mircea Dumitru Croitoru ◽  
Éva Katalin Kelemen ◽  
Mona Obreja ◽  
...  
Keyword(s):  
Experimental Design ◽  
Strontium Ranelate ◽  
Method Development ◽  
Limit Of Detection ◽  
Cost Effective ◽  
Reversed Phase ◽  
Hplc Method ◽  
Intermediate Precision ◽  
Limit Of Quantitation ◽  
Development And Validation

Abstract A reverse-phase HPLC (RP-HPLC) method was developed for strontium ranelate using a full factorial, screening experimental design. The analytical procedure was validated according to international guidelines for linearity, selectivity, sensitivity, accuracy and precision. A separate experimental design was used to demonstrate the robustness of the method. Strontium ranelate was eluted at 4.4 minutes and showed no interference with the excipients used in the formulation, at 321 nm. The method is linear in the range of 20–320 μg mL−1 (R2 = 0.99998). Recovery, tested in the range of 40–120 μg mL−1, was found to be 96.1–102.1 %. Intra-day and intermediate precision RSDs ranged from 1.0–1.4 and 1.2–1.4 %, resp. The limit of detection and limit of quantitation were 0.06 and 0.20 μg mL−1, resp. The proposed technique is fast, cost-effective, reliable and reproducible, and is proposed for the routine analysis of strontium ranelate.

scholarly journals THE RAPID AND GREEN HAIR ANALYSIS METHOD DEVELOPMENT USING FTIR FOR PAPAVERINE HCL DETERMINATION

2019 ◽  
pp. 211-217 ◽  
Author(s):  
ILMA NUGRAHANI ◽  
STEPHANIE SULISTIANA ◽  
SLAMET IBRAHIM
Keyword(s):  
Hair Sample ◽  
Method Development ◽  
Limit Of Detection ◽  
Area Under The Curve ◽  
Forensic Analysis ◽  
Percent Recovery ◽  
Relative Standard ◽  
Validation Parameters ◽  
Limit Of Quantitation ◽  
Papaverine Hydrochloride

Objective: This study was aimed to develop a rapid analysis using FTIR (Fourier Transform Infra-Red) for papaverine hydrochloride (HCl) determination in the hair sample, supported by a mathematically manipulation; which never been reported before in toxicology and forensic analysis. Methods: Firstly, the method was checked its validity to ensure the feasibility for the quantitative purpose. The absorbance spectrums were collected by measure the drug, matrix, and its mixture. A spectra which showed the best specificity and linearity then was selected and derived. Afterwards, the area under the curve (AUC) was measured. A series of concentration was used for compose the calibration curve. Based on the result, some validation parameters were checked thoroughly. Further, for sample preparation, hair was collected non-invasively, then was decontaminated using soap. Next, it was immersed into a papaverine HCl solution at a concentration of 25 mg/ml along days. Finally, the amount of drugs absorbed were measured by the developed method using FTIR. Results: Experimental data showed that all validation parameters could be fulfilled by the developed method. The selected spectra for the content determination was 1320-1230 cm-1. Its linearity was represented by a correlation coefficient value (r) ≥ 0.9999, variation coefficient (Vxo) ≤ 2.0%. The limit of detection (LOD) was 0.00618% w/w, meanwhile, the limit of quantitation (LOQ) was 0.02060% w/w, respectively. The percent recovery was in the range 97-103% with the relative standard deviation (RSD) was ≤ 2.0%. The drug has detected after 72 h immersion, moreover, after 192 h the concentration gained was 0.1594±0.0011% w/w. Conclusion: As the conclusion, FTIR absorbance-derivative method is adequate as a rapid procedure for determine papaverine HCl in the hair sample. This method shows the appropriate of specificity, accuracy and precise. In addition, it shows the advantages of simplicity, green/eco-friendlier, and cost-efficiency.

scholarly journals Development and Validation of RP-HPLC Chromatographic Dissolution Method for the Simultaneous Estimation of Ramipril and Hydrochlorothiazide from Solid Dosage Formulation

2021 ◽  
pp. 203-217
Author(s):  
Prabhakar V. Raut ◽  
Sudhakar L. Padwal ◽  
Madhusudhan T. Bachute ◽  
Satish A. Polshettiwar
Keyword(s):  
Method Development ◽  
Theoretical Plate ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Dissolution Medium ◽  
Dissolution Method ◽  
Rp Hplc ◽  
Relative Standard ◽  
Limit Of Quantitation ◽  
Development And Validation

The present study describes the dissolution method development and validation of Ramipril and Hydrochlorothiazide in tablet dosage form by HPLC Method. A simple, rapid, selective, reproducible and isocratic reversed-phase high performance liquid chromatographic (RP-HPLC) method has been developed and validated as per ICH guidelines. Analysis was performed on a Thermo, Sunniest C8 (150 mm x 4.6 mm, 5 µm) with the mobile phase consisting of mixing 500 mL of buffer solution and 500 mL of acetonitrile at a flow rate of 1.0mL/min. UV detection was performed at 210nm and the Run time for Ramipril and Hydrochlorothiazide were 10 minutes. The calibration curve was linear (correlation coefficient = 1.000) in the selected range for both analytes. The optimized dissolution conditions include the USP Type 1 (Basket) rotation rate of 100 rpm and 750 mL of 0.1 N Hydrochloric acid as dissolution medium, at 37.0 ± 0.5°C. The method was validated for precision, linearity, specificity, accuracy, limit of quantitation and ruggedness. The system suitability parameters, such as theoretical plate, tailing factor and relative standard deviation (RSD) between six standard replicates were well within the limits. The stability result shows that the drug is stable in the prescribed dissolution medium.

scholarly journals ULTRAVIOLET-SPECTROPHOTOMETRIC METHOD DEVELOPMENT AND VALIDATION FOR THE DETERMINATION OF NORFLOXACIN PRESENT IN TASTE MASKED DRUG RESIN COMPLEX

2018 ◽  
Vol 11 (4) ◽  
pp. 244
Author(s):  
Ayya Rajendra Prasad ◽  
Jayanthi Vijaya Ratna
Keyword(s):  
Spectrophotometric Method ◽  
Absorption Maximum ◽  
Method Development ◽  
Limit Of Detection ◽  
Statistical Parameters ◽  
Limit Of Quantification ◽  
Relative Standard ◽  
Validation Parameters ◽  
Development And Validation

 Objective: The objective of this study was developed and validated a novel, specific, precise, and simple ultraviolet (UV)-spectrophotometric method for the estimation of norfloxacin present in taste masked drug-resin complex.Methods: UV-spectrophotometric determination was performed with ELICO SL 1500 UV-visible spectrophotometer using 0.1 N HCl as a medium. The spectrum of the standard solution was run from 200 to 400 nm range for the determination of absorption maximum (λ max). λ max of norfloxacin was found at 278 nm. The absorbance of standard solutions of 1, 2, 3, 4, and 5 μg/ml of drug solution was measured at an absorption maximum at 278 nm against the blank. Then, a graph was plotted by taking concentration on X-axis and absorbance on Y-axis which gave a straight line. Validation parameters such as linearity and range, selectivity and specificity, limit of detection (LOD) and limit of quantification (LOQ), accuracy, precision, and robustness were evaluated as per the International Conference on Harmonization (ICH) guidelines.Results: Linearity for the UV-spectrophotometric method was noted over a concentration range of 1–5 μg/ml with a correlation coefficient of 0.9995. The LOD and LOQ for norfloxacin were found at 0.39 μg/ml and 1.19 μg/ml, respectively. Accuracy was in between 99.00% and 99.17%. % relative standard deviation for repeatability, intraday precision, and interday precision was found to be 0.600, in between 0.291 and 0.410, and in between 0.682 and 1.439, respectively. The proposed UV spectrophotometric method is found to be robust.Conclusion: The proposed UV-spectrophotometric method was validated according to the ICH guidelines, and results and statistical parameters demonstrated that the developed method is sensitive, precise, reliable, and simple for the estimation of norfloxacin present in taste masked drug-resin complex.

Analytical Method Development and Validation for Simultaneous Estimation of Trimetazidine Hydrochloride and Metoprolol Succinate Using HPTLC

2019 ◽  
Vol 15 (3) ◽  
pp. 243-250 ◽  
Author(s):  
Surendra Agrawal ◽  
Pravina Gurjar ◽  
Bhavik Katheriya
Keyword(s):  
Dosage Form ◽  
Method Development ◽  
Limit Of Detection ◽  
Simultaneous Estimation ◽  
Metoprolol Succinate ◽  
Limit Of Quantitation ◽  
Label Claim ◽  
Tablet Dosage ◽  
Hptlc Method

Introduction: Trimetazidine and Metoprolol combination is more effective in the treatment of cardiac disorders as compared to single drug therapy.Background: Materials and Methods: A rapid, simple, and sensitive HPTLC method was developed for the simultaneous determination of Trimetazidine and metoprolol from its tablet dosage form and validated. In HPTLC method, standard and sample solutions of Trimetazidine hydrochloride and metoprolol succinate were applied on pre-coated silica gel G 60 F254 TLC plate, and developed by using mobile phase, n-butanol :water: methanol: ammonia as solvent (8.5:0.1:0.1: 0.85, v/v). The drugs on plate were scanned at 213 nm. The method produced compact and well-resolved bands at Rf of 0.32 ± 0.02 and 0.66 ± 0.02 for Trimetazidine Hydrochloride and Metoprolol succinate respectively. The range for linearity was observed as 500-2500 ng band-1 for Trimetazidine hydrochloride and 500-2500 ng band-1 for metoprolol succinate and correlation coefficient were 0.9991 and 0.9997 respectively. Conclusion: The developed method was validated according to the ICH guidelines for precision, accuracy, Limit of detection, Limit of quantitation, specificity and robustness. The method was checked for suitability in determination of Trimetazidine hydrochloride and Metoprolol succinate in their tablet dosage form. The assay result was found to be 99.64 % ± 0.45 and 99.94 % ± 0.53 of percentage label claim for Trimetazidine hydrochloride and Metoprolol succinate respectively.

Bioanalysis - Method Development, Validation, Sample Preparation, its Detection Techniques and its Application

2021 ◽  
pp. 297-305
Author(s):  
Seema R. Nikam ◽  
Amol S. Jagdale ◽  
Sahebrao S. Boraste ◽  
Shrikant B Patil
Keyword(s):  
Sample Preparation ◽  
Method Development ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Bioequivalence Study ◽  
Time Frame ◽  
Biological Drugs ◽  
Detection Techniques ◽  
Validation Parameters ◽  
Limit Of Quantitation

Quantitatively measurements of chemical and biological drugs and their metabolites in the biological sample. This used in clinical and non-clinical studies. Non clinical including Pharmacokinetic and Toxic kinetic study, and clinical including Bioavailability, Bioequivalence study. This are play significant role and help in improvement in technology and analytical methods. Recent years have witnessed the introduction of several high- quality review articles into the literature covering various scientific and technical aspects of bioanalysis. Method validation and development use for the purpose of suitability of method for their intended purpose, this are important in Drug Discovery and Development. It including a validation parameters are Accuracy, Precision, Range, Calibration Curve, Recovery, Limit of Detection, Limit of Quantitation, Specificity, Selectivity and Stability, Ruggedness. This applicable in bio analysis, FDA and EMA guidelines. There are 3 main Extraction techniques used in sample preparation in bioanalysis is precipitation, liquid –liquid extraction, solid phase extraction. Detection of analyte by using hyphenated and chromatographic techniques like LC-MS/MS, HPLC, GC-MS. This LC-MS/MS is commonly used in a bioanalysis. This bio analysis study used in Pharmaceutical, Biomedical research purpose. Many challenges in pharmaceutical industry that fulfill by the utilization of analytical technologies and high-throughput automated platforms has been employed; in order to perform more experiments in a shorter time frame with increased data quality.

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