scholarly journals Analytical Method Development and Validation for the Quantification of Acetone and Isopropyl Alcohol in the Tartaric Acid Base Pellets of Dipyridamole Modified Release Capsules by Using Headspace Gas Chromatographic Technique

2018 ◽  
Vol 2018 ◽  
pp. 1-10 ◽  
Author(s):  
Sriram Valavala ◽  
Nareshvarma Seelam ◽  
Subbaiah Tondepu ◽  
V. Shanmukha Kumar Jagarlapudi ◽  
Vivekanandan Sundarmurthy
Keyword(s):  
Tartaric Acid ◽  
Method Development ◽  
Isopropyl Alcohol ◽  
Fused Silica ◽  
Chromatographic Technique ◽  
Modified Release ◽  
Flame Ionization ◽  
Technical Requirements ◽  
Headspace Gas ◽  
Gas Chromatographic Method

A simple, sensitive, accurate, robust headspace gas chromatographic method was developed for the quantitative determination of acetone and isopropyl alcohol in tartaric acid-based pellets of dipyridamole modified release capsules. The residual solvents acetone and isopropyl alcohol were used in the manufacturing process of the tartaric acid-based pellets of dipyridamole modified release capsules by considering the solubility of the dipyridamole and excipients in the different manufacturing stages. The method was developed and optimized by using fused silica DB-624 (30 m × 0.32 mm × 1.8 µm) column with the flame ionization detector. The method validation was carried out with regard to the guidelines for validation of analytical procedures Q2 demanded by the International Council for Harmonisation of Technical Requirements for Pharmaceuticals for Human Use (ICH). All the validation characteristics were meeting the acceptance criteria. Hence, the developed and validated method can be applied for the intended routine analysis.

Gas Chromatographic Method for Determination of Dimethylamine, Trimethylamine, and Trimethylamine Oxide in Fish-Meat Frankfurters

1991 ◽  
Vol 74 (2) ◽  
pp. 400-403
Author(s):  
Walter Fiddler ◽  
Robert C Doerr ◽  
Robert A Gates
Keyword(s):  
Atlantic Menhaden ◽  
Chromatographic Technique ◽  
Acid Extraction ◽  
Fish Meat ◽  
Flame Ionization ◽  
Trimethylamine Oxide ◽  
Headspace Gas ◽  
Gas Chromatographic Method ◽  
Gas Tight

Abstract A method Is described for analysis of minced fish-meat and surlmi-meat frankfurters for dimethylamine (DMA), trimethyiamine (TMA), and trimethyiamine oxide (TMAO) using a headspace-gas chromatographic technique. After simple acid extraction and addition of NaOH, the headspace was directly Injected Into a gas chromatograph by a gas-tight syringe. DMA and TMA were separated on a Chromosorb 103 column and detected by a flame Ionization detector. TMAO was measured as TMA after Zn reduction. Repeatability of the method for DMA, TMA, and TMAO was 6.6,1.0, and 18.8 ppm, respectively. The method was applicable to Alaska pollock-meat and Atlantic menhaden-meat frankfurters, unwashed, and washed mince and surlml.

A Headspace Gas Chromatographic Method for Determination of Formic acid Content in Isosulfan Blue and in Various Drugs

2021 ◽  
Vol 37 (2) ◽  
pp. 321-329
Author(s):  
Nilesh Takale ◽  
Neelakandan Kaliyaperumal ◽  
Gopalakrishnan Mannathusamy ◽  
Rajarajan Govindasamy
Keyword(s):  
Sulfuric Acid ◽  
Formic Acid ◽  
Chromatographic Method ◽  
Isopropyl Alcohol ◽  
Class Iii ◽  
Drug Substances ◽  
Headspace Gas ◽  
Concentrated Sulfuric Acid ◽  
Gas Chromatographic Method

The Pharmaceutical industry uses formic acid in the manufacturing of various drug substances or API. At the time of manufacturing of API formic acid is use as an oxidizing agent. Formic acid is the simplest carboxylic acid. It also called methanoic acid.Formic acid present in API at high concentrations is very hazardous but in low concentrations is very beneficial. The developed and validated method was short, precise, cost effective and reproducible with FID detector and easy to use. The method is a selective and superficial analytical method for determination of formic acid in different drug substances. We report here the development and validation study of headspace gas chromatographic method to determine formic acid in different drug substances we are reported here. As per this method, the drug sample was dissolved in 0.1% (v/v) of concentrated sulfuric acid in isopropyl alcohol (IPA) in a GC headspace vial and 0.1% (v/v) of concentrated sulfuric acid in isopropyl alcohol used as a diluent. A AB-Inowax capillary column (30 m x 0.32 mm I.D. and 0.5 µm film thickness) was used under gradient conditions with FID. The formic acid peak was well separated from all other solvents that are used in synthesis of particular drug substance. The LOD and LOQof the method for formic acid are 82 ppm and 249 ppm respectively. Formic acid are low toxic class-III solvent as per ICH guideline.

scholarly journals Identification of the Organic Volatile Impurities in Ezitamibe using GC-HS Technique

2021 ◽  
Vol 33 (3) ◽  
pp. 605-610
Author(s):  
Durgababu Rapeti ◽  
Kapavarapu Maruthi Venkata Narayanarao ◽  
Pulipaka Shyamala ◽  
Rallabhandi Murali Krishna
Keyword(s):  
Chromatographic Method ◽  
Isopropyl Alcohol ◽  
Organic Chemical ◽  
Dimethyl Formamide ◽  
Flame Ionization ◽  
Drug Substances ◽  
Periodic Analysis ◽  
Ionization Mode ◽  
Gas Chromatographic Method ◽  
Volatile Impurities

Ezetimibe prevents intestinal cholesterol synthesis, which in turn reduces the quantity of cholesterol and thereby helps to reduce heart problems and strokes. In the production of ezetimibe, several organic chemical solvents such as methanol, acetone, isopropyl alcohol, dichloromethane, n-hexane, ethyl acetate, tetrahydrofuran, toluene and dimethyl formamide were used. The measurement of residual solvents is necessary for release checks of all drug substances, based on sound manufacturing processes. The analysis of above mentioned nine solvents in ezetimibe drug was investigated using gas chromatographic method employing detection with flame ionization mode. All analyses were performed using ZB-624 column (30 m length × 0.53 mm identification, 3.0 μm thickness film). The column oven temperature flux was managed to maintain for 11 min at 40 ºC and then continued to upsurge to a temperature close of 240 ºC at a rate of 20 ºC/min and retained for 4 min. The flame ionization detector and injector port were managed at 260 and 200 ºC, respectively. Results after the validation of the gas chromatographic method showed the satisfactory linearity, sensitivity, robustness, accuracy, selectivity and precision for the tested organic solvents. This gas chromatographic approach can therefore be exploited in the assessment of studied nine residual chemical solvents for periodic analysis by gas chromatography for samples of ezetimibe drug.

scholarly journals A Headspace Gas Chromatographic Method for Determination of Formic Acid Content in Isosulfan Blue and Various Drug Substances

2021 ◽  
Vol 37 (02) ◽  
pp. 321-329
Author(s):  
Nilesh Takale ◽  
Neelakandan Kaliyaperumal ◽  
Gopalakrishnan Mannathusamy ◽  
Rajarajan Govindasamy
Keyword(s):  
Sulfuric Acid ◽  
Formic Acid ◽  
Chromatographic Method ◽  
Isopropyl Alcohol ◽  
Class Iii ◽  
Drug Substances ◽  
Headspace Gas ◽  
Concentrated Sulfuric Acid ◽  
Gas Chromatographic Method

The Pharmaceutical industry uses formic acid in the manufacturing of various drug substances or API. At the time of manufacturing of API formic acid is use as an oxidizing agent. Formic acid is the simplest carboxylic acid. It also called methanoic acid.Formic acid present in API at high concentrations is very hazardous but in low concentrations is very beneficial. The developed and validated method was short, precise, cost effective and reproducible with FID detector and easy to use. The method is a selective and superficial analytical method for determination of formic acid in different drug substances. We report here the development and validation study of headspace gas chromatographic method to determine formic acid in different drug substances we are reported here. As per this method, the drug sample was dissolved in 0.1% (v/v) of concentrated sulfuric acid in isopropyl alcohol (IPA) in a GC headspace vial and 0.1% (v/v) of concentrated sulfuric acid in isopropyl alcohol used as a diluent. A AB-Inowax capillary column (30 m x 0.32 mm I.D. and 0.5 µm film thickness) was used under gradient conditions with FID. The formic acid peak was well separated from all other solvents that are used in synthesis of particular drug substance. The LOD and LOQof the method for formic acid are 82 ppm and 249 ppm respectively. Formic acid are low toxic class-III solvent as per ICH guideline.

Headspace Gas Chromatographic Method for Determination of Ethanol in Canned Salmon: Collaborative Study

1986 ◽  
Vol 69 (3) ◽  
pp. 524-526
Author(s):  
Thomas A Hollingworth ◽  
Harold R Throm ◽  
Marleen M Wekell ◽  
William F Trager ◽  
Michael W O’Donnell ◽  
...  
Keyword(s):  
Chromatographic Method ◽  
Collaborative Study ◽  
Internal Standard ◽  
Sampling Technique ◽  
Flame Ionization ◽  
Coefficients Of Variation ◽  
Headspace Gas ◽  
The Mean ◽  
Gas Chromatographic Method

Abstract Six laboratories collaboratively studied a headspace gas chromatographic method for determination of ethanol in the aqueous phase of canned salmon. Ethanol is determined by a headspace sampling technique with tert-butanol as the internal standard, using a gas chromatograph equipped with a Super Q column and a flame ionization detector. With outliers excluded, the mean recoveries from samples spiked with 25.1 and 78.4 ppm ethanol were 112 and 110%, respectively. For the 4 sample pairs quantitated, repeatability coefficients of variation ranged from 1.42 to 4.25% and reproducibility coefficients of variation from 2.55 to 8.09%, with 3 of the 4 reported values less than 5%. The method has been adopted official first action.

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.

Stability-Indicating Method Development and Validation for Busulfan Drug Substance by Gas Chromatography-Flame Ionization Detector

2020 ◽  
Author(s):  
Ashraf Khan ◽  
Greg Winter ◽  
Shane Tan
Keyword(s):  
Gas Chromatography ◽  
Method Development ◽  
Fused Silica ◽  
Drug Substance ◽  
Forced Degradation ◽  
Stability Indicating ◽  
Flame Ionization ◽  
Stability Indicating Method ◽  
Organic Impurities ◽  
Chromatographic Parameters

Abstract A new, simple and stability-indicating gas chromatography-flame ionization detection (GC-FID) method was developed and validated for the quantitative determination of busulfan and its organic impurities (OI) in drug substance without derivatization. The chromatographic attributes were achieved on a fused silica capillary column (0.53 mm × 30 m, 1.0 μm, USP Phase G42), using hydrogen as a carrier gas with a split ratio of 1:1. Forced degradation studies were conducted to establish the stability-indicating capability and method specificity that showed the stressed busulfan peak was free from any co-elution. Robustness study demonstrated the chromatograms remained mostly unaffected under deliberate, but small variations of chromatographic parameters, establishing the reliability of the method during routine usage. The method was shown to be reliable, sensitive, specific, linear, accurate, precise and rugged in the 1,4-butanediol concentration range of 1–20 μg/mL. The method, intended for compendial uses, is suitable for quantitative analysis of busulfan and its organic impurities in drug substances.

Quantitative Multiresidue Analyses for Volatile Organics in Water and Milk, Using a Fused Silica Open-Tubular Wide-Bore Capillary Column and Automated Headspace Gas Chromatography

1990 ◽  
Vol 73 (2) ◽  
pp. 328-331
Author(s):  
Timothy P Mcneal ◽  
Henry C Hollifield
Keyword(s):  
Gas Chromatography ◽  
Capillary Column ◽  
Methylene Chloride ◽  
Capillary Columns ◽  
Fused Silica ◽  
Headspace Gas Chromatography ◽  
Flame Ionization ◽  
Headspace Gas ◽  
Standard Additions

Abstract A modified multiresidue capillary gas chromatographic (GC) procedure has been developed using automated headspace sampling and a wide-bore fused silica open-tubular (FSOT) capillary column for the determination of volatiles in water and milk. Compounds are quantltated by the method of standard additions. An IBM System 9000 computer with the CAPMC3 chromatographic applications package and a BASIC linear regression program are used for data reduction. Data are presented for solutions prepared by fortifying water and milk with volatile solvents such as acetone, methyl ethyl ketone, benzene, methylene chloride, and chloroform, which are commonly used in the manufacture of packaging materials and adheslves. The wide-bore FSOT capillary columns showed dramatically improved detection for certain compounds, compared with normal-bore capillary GC columns. Data presented for various chemicals demonstrate the improved limits of detection from the use of automated headspace gas chromatography with wide-bore capillary columns and flame ionization detection.

Ayurvedic formulations containing benzoic and ascorbic acids as additives: benzene formation during storage and impact of additives on quality parameters

2020 ◽  
Vol 0 (0) ◽  
Author(s):  
Priyanka Sharma ◽  
Mukesh Maithani ◽  
Vikas Gupta ◽  
Parveen Bansal
Keyword(s):  
Ascorbic Acid ◽  
Quality Parameters ◽  
Over The Counter ◽  
Flame Ionization ◽  
Class 1 ◽  
Short And Long Term ◽  
Pharmaceutical Industries ◽  
Increasing Demand ◽  
Gas Chromatographic Method ◽  
Ascorbic Acids

AbstractObjectivesAyurvedic formulations are becoming the prior choice of people as health care supplements. The increasing demand for these formulations has led to extensive development of Ayurvedic pharmaceutical industries worldwide. The reaction between the preservatives (sodium benzoates and ascorbic acid) used in these formulations could generate benzene. Benzene is classified as class-1 human carcinogen and responsible for various short and long term health effects.MethodsIn this study, 25 formulations (containing ascorbic acid and sodium benzoate) of various manufacturers available as over the counter products were obtained and their benzene content were determined using gas chromatograph with flame ionization detector.ResultsThe result showed that 64% of the formulations were free from benzene contamination whereas 36% of formulations were found to be contaminated with benzene. A simple, less time-consuming, economic, and validated gas chromatographic method for estimation of benzene in Ayurvedic formulations was also developed successfully in present study.ConclusionsThe data revealed that the level of benzene was within permissible limits, yet the presence of a carcinogen in the marketed formulations intended for internal use is an alarming situation.

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