scholarly journals DETERMINATION OF RESIDUAL DIMETHYL SULFATE IN METHOXSALEN DRUG SUBSTANCE BY PRE-COLUMN DERIVATIZATION WITH STATIC HEADSPACE GAS CHROMATOGRAPHY

2018 ◽  
Vol 10 (8) ◽  
pp. 84
Author(s):  
Ajit Anerao ◽  
Bhushan Patil ◽  
Nitin Pradhan
Keyword(s):  
Gas Chromatography ◽  
Method Development ◽  
Limit Of Detection ◽  
Dimethyl Sulfate ◽  
Drug Substance ◽  
Headspace Gas Chromatography ◽  
Limit Of Quantification ◽  
Static Headspace Gas Chromatography ◽  
Headspace Gas

Objective: Dimethyl sulfate has been highlighted as potential genotoxic and carcinogenic impurity. A sensitive Headspace gas chromatography (HS-GC) method with pre-column derivatization was developed and validated for the determination of dimethyl sulfate impurity in methoxsalen active pharmaceutical ingredient.Methods: HS-GC method on the column Agilent DB-5, 30m X 0.53 mm, film thickness 1.5 µm, with flame ionization detector (FID) was used. Derivatization reagent concentration, time of reaction and pH of the solution were optimized during method development. This analytical method was evaluated by performing method validation as per ICH guideline.Results: The proposed method was specific, linear, accurate, rugged and precise. The calibration curves showed good linearity over the concentration range of 0.5 μg/ml to 3.0 μg/ml and the correlation coefficient was 0.999. Method had very low limit of detection (LOD) and limit of quantification (LOQ) 2.0 μg/g and 5.0 μg/g respectively. Accuracy was observed within 98.1%–104.5%.Conclusion: The developed method was demonstrated to be accurate, robust and sensitive for the determination of dimethyl sulfate impurity in methoxsalen drug substance.

scholarly journals Microbes a Tool for the Remediation of Organotin Pollution Determined by Static Headspace Gas Chromatography-Mass Spectrometry

2018 ◽  
Author(s):  
Christopher Finnegan ◽  
David Ryan ◽  
Ann-Marie Enright ◽  
Guiomar Garcia-Cabellos
Keyword(s):  
Gas Chromatography ◽  
Limit Of Detection ◽  
Gas Chromatography Mass Spectrometry ◽  
Headspace Gas Chromatography ◽  
Static Headspace ◽  
Limit Of Quantification ◽  
Chromatography Method ◽  
Microbial Inoculant ◽  
Static Headspace Gas Chromatography ◽  
Headspace Gas

Tributyltin (TBT) is one of the most toxic anthropogenic compounds introduced into the marine environment. Despite its global ban in 2008, TBT is still a problem of great concern due to its high affinity for particulate matter, providing a direct and potentially persistent route of entry into benthic sediments. Bioremediation strategies may constitute an alternative approach to conventional physicochemical methods, benefiting from the microorganism’s potential to metabolize anthropogenic compounds. In this work, a simple, precise and accurate static headspace gas chromatography method was developed to investigate the ability of TBT degrading microbes in sedimentary microcosms over a period of 120 days. The proposed method was validated for linearity, repeatability, accuracy, specificity, limit of detection and limit of quantification. The method was subsequently successfully applied for the detection and quantification of TBT and degrading compounds in sediment samples on day 0, 30, 60, 90 and 120 of the experiment employing the principles of green chemistry. On day 120 the concentration of TBT remaining in the microcosms ranged between 91.91 ng/g wet wt for the least effective microbial inoculant to 52.73 ng/g wet wt for the most effective microbial inoculant from a stating concentration of 100 ng/g wet wt.

Determination of ethylene glycol in lubricants by derivatization static headspace gas chromatography

2015 ◽  
Vol 7 (13) ◽  
pp. 5545-5550 ◽  
Author(s):  
Kaelyn Gras ◽  
Jim Luong ◽  
Monica Lin ◽  
Ronda Gras ◽  
Robert A. Shellie
Keyword(s):  
Gas Chromatography ◽  
Ethylene Glycol ◽  
Reliable Method ◽  
Headspace Gas Chromatography ◽  
Static Headspace ◽  
Static Headspace Gas Chromatography ◽  
Headspace Gas ◽  
Synthetic Lubricants

A practical and reliable method for the analysis of ethylene glycol in either hydrocarbon based or synthetic lubricants has been successfully developed and implemented.

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