DETERMINATION OF RESIDUAL METHYL IODIDE IN TEDIZOLID PHOSPHATE AND ALOGLIPTIN BENZOATE BY STATIC HEADSPACE GAS CHROMATOGRAPHY WITH ELECTRON CAPTURE DETECTION

INDIAN DRUGS ◽  
2017 ◽  
Vol 54 (11) ◽  
pp. 39-45
Author(s):  
A. Anerao ◽  
◽  
B Patil ◽  
R Jaguste ◽  
N. Pradhan
Keyword(s):  
Electron Capture ◽  
Methyl Iodide ◽  
Limit Of Detection ◽  
Active Pharmaceutical Ingredient ◽  
Electron Capture Detection ◽  
Static Headspace Gas Chromatography ◽  
Quality Control Tool ◽  
Headspace Gas ◽  
Test Concentration

Methyl iodide has been highlighted as a potential genotoxic impurity (PGI). A sensitive HS-GC method with ECD was developed and validated for the determination of methyl iodide impurity in Tedizolid phosphate, an active pharmaceutical ingredient. HS-GC method on DB-624,column 60m X 0.53mm, film thickness 3μm, with electron capture detector (ECD) was used. The proposed method was specific, linear, accurate, rugged and precise. The calibration curves showed good linearity over the concentration range of 0.78 μg/g to 11.7 μg/g and the correlation coefficient was 0.997. Method had very low limit of detection (LOD) and limits of quantification (LOQ) are 0.23 μg/g and 0.78 μg/g, respectively, with respect to test concentration. Accuracy was observed within the range 96.0% to 103.2%. This method is a further extended good quality control tool for low level quantitation of methyl iodide impurity in another API, alogliptin benzoate.

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.

Gas Chromatographic Determination Of Residue Levels Of The Herbicides Trifluralin, Benefin, Ethalfluralin, And Isopropalin In Soil With Confirmation By Mass Selective Detection

1988 ◽  
Vol 71 (6) ◽  
pp. 1082-1085 ◽  
Author(s):  
Sheldon D West ◽  
Jack H Weston ◽  
Edgar W Day
Keyword(s):  
Gas Chromatography ◽  
Electron Capture ◽  
Limit Of Detection ◽  
Detection System ◽  
Gas Chromatography Mass Spectrometry ◽  
Electron Capture Detection ◽  
Selective Detection ◽  
Mass Selective Detector ◽  
Selective Detector

Abstract A method is presented for the simultaneous or individual determination of the dinitroaniline herbicides trifluralin, benefin, ethalfluralin, and isopropalin in soil. The herbicides are extracted with acetonitrile- water (99 + 1), and the extracts are purified with small, disposable Florisil cartridges prior to analysis by gas chromatography using an electron capture detector or a mass selective detector. When electron capture detection is used as the primary detection system, confirmation with selective detection can be obtained using gas chromatography-mass spectrometry with a mass selective detector and a capillary column operated in the split mode. The limit of detection is 0.01 ppm, and recoveries averaged 95-112% for the 4 herbicides in several different soil types fortified at levels of 0.01- 0.33 ppm

scholarly journals Low Level Determinations of Methyl Methanesulfonate and Ethyl Methanesulfonate Impurities in Emtricitabine Active Pharmaceutical Ingredient by LC/MS/MS using Electrospray Ionization

2011 ◽  
Vol 6 ◽  
pp. ACI.S6471 ◽  
Author(s):  
P.R. Kakadiya ◽  
T.G. Chandrashekhar ◽  
S. Ganguly ◽  
D.K. Singh ◽  
V. Singh
Keyword(s):  
Electrospray Ionization ◽  
Limit Of Detection ◽  
Multiple Reaction Monitoring ◽  
Active Pharmaceutical Ingredient ◽  
Case Method ◽  
Limit Of Quantification ◽  
Low Level ◽  
Quality Control Tool ◽  
Genotoxic Impurities

Alkyl methanesulfonates have been highlighted as potential genotoxic impurities (PGIs). A sensitive LC/MS/MS method was developed and validated for the determination of Alkyl methanesulfonate impurities in Emtricitabine API (active pharmaceutical ingredient). LC/MS/MS method on Zorbax SB C18 column (150 × 4.6 mm i.d.), 3.5 μm, with electrospray ionization (ESI) in multiple reaction monitoring (MRM) mode was used. The proposed method was specific, linear, accurate, rugged and precise. The calibration curves showed good linearity over the concentration range of 0.0025 μg/ml to 0.3 μg/ml the correlation coefficient was >0.999 in each case. Method had very low limit of detection (LOD) and limit of quantification (LOQ) as 0.3 μg/g and 0.4 μg/g respectively for both the analytes. Accuracy was observed within 80%-120% for both the analytes. This method can be further extended a good quality control tool for low level quantitation of Alkyl methanesulfonate impurities in other API.

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