An Analytical Method for Trifluoroacetic Acid in Water and Air Samples Using Headspace Gas Chromatographic Determination of the Methyl Ester

1996 ◽  
Vol 68 (19) ◽  
pp. 3450-3459 ◽  
Author(s):  
Dov Zehavi ◽  
James N. Seiber
Author(s):  
Kishorkumar L. Mule

Objective: To develop and validate new, simple and rapid assay method for Prochlorperazine edisylate drug substance by UPLC as per ICH guidelines.Methods: Ultra performance liquid chromatographic method was developed, optimized and validated on Acquity UPLC by using Acquity BDH300 C4 (100 x 2.1 mm) 1.7µ column. 3.85g ammonium acetate in 1000 ml of water add 0.5 ml trifluoroacetic acid and 1 ml triethylamine (Mobile phase A): 0.5 ml trifluoroacetic acid in 1000 ml acetonitrile mobile phase (Mobile phase B) with gradient program. Detector wavelength 254 nm and column temperature 30 °C.Results: Linearity study was carried out for prochlorperazine edisylate, linearity was calculated from 80 % level to 120% with respect to specification level. The correlation coefficient (r) = 0.999 was proved that the method is robust. The resolution between known impurities and Prochlorperazine edisylate found more than 2.5, it was evident from specificity test that Prochlorperazine edisylate peak are well separated from its related impurities, hence the method is specific. Prochlorperazine edisylate sample solution and mobile phase were found to be stable for at least 3 d.Conclusion: A new, simple and rapid method has been developed and validated for assay determination of prochlorperazine edisylate in drug substance by Ultra Performance Liquid Chromatography (UPLC). The analytical method was developed and validated as per ICH guidelines. The developed method can be used for the fast assay determination of prochlorperazine edisylate drug substances in research laboratories and in the pharmaceutical industry. 


1986 ◽  
Vol 21 (12) ◽  
pp. 701-704 ◽  
Author(s):  
R. Binetti ◽  
S. Di Marzio ◽  
P. Di Prospero ◽  
L. Gramiccioni ◽  
G. Viviano ◽  
...  

1976 ◽  
Vol 48 (9) ◽  
pp. 1395-1398 ◽  
Author(s):  
R. H. Hill ◽  
C. S. McCammon ◽  
A. T. Saalwaechter ◽  
A. W. Teass ◽  
W. J. Woodfin

1982 ◽  
Vol 65 (5) ◽  
pp. 1066-1072
Author(s):  
Brian D Ripley ◽  
Bruce J French ◽  
Lloyd V Edgington

Abstract An analytical method is described for the determination of mono- and dialkylamines in foodstuffs. Amines are derivatized to their pentafluorobenzamides which may be separated by gas chromatography (GC) and determined using an N-P detector. Analysis of the derivatives by GC-mass spectrometry indicated they were all mono-substituted. The amines were isolated from foodstuffs by alkaline distillation of ≥75% sample volume. The distribution of dimethylamine (DMA) in distillate volumes indicated 2 maxima from barley and malt, which could represent 2 or more sources of DMA. DMA concentrations of 6.6-8.8 ppm in barley, 11 ppm in malt, and 1.2 ppm in beer are higher than previously reported.


1967 ◽  
Vol 50 (3) ◽  
pp. 637-641
Author(s):  
J G Saha ◽  
L A Gadallah

Abstract A method is presented for determining the herbicide tordon (4-amino-3,5,6-trichIoropicolinic acid) in soil. It involves extraction of tordon as the free acid with acetone and phosphoric acid, followed by esterification with diazomethane and estimation of the methyl ester by electron capture gas chromatography. Recoveries of tordon added to soil samples at 0.05—1.0 ppm were between 83 and 92%. The minimum amount detectable by this method was 0.01 ppm. The difficulties of developing an analytical method for this compound are discussed in the light of its structure and solubility


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