Gas-Liquid Chromatographic Determination of Nikethamide in Injectable Preparations

1976 ◽  
Vol 59 (1) ◽  
pp. 93-97 ◽  
Author(s):  
John M Newton

Abstract A gas-liquid chromatographic (GLC) method, using a 4% XE-60 on 80-100 mesh Gas-Chrom Q column, a flame ionization detector, and anthracene as the internal standard, has been developed for the direct determination of nikethamide. Eight collaborators analyzed 4 samples, using methanol as the solvent; the coefficients of variation obtained ranged from 1.19 to 3.20%. In a limited study with acetone as the solvent, the coefficients of variation ranged from 0.59 to 1.96%. The GLC method with acetone as a solvent has been adopted as official first action.

1981 ◽  
Vol 64 (4) ◽  
pp. 829-832
Author(s):  
Bram Van Rossum ◽  
Albertus Martijn ◽  
James E Launer ◽  
◽  
E C Calamita ◽  
...  

Abstract The gas-liquid chromatographic determination of tetradifon technical and formulations was collaboratively studied in duplicate with 12 laboratories. Six samples were dissolved in dichloroethane with n-hexacosane as the internal standard, chromatographed on a column of 3% SE-52, and detected by flame ionization. The average coefficients of variation were 1.2% for the 2 technical samples, 1.6% for the 2 wettable powders, and 1.5% for the 2 emulsifiable concentrates. The method has been adopted official first action.


1977 ◽  
Vol 60 (6) ◽  
pp. 1341-1344
Author(s):  
David G Prue ◽  
Raymond N Johnson ◽  
Boen T Kho

Abstract A gas-liquid chromatographic (GLC) method is described for determining isosorbide dinitrate (ISDN) in tablets. ISDN is extracted from tablet excipients by a 2-phase system composed of water-ethyl ether, and detected and quantitated with a flame ionization detector after separation from the internal standard (glyceryl tributyrate) on a 3% OV-210 column. Ten replicate assays on 2 different batches of tablets, each containing 5 mg ISDN, gave coefficients of variation of 1.16 and 1.48%, respectively. Comparison of results obtained for tablets containing 5, 10, and 40 mg ISDN, and for diluted isosorbide dinitrate raw material containing 25% ISDN, showed good correlation among the GLC, USP colorimetric, and USP polarographic procedures. Assay of synthetic mixtures containing ISDN, isosorbide-2-mononitrate, and isosorbide-5-mononitrate demonstrated that the GLC procedure is specific for ISDN, whereas the USP polarographic procedure is subject to interference from the mononitrates.


1975 ◽  
Vol 58 (4) ◽  
pp. 845-849
Author(s):  
Vernon J Meinen

Abstract A gas-liquid chromatographic (GLC) method is described for the quantitative determination of /V-octylbicycloheptene dicarboximide (MGK 264 synergist) in technical materials and in various formulations. The samples are diluted with acetone and analyzed by GLC, using a flame ionization detector and a column packed with OV-1 on Chromosorb W (HP). Preliminary work indicates that satisfactory results can be obtained with the technical material and several different formulations.


1978 ◽  
Vol 61 (1) ◽  
pp. 164-166
Author(s):  
Fred A Moseley ◽  
Joel S Salinsky ◽  
Robert W Woods

Abstract A rapid and simple method of analysis has been developed for sorbitol in cooked sausage products. Sorbitol is extracted from cooked sausage products with water, an aliquot of the extract is freeze-dried, and the trimethylsilyl (TMS) derivative of sorbitol is formed. An aliquot of the TMS-sorbitol is injected into a gas chromatograph and measured by a flame ionization detector. Analysis of fortified samples shows that the recovery compares well with known amounts of sorbitol added.


1975 ◽  
Vol 58 (5) ◽  
pp. 1032-1036
Author(s):  
Richard A Simonaitis ◽  
R Spencer Cail

Abstract gas-liquid chromatographic (GLC) method was developed for the determination of residues of resmethrin ((5-benzyl-3-furyl)methyl cistraras-(±)- 2,2-dimethyl-3-(2-methylpropenyl)-cyclopropanecarboxylate) in corn, cornmeal, flour, and wheat. The commodity, fortified with resmethrin, was extracted by tumbling with pentane and transferred to acetonitrile, the fat was partitioned off, and the sample was chromatographed with 3% ethyl acetate in pentane on Florisil containing 0.5% water. The resmethrin residue was determined by GLC with a flame ionization detector. The results were compared with known standards that had undergone the same cleanup procedures. The method was sensitive to concentrations of resmethrin to 0.2 ppm, recoveries averaged 83%, and reproducibility was good.


1978 ◽  
Vol 61 (3) ◽  
pp. 561-563
Author(s):  
Robert L Smallidge

Abstract A gas-liquid chromatographic method is presented for determining ethopabate in 0.8 and 8.0% premixes. A sample is extracted with tetrahydrofuran containing an internal standard, by sonication or overnight soaking. The extract is clarified by centrifugation, diluted if necessary, and injected into a gas chromatograph equipped with a flame ionization detector. Average per cent recoveries for spiked blank samples were 100.6 at the 0.8% level and 100.4 at the 8.0% level. Precision, as indicated by replicate analyses of several premixes, ranged from 0.5 to 1.7% relative standard deviation


1980 ◽  
Vol 63 (1) ◽  
pp. 33-36
Author(s):  
Molly I Keating

Abstract A rapid method for the analysis of dip washes is described which eliminates the usual solvent extraction procedure. The dip wash is initially diluted with acetone and then with petroleum ether. The diluted dip wash is analyzed by gasliquid chromatography, using an alkali ionization detector sensitive to phosphorus compounds. The method was applied to the determination of dioxathion (2,3-ρ-dioxanedithiol S,S-bis(O,O-diethyl phosphorodithioate)), and quintiofos (O-ethyl O-8-quinolyl phenylphosphonothioate) dip washes. Average recoveries from fouled dip washes were 100 and 104%. GLC of these compounds with an internal standard is described, which improves the precision of the method to ±2%.


1985 ◽  
Vol 68 (3) ◽  
pp. 586-589
Author(s):  
Stephen C Slahck

Abstract A liquid chromatographic method for the determination of triadimefon (Bayleton™) in triadimefon technical and formulated products has been developed and subjected to a collaborative study with 7 participating collaborators. Formulations were extracted with mobile solvent and analyzed by normal phase chromatography, with 4-chlorophenyl sulfoxide as an internal standard. Collaborators were furnished with standards and samples of technical products, 50% wettable powders, and 25% wettable powders for analysis. Coefficients of variation of the values obtained on these samples were 1.42, 0.82, and 1.05%, respectively. The method has been adopted official first action.


1978 ◽  
Vol 61 (1) ◽  
pp. 161-163
Author(s):  
Giuseppe Cellerino ◽  
Mariarosa Re

Abstract Simultaneous determination of the active ingredient and of by-products in technical and formulated pyridazinones was rapidly performed by gas-liquid chromatography with complete resolution of all compounds. Quantitative determination by the internal standard technique is accurate and precise. The lower limit of detectability is 8 × 10–12 g/sec with a flame ionization detector and 1 × 10–12 g/sec with a nitrogen-phosphorus selective detector operating in the nitrogen mode.


1978 ◽  
Vol 61 (1) ◽  
pp. 68-71
Author(s):  
Dorothy K Wyatt ◽  
Lee T Grady

Abstract Gas-liquid chromatography (GLC) coupled with column chromatography was used to accurately determine as little as 25 ppm p-chloroacetanilide in acetaminophen. p-Chloroacetanilide was eluted from a pH 8 phosphate-buffered diatomite partition column by using purified tetrachloroethylene (acetaminophen was retained). This solution was concentrated, internal standard (docosane) was added, and p-chloroacetanilide was determined by using a 0.9 m × 2 mm glass column packed with 3% Poly A 103 on Supelcoport and a flame ionization detector with electronic integration. Standard curves were linear for 10–100 ppm p-chloroacetanilide. Various chromatographic materials were investigated for optimal retention characteristics. High pressure liquid chromatography (HPLC) was also evaluated as an alternative; however, lack of reproducibility of the HPLC column favored the GLC procedure.


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