Liquid Chromatographic Determination of Triadimefon in Technical and Formulated Products: Collaborative Study

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.

1986 ◽  
Vol 69 (5) ◽  
pp. 908-911
Author(s):  
Peter L Carter ◽  
Keith C Overton ◽  
◽  
P G Baker ◽  
O O Bennett ◽  
...  

Abstract A liquid chromatographic method for determination of bendiocarb in technical materials and wettable powders was tested by 12 collaborators. Bendiocarb is dissolved in acetonitrile containing 0.1% propiophenone as internal standard. This solution is analyzed on a liquid chromatograph utilizing a reverse phase (C18) column. The compound is detected at 254 nm and peak area is used for quantitation. The 3 different materials studied contained 20, 80, and nominally 100% bendiocarb. Each was examined in duplicate to provide the necessary matched pairs. Collaborators approved of the ease and simplicity of the method and, in particular, the way the method can be applied to automatic injection assemblies. The statistical data show acceptable precision of the method: Reproducibility coefficients of variation were 20% material, 2.04%; 80% material, 1.02%; and nominal 100% material (technical product), 0.64%. The method has been adopted official first action.


1985 ◽  
Vol 68 (3) ◽  
pp. 545-546
Author(s):  
Michael Tsougros

Abstract A stability indicating liquid chromatographic method for the determination of diazepam in tablets was collaboratively studied by 6 laboratories. The method uses a Cig reverse phase column, a methanolwater mobile phase, p-tolualdehyde as the internal standard, and photometric detection at 254 nm. The collaborators were supplied with a synthetic tablet powder and 3 commercial tablet samples. The mean recovery of diazepam from the synthetic tablet powder was 100.2%. For all samples analyzed, the coefficient of variation was < 1.5%. The method has been adopted 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.


1984 ◽  
Vol 67 (3) ◽  
pp. 497-499
Author(s):  
Stephen C Slahck ◽  
◽  
J B Audino ◽  
O O Bennett ◽  
B D Folsom ◽  
...  

Abstract A liquid chromatographic method for the determination of propoxur in technical and formulated products has been subjected to a collaborative study with 8 participating collaborators. Formulations are extracted with acetonitrile and analyzed by reverse phase chromatography, with n-butyrophenone as an internal standard. Collaborators were furnished with samples of technical, 70% wettable powder, 1.5 emulsifiable, and 2% bait. Coefficient of variation values obtained on the 4 samples were 0.34, 0.68, 3.25, and 5.41%, respectively. The method has been adopted official first action.


1983 ◽  
Vol 66 (4) ◽  
pp. 864-866
Author(s):  
Eileen S Bargo ◽  
◽  
E Aranda ◽  
C Bonnin ◽  
S Hauser ◽  
...  

Abstract A reverse phase high pressure liquid chromatographic method for the determination of oxazepam in tablets and capsules was collaboratively studied by 9 laboratories. Collaborators were supplied with 6 samples that included synthetic and commercial formulations. Tablet and capsule composites are diluted with methanol and filtered. Oxazepam is determined at 254 nm by using a C18 column. Mean recoveries of oxazepam from synthetic tablet and capsule formulations were 97.2 and 99.0%, respectively. Mean coefficients of variation for tablets and capsules ranged from 1.85 to 2.86%. The method has been adopted official first action.


1986 ◽  
Vol 69 (4) ◽  
pp. 594-597 ◽  
Author(s):  
Elia D Coppola ◽  
Martin S Starr ◽  
◽  
G H Chang ◽  
J DeVries ◽  
...  

Abstract Twelve laboratories collaboratively studied a liquid chromatographic method for determination of quinic, malic, and citric acids in cranberry juice cocktail and apple juice. Samples are passed through a disposable silica cartridge, filtered, and directly injected into the chromatograph. The mobile phase is 0.2M KH2PO4 (pH 2.4). Two reverse phase columns are used, with UV detection at 214 nm. Six samples of cranberry juice cocktail and 6 samples of apple juice were sent to each collaborator. Repeatability and reproducibility coefficients of variation ranged from 1.2 to 7.6% and from 2.9 to 14.7%, respectively, for quinic, malic, and citric acid levels above 0.10%. The precision of the method is satisfactory. The method has been adopted official first action.


1985 ◽  
Vol 68 (3) ◽  
pp. 567-569 ◽  
Author(s):  
Stephen C Slahck

Abstract An LC method for determination of aminocarb (Matacil™) in aminocarb technical and formulated products has been developed and subjected to a collaborative study with 10 participating collaborators. Formulations are extracted with tetrahydrofuran-buffer (60 + 40) and analyzed by reverse phase chromatography, with n-butyrophenone as internal standard. Collaborators were furnished with standards and samples of technical and 180 oil flowable products for analysis. Coefficients of variation obtained on these samples were 0.72 and 1.7%, respectively. The method has been adopted official first action.


1984 ◽  
Vol 67 (2) ◽  
pp. 218-221 ◽  
Author(s):  
Milda J Walters ◽  
◽  
N Falcone ◽  
K G Hanel ◽  
E H Jefferson ◽  
...  

Abstract A normal phase liquid chromatographic (LC) method for determining the hydrocortisone content of bulk drug substance, tablet composites, and individual tablets was subjected to a collaborative study by 6 laboratories. The results showed a mean recovery of 98.5% for an authentic tablet formulation and reproducibility coefficients of variation of 0.97, 1.6, and 2.7% for bulk drug substance, tablet composites, and individual tablets, respectively. Infrared (IR) and thin layer chromatographic (TLC) identification tests, also included in the collaborative study, were satisfactory. The LC method for determining hydrocortisone in bulk drug substance, tablet composites, and individual tablets, with IR and TLC identification, has been adopted official first action.


1977 ◽  
Vol 60 (4) ◽  
pp. 935-939 ◽  
Author(s):  
Harold F Hanel

Abstract Eight laboratories collaboratively studied a procedure for the quantitative determination of methaqualone. HCl in pharmaceutical and clandestine preparations. Methaqualone is extracted from an aqueous bicarbonate solution into chloroform and quantitated by gas-liquid chromatography on a 3% OV-1 column. Tetraphenylethylene is used as an internal standard. Two commercial preparations and 4 sample mixtures prepared by the author were studied. Recoveries for the 4 prepared samples ranged from 100.0 to 102.6%, and the coefficients of variation ranged from 1.58 to 4.15% for the 6 samples studied. The method has been adopted as official first action.


1988 ◽  
Vol 71 (1) ◽  
pp. 33-35
Author(s):  
Donald Shostak ◽  
Clifford Klein ◽  
◽  
C Cappon ◽  
N Falcone ◽  
...  

Abstract A liquid chromatographic method for the determination of flucytosine in capsules was collaboratively studied by 7 laboratories. The method uses a C18 reverse phase column, water-methanol-acetic acid mobile phase containing 1-octanesulfonic acid sodium salt, p-aminobenzoic acid as internal standard, and photometric detection at 285 nm. The mean recovery value (±SD) of flucytosine from a synthetic formulation representing capsules was 99.2 ± 1.72% (CV = 1.73%). Composited samples of 250 and 500 mg commercial capsules gave assay values of (mean ± SD) 103.17 ± 2.21 and 99.29 ± 1.29% of declared, respectively. CV values were 2.15 and 1.30%. Reproducibility and repeatability CVs were 2.19 and 1.50%, respectively, for the 250 mg capsules, and 1.34 and 0.63%, respectively, for the 500 mg capsules. The method has been adopted official first action.


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