Gas Chromatographic Determination of Fluazifop-butyl in Formulations: Collaborative Study

1984 ◽  
Vol 67 (3) ◽  
pp. 499-502
Author(s):  
Peter D Bland ◽  
◽  
L Chenery ◽  
N Ellis ◽  
L Firestone ◽  
...  

Abstract A method is described for the determination of butyl 2-(4-(5-trifluoromethyl- 2-pyridinyloxy)phenoxy) propanoate in technical and formulated material by gas chromatography (GC). Samples of technical or formulated material are dissolved in methylene chloride containing dibenzyl succinate as internal standard. The solution is injected into a gas chromatograph fitted with a flame ionization detector and a 6 ft × 2 mm glass column. The column is packed with 3% OV-17 on 100–120 mesh Chromosorb WHP and is maintained at 230°C. Peak areas obtained at the retention times of the internal standard and the active ingredient are measured with an integrator. The quantity of fluazifop-butyl is determined by comparing the internal standard and active ingredient peak areas with the peak areas obtained from a calibration solution containing known amounts of internal standard and pure active ingredient. Four samples were chosen for collaboration: technical fluazifop-butyl, a 4 lb/US gal. emulsifiable concentrate, a 560 g/L oil concentrate, and a 5% granular. Fourteen collaborators carried out replicate determinations on each sample. Coefficients of variation between laboratories were 0.80 for the technical, 0.88 for the emulsifiable concentrate, 1.03 for the oil concentrate, and 2.04 for the granular. Parallel peak height determinations showed substantially higher coefficients of variation for all except the granular sample. The method has been adopted official first action.

1985 ◽  
Vol 68 (3) ◽  
pp. 592-595
Author(s):  
Peter D Bland

Abstract A method is described for the determination of cypermethrin, 3-(2,2- dichloroethenyl)-2,2-dimethyl-cyclopropanecarboxylate cyano-(3- phenoxyphenyl)methyl ester, in technical and formulated material by capillary gas chromatography (CGC). Samples of technical or formulated material are dissolved in CH2Cl2 containing dicyclohexyl phthalate as internal standard. The solution is injected into a gas chromatograph fitted with a flame ionization detector and capillary column of 25 m x 0.32 mm fused silica with a thick film OV-1 phase at 240°C. Injection is made into a heated injection port fitted with an antidiscrimination device in a split mode. Peak areas obtained at retention times of the internal standard and active ingredient are measured with an integrator. The quantity of cypermethrin is determined by comparing the internal standard and active ingredient peak areas with those obtained from a calibration solution containing known amounts of internal standard and pure active ingredient. Five samples were chosen for collaborative study: technical cypermethrin, 70% liquid concentrate, 3 lb/US gal. emulsifiable, 3 ib/US gal. oil concentrate, and 40% wettable powder. Twelve collaborators carried out replicate determinations on each sample on separate days. Coefficients of variation between laboratories (CVX) were 2.13 for the technical, 2.94 for the emulsifiable concentrate, 3.51 for the liquid concentrate, 2.66 for the wettable powder, and 2.29 for the oil concentrate. The method was adopted official first action.


1984 ◽  
Vol 67 (4) ◽  
pp. 840-843
Author(s):  
William R Betker ◽  
◽  
D Anderson ◽  
J M Bajovich ◽  
O O Bennett ◽  
...  

Abstract A collaborative study was conducted on a gas chromatographic method for determining metribuzin. Two 75% dry flow able and two 42% liquid flowable formulations were analyzed by 18 laboratories. Formulations were extracted by shaking or ultrasonic mixing for 1-5 min with methylene chloride which contained di-n-butyl phthalate as an internal standard. The extracts were injected into a gas chromatograph equipped with an OV-225 column. Peak area ratios and peak height ratios showed no significant difference. The reproducibility coefficient of variation was 0.75% for the 75% formulation and 1.41% for the 42% formulation. This GC method has been adopted official first action.


1986 ◽  
Vol 69 (3) ◽  
pp. 488-490
Author(s):  
William R Betker ◽  
◽  
E W Balcer ◽  
O O Bennett ◽  
W R Coffman ◽  
...  

Abstract A collaborative study was conducted on a gas chromatographic method for determination of fensulfothion. Eleven laboratories analyzed 2 technical and two 6 lb/U.S. gal. spray concentrate samples. In the analysis, samples are dissolved in methylene chloride which contains 4-chlorophenyl sulfoxide as an internal standard, and solutions are injected into a gas chromatograph equipped with an OV-330 column. Withinlaboratory repeatability was 0.79% for technical product and 0.37% for the spray concentrate samples, with coefficients of variation of 0.88 and 0.58%, respectively. Among-laboratories reproducibility was 0.81% for technical product and 0.53% for the spray concentrate, with coefficients of variation of 0.91 and 0.84%, respectively. The method has been adopted official first action.


1985 ◽  
Vol 68 (3) ◽  
pp. 570-572
Author(s):  
Thomas G Gale ◽  
Arthur H Hofberg

Abstract A gas chromatographic (GC) procedure for the determination of metolachlor in emulsifiable concentrate formulations containing about 76% active ingredient was collaboratively studied using the matched pair scheme. Metolachlor was extracted from the formulation with acetone containing dipentyl phthalate as the internal standard, chromatographed on OV-101, and detected by flame ionization. Determinations on the 4 samples by 21 government, university, and industrial collaborators using peak area measurements showed within-laboratory repeatability of better than 0.5%. Reproducibility was better than 1% for the formulation. The method has been adopted official first action.


1987 ◽  
Vol 70 (6) ◽  
pp. 967-973
Author(s):  
Elaine A Bunch

Abstract A normal phase liquid chromatographic method for the determination of dexamethasone in bulk drugs and elixirs was collaboratively studied by 6 laboratories. The method uses a silica column, water-modified acetic acid-methanol-methylene chloride mobile phase, cortisone internal standard, and photometric detection at 254 nm. Collaborators were supplied blind duplicate samples of 3 bulk drugs, 2 commercial elixirs, and 1 authentic elixir. Dexamethasone elixir dosage level is 0.5 mg/5 tnL. Mean recovery of dexamethasone from the authentic elixir formulated to contain 0.471 mg/5 mL was 94.5%. (Authentic elixirs were found to stabilize about 6% below the theoretical concentration.) Mean recovery for the bulk drugs was between 97.1 and 100.1%. Mean coefficients of variation for bulk drug and elixir samples were less than 0.8% and 3.6%, respectively. Identification tests for dexamethasone by thin-layer chromatography, infrared spectroscopy, and relative LC retention times, as well as the gas chromatographic determination of alcohol in the elixirs were also collaboratively studied. Mean recovery of alcohol from the synthetic elixir was 98.6%. The mean coefficient of variation for alcohol for all samples analyzed was less than 1.4%. The LC method for dexamethasone in drug substance and elixirs, the identification tests, and the GC method for alcohol in dexamethasone elixirs have been adopted official first action.


1985 ◽  
Vol 68 (3) ◽  
pp. 589-592
Author(s):  
Thomas G Gale ◽  
Arthur H Hofberg

Abstract Agaschromatographic (GC) procedure for the determination of chlordimeform in emulsiflable concentrate formulations containing about 46% active ingredient was collaboratively studied using the matched pair scheme. Chlordimeform was extracted from the formulation with methylene chloride containing diethyl terephthalate as the internal standard, chromatographed on CBWX-20M, and detected by flame ionization. Determinations on the 4 samples by 20 government, university, and industrial collaborators using peak area measurements showed within-laboratory repeatability of better than 1%. Reproducibility was 1.2% for the formulation. 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.


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.


1992 ◽  
Vol 75 (6) ◽  
pp. 1103-1106
Author(s):  
Benjamin A Belkind

Abstract An isocratic normal-phase liquid chromatographic (LC) method for measuring methazole in technical and formulated products was collaboratively studied by 12 laboratories. Samples of technical or formulated products are dissolved in 1,4-dioxane-hexane containing 2-chloro-5-nitrobenzophenone as internal standard. Following centrifugation and further dilution, the sample is analyzed by LC on a 25 cm x 4.6 mm stainless steel column packed with 5 μm silica, with ultraviolet detection at 254 nm. Premixed 1% 2-propanol in hexane is used as the mobile phase. Peak areas are obtained at the retention times corresponding to the internal standard and methazole. The quantity of active ingredient is determined by comparing the area ratio of active ingredient to internal standard in the sample with the same ratio in a single calibration solution. Collaborators were provided with 1 Youden matched pair for each of the technical, 75% wettable granular, and 4 lb/gal flowable products studied. The reproducibility relative standard deviations (RSDR) for the product types studied were 1.05% for technical, 1.80% for granular, and 4.76% for flowable. The method has been adopted first action by AOAC International.


1977 ◽  
Vol 60 (3) ◽  
pp. 724-727
Author(s):  
Edwin R Jackson

Abstract Methyl parathion in technical material, 4 lb/gal. emulsifiable concentrate, and 6 lb toxaphene-3 lb methyl parathion/gal. emulsifiable concentrate was chromatographed on microparticulate silica with 40% water-saturated chloroform mobile phase and 254 nm ultraviolet detection. Ten collaborators reported results on 3 matched pairs of samples by peak height measurements with acetophenone as internal standard. The mean of the coefficients of variation for the 6 samples was 1.71%. Results for 4 of the samples were compared with gas-liquid chromatographic results on the same samples. No difference in the means by the 2 methods was noted at the 95% confidence level. The method has been adopted as official first action.


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