Collaborative Study of the Quantitative Gas-Liquid Chromatographic Determination of Fusel Oil and Other Components in Whisky

1972 ◽  
Vol 55 (3) ◽  
pp. 549-556
Author(s):  
J H Kahn ◽  
E T Blessinger
Keyword(s):  
Ethyl Acetate ◽  
Collaborative Study ◽  
Chromatographic Determination ◽  
Official Method ◽  
Fusel Oil ◽  
Fusel Alcohols ◽  
Aoac Method ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract Fifteen chemists participated in a collaborative study for the quantitative pas-liquid chromatographic determination of the individual fusel alcohols and ethyl acetate in whisky. Two levels of congeners represented by 4 coded samples of whisky were analyzed by using t h e proposed method, employing a glycerol-1,2,6-hexanetriol column, and the official AOAC method, 9.063-9.065. Since isobutyl and the atnyl alcohols comprise by far the greatest part of fusel oil, their determination is of major importance to the total fusel oil content . Statistical analyses show that the proposed method is superior to the AOAC method for the determination of these alcohols, whereas the official method is superior for the determination of ethyl acetate and n-propyl alcohol. In general, collaborators employing modern instrumentation preferred the proposed method over the AOAC method. The former method also separates and permits the quantitative measurement of active amyl and isoamyl alcohols. The proposed method has been adopted as official first action as an alternative to 9.063–9.065 for the determination of higher alcohols and ethyl acetate in whisky.

Liquid Chromatographic Determination of Vanillin and Related Flavor Compounds in Vanilla Extract: Cooperative Study

1985 ◽  
Vol 68 (6) ◽  
pp. 1198-1201 ◽  
Author(s):  
Philip A Guarino ◽  
Susan M Brown
Keyword(s):  
Collaborative Study ◽  
Chromatographic Determination ◽  
Technical Committee ◽  
Flavor Compounds ◽  
Official Method ◽  
Ethyl Vanillin ◽  
Liquid Chromatographic Determination ◽  
Phase Liquid ◽  
Liquid Chromatographic

Abstract Vanillin and related flavor compounds present in vanilla extract were determined by reverse phase liquid chromatography. Results compared favorably with the official AOAC spectrophotometric method. Compounds such as p-hydroxybenzaldehyde and ethyl vanillin known to interfere in the official method were resolved from vanillin. The method was evaluated by 6 industrial laboratories under the aegis of the Technical Committee of the Flavor and Extract Manufacturers Association. The method is suggested for AOAC collaborative study.

High Pressure Liquid Chromatographic Determination of Monoand Disaccharides in Presweetened Cereals: Collaborative Study

1982 ◽  
Vol 65 (2) ◽  
pp. 256-264 ◽  
Author(s):  
Lucian C Zygmunt ◽  
◽  
E Anderson ◽  
B Behrens ◽  
R Bowers ◽  
...  
Keyword(s):  
High Pressure ◽  
Collaborative Study ◽  
Chromatographic Determination ◽  
Hplc Method ◽  
High Pressure Liquid Chromatographic ◽  
Aoac Method ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic ◽  
Water Alcohol

Abstract A collaborative study was conducted using a modified AOAC method (sugars in chocolate) for the determination of fructose, glucose, sucrose, and maltose in presweetened cereals by high pressure liquid chromatography (HPLC). Eight samples consisting of 6 products were analyzed in duplicate by the HPLC method and the AOAC Lane-Eynon method. The AOAC method was modified to use water-alcohol (1 + 1) and Sep-Pak C18 cartridges for sample cleanup. The HPLC results indicate precision comparable to the Lane-Eynon method and the chocolate method. The modified HPLC method has been adopted official first action.

Liquid Chromatographic Determination of Glyphosate and Aminomethylphosphonic Acid (AMPA) in Environmental Water: Collaborative Study

1991 ◽  
Vol 74 (2) ◽  
pp. 317-323 ◽  
Author(s):  
Mark E Oppenhuizen ◽  
John E Cowell
Keyword(s):  
Collaborative Study ◽  
Chromatographic Determination ◽  
Environmental Water ◽  
Aminomethylphosphonic Acid ◽  
Relative Standard ◽  
Total Variability ◽  
Liquid Chromatographic Determination ◽  
Predicted Values ◽  
Liquid Chromatographic

Abstract A new method for determination of glyphosate and amlnomethylphosphonlc acid (AMPA) residues In environmental water was collaboratively studied by 6 laboratories. The method Is simpler and shorter than previous methods. A filtered volume of water is evaporated to dryness and the residue Is dissolved In a buffered EDTA solution. Glyphosate and AMPA are determined by liquid chromatography with postcolumn reaction detection. The method was validated over the range 0.50-5000 ppb, although one of the collaborating laboratories could not reliably quantltate below 1.0 ppb. Statistical analysis of the results showed that typical reproducibility relative standard deviations (RSDR) ranged from 11 to 20% for both glyphosate and AMPA, which compares very well with predicted values for this concentration range. Total variability (as measured by sR) Increased with increasing fortification level. The method has been adopted official first action by AOAC.

Liquid Chromatographic Determination of Diazepam in Tablets: Collaborative Study

1985 ◽  
Vol 68 (3) ◽  
pp. 545-546
Author(s):  
Michael Tsougros
Keyword(s):  
Collaborative Study ◽  
Internal Standard ◽  
Chromatographic Determination ◽  
Reverse Phase ◽  
Photometric Detection ◽  
Liquid Chromatographic Method ◽  
Liquid Chromatographic Determination ◽  
The Mean ◽  
Liquid Chromatographic

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.

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

1984 ◽  
Vol 67 (3) ◽  
pp. 492-493
Author(s):  
Stephen C Slahck ◽  
◽  
A A Carlstrom ◽  
L T Chenery ◽  
N D Ellis ◽  
...  
Keyword(s):  
Coefficient Of Variation ◽  
Collaborative Study ◽  
Internal Standard ◽  
Chromatographic Determination ◽  
Reverse Phase ◽  
Reverse Phase Chromatography ◽  
Wettable Powder ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract An LC method for the determination of methiocarb in methiocarb technical and formulated products has been subjected to a collaborative study with 9 participating collaborators. Formulations are extracted with acetonitrile and analyzed by reverse phase chromatography, with acetophenone as an internal standard. Collaborators were furnished samples of technical, 75% wettable powder, 75% seed treater, 75% concentrate, and 50% hopper box treater. Coefficient of variation values obtained on the 5 samples were 0.71, 0.83, 0.62, 1.57, and 0.82%, respectively. The method has been adopted official first action.

Improved Liquid Chromatographic Determination of Riboflavin in Milk and Dairy Products

1985 ◽  
Vol 68 (4) ◽  
pp. 693-696 ◽  
Author(s):  
Samy H Ashoor ◽  
Michael J Knox ◽  
Jacquelyn R Olsen, ◽  
Dru Ann Deger
Keyword(s):  
Dairy Products ◽  
Chromatographic Determination ◽  
Simple Liquid ◽  
Uv Detector ◽  
Aoac Method ◽  
Total Analysis ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic ◽  
Milk And Dairy Products

Abstract Reported here is a simple liquid chromatographic (LC) method for the i determination of riboflavin in milk (liquid, evaporated, and dry), yogurt, ' and cheese. The method involves passing liquid samples or filtrates of semisolid and solid samples through a Clg cartridge. Retained riboflavin is then eluted with an aliquot of 50% methanol in 0.02M acetate buffer of pH 4. A volume of the eluate is injected into the LC system | consisting of a CJ8 column, a solvent of water-methanol-acetic acid (65 + 35 + 0.1, v/v) with a flow rate of 1 mL/min, and a UV detector set at 270 nm. The method is precise and accurate and compares i favorably with the present AOAC method. Moreover, it involves fewer sample preparation steps and has a total analysis time of less than 1 h.

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

1986 ◽  
Vol 69 (5) ◽  
pp. 915-918
Author(s):  
Edward J Kikta ◽  
◽  
E Bane ◽  
A Burns ◽  
A Christensen ◽  
...  
Keyword(s):  
Mobile Phase ◽  
Collaborative Study ◽  
Internal Standard ◽  
Chromatographic Determination ◽  
Data Sets ◽  
Matched Pairs ◽  
Reverse Phase ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract A liquid chromatographic (LC) method for the analysis of technical and formulated carbofuran samples was evaluated in a collaborative study. Carbofuran is determined by reverse phase LC, using a water-methanol mobile phase and acetophenone as internal standard, and detected at 280 nm. Twelve samples, 5 formulations and technical matched pairs, were analyzed by 17 collaborating laboratories. Accuracy and variability of results are typical of large LC data sets. The method has been adopted official first action.

Gas-Liquid Chromatographic Determination of Tetradif on Technical and Formulations: Collaborative Study

1981 ◽  
Vol 64 (4) ◽  
pp. 829-832
Author(s):  
Bram Van Rossum ◽  
Albertus Martijn ◽  
James E Launer ◽  
◽  
E C Calamita ◽  
...  
Keyword(s):  
Collaborative Study ◽  
Internal Standard ◽  
Chromatographic Determination ◽  
Flame Ionization ◽  
Coefficients Of Variation ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

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.

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

1985 ◽  
Vol 68 (3) ◽  
pp. 586-589
Author(s):  
Stephen C Slahck
Keyword(s):  
Collaborative Study ◽  
Internal Standard ◽  
Chromatographic Determination ◽  
Normal Phase ◽  
Coefficients Of Variation ◽  
Liquid Chromatographic Method ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic ◽  
Technical Products

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.

Liquid Chromatographic Determination of Morphine Sulfate and Some Contaminants in Injections and Bulk Drug Material: Collaborative Study

1988 ◽  
Vol 71 (5) ◽  
pp. 1046-1048
Author(s):  
Ada C Bello ◽  
Rita K Jhangiani
Keyword(s):  
Collaborative Study ◽  
Chromatographic Determination ◽  
Morphine Sulfate ◽  
System Suitability ◽  
Liquid Chromatographic Method ◽  
Relative Standard ◽  
Liquid Chromatographic Determination ◽  
Bulk Drug ◽  
Liquid Chromatographic

Abstract A liquid chromatographic method for the assay of morphine sulfate and some preservatives and impurities in the bulk drug and in injections has been developed and collaboratively studied in 8 laboratories. Each collaborator analyzed 5 samples: 1 bulk drug, 3 different concentrations of injectable dosages, and 1 prepared mixture containing, in addition to morphine sulfate, phenol, 2-mercaptobenzothiazole, and pseudomorphine. The proposed method quantitates morphine sulfate and resolves the other components for identification using a Clg reverse-phase column with a mobile solvent containing 240 mL methanol, 720 mL 0.005M 1-heptanesulfonic acid Na salt, and 10 mL acetic acid. Samples are prepared by direct dilution with mobile solvent minus 1-heptanesulfonic acid. All collaborators met system suitability requirements and performed the analysis without difficulty. No outliers were found when data were analyzed by the Dixon, Grubbs, double Grubbs, and Cochran tests. Relative standard deviations between laboratories (RSDR) for duplicate determinations of morphine sulfate ranged from 1.4 to 2.1%. Mean morphine sulfate recoveries for the bulk drug and the prepared mixture were 100.8 and 100.4%, respectively. The method has been approved interim official first action.

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