Collaborative Study of the Quantitative Determination of Fusel Oil and Ethyl Acetate by Gas-Liquid Chromatography

Abstract Thirteen chemists representing twelve laboratories participated in a collaborative study for the quantitative determination of ethyl acetate and fusel oil by GLC. The results on four samples containing various amounts of ethyl acetate and fusel oil were compared with the official AOAC procedures. For all samples, the standard deviations were lower with GLC. Collaborators preferred the GLC procedure because the simultaneous determination of ethyl acetate and n-propyl, iso-butyl, and isoamyl alcohols is possible. Results from preliminary work performed on the quantitative determination of acetaldehyde by GLC were encouraging. It is recommended that the proposed GLC procedure for the quantitative determination of ethyl acetate and fusel oil be adopted as official, first action, and that work be continvied on the determination of acetaldehyde by GLC.

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Collaborative Study of an Extension of the Mills et al. Method for the Determination of Pesticide Residues in Foods

Journal of AOAC INTERNATIONAL ◽

10.1093/jaoac/59.1.169 ◽

1976 ◽

Vol 59 (1) ◽

pp. 169-171

Author(s):

Charles E Finsterwalder

Keyword(s):

Liquid Chromatography ◽

Potassium Chloride ◽

Electron Capture ◽

Pesticide Residues ◽

Collaborative Study ◽

Heptachlor Epoxide ◽

Gas Liquid Chromatography ◽

Standard Deviations

Abstract Fifteen laboratories collaboratively determined parathion, o,p′-DDT, p,p′-DDT, and p,p′-DDE in kale, and lindane, dieldrin, heptachlor epoxide, and p,p′-DDE in eggs, using electron capture gas-liquid chromatography (potassium chloride thermionic detector for parathion). Pesticide levels ranged from 0.033 ppm heptachlor epoxide to 3.32 ppm p,p′-DDT. Mean recoveries (± standard deviations) were: parathion 91±15%, o,p′-DDT 99±8%, p,p′-DDT 97±8%, lindane 94±4%, dieldrin 106±8%, heptachlor epoxide 106±5%, p,p′-DDE 94±8% in eggs and 101±9% in kale. The methods have been adopted as official first action.

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Collaborative Study of Gas-Liquid Chromatographic Determination of Methaqualone in Pharmaceutical and Clandestine Preparations

Journal of AOAC INTERNATIONAL ◽

10.1093/jaoac/60.4.935 ◽

1977 ◽

Vol 60 (4) ◽

pp. 935-939 ◽

Cited By ~ 1

Author(s):

Harold F Hanel

Keyword(s):

Liquid Chromatography ◽

Quantitative Determination ◽

Collaborative Study ◽

Internal Standard ◽

Chromatographic Determination ◽

Gas Liquid Chromatography ◽

Coefficients Of Variation ◽

Liquid Chromatographic Determination ◽

Liquid Chromatographic

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.

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Evaluation of Gas-Liquid Chromatography for the Quantitative Determination of Fusel Oil in Distilled Spirits

Journal of AOAC INTERNATIONAL ◽

10.1093/jaoac/50.2.322 ◽

1967 ◽

Vol 50 (2) ◽

pp. 322-329

Author(s):

Richard L Brunelle

Keyword(s):

Liquid Chromatography ◽

Quantitative Determination ◽

Oil Content ◽

Gas Liquid Chromatography ◽

Fusel Oil ◽

Distilled Spirits ◽

Collaborative Studies ◽

Aoac Method ◽

Official Procedure

Abstract Gas-liquid chromatography (GLC) was compared to the official AOAC method for the quantitative determination of fusel oil in distilled spirits on 12 samples by 12 collaborators. Results indicated that the GLC procedure described is at least as accurate as the official procedure. Analyses of 26 distilled spirits samples showed that the GLC method was sensitive and capable of reproducing fusel oil content in the 0—10 g/100 L range to ± 0.03 g/100 L. It is recommended that collaborative studies be conducted on the GLC determination of fusel oil, and that work be extended to include analysis of other important congeners in distilled spirits such as ethyl acetate, acetaldehyde, and methanol.

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Quantitative Determination of Chlorobutanol in Milk by Gas-Liquid Chromatography

Journal of AOAC INTERNATIONAL ◽

10.1093/jaoac/55.5.948 ◽

1972 ◽

Vol 55 (5) ◽

pp. 948-950

Author(s):

John E Wiskerchen ◽

Joseph Weishaar

Keyword(s):

Liquid Chromatography ◽

Quantitative Determination ◽

Electron Capture ◽

Steam Distillation ◽

Collaborative Study ◽

Electron Capture Detection ◽

Gas Liquid Chromatography

Abstract A method is described for the quantitative determination of chlorobutanol in milk by gas-liquid chromatography. The cleanup includes isolation of chlorobutanol from milk by steam distillation and extraction with ether. The chlorobutanol is quantitatively determined on a column of 5% Igepal 880 on Gas-Chrom Q with electron capture detection. Recoveries were 87–101% for milk fortified at 0.01–10 ppm levels. Collaborative study is recommended after an intralaboratory study is completed.

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Quantitative Determination of Ammonium Glycyrrhizinate by Gas-Liquid Chromatography: Collaborative Study

Journal of AOAC INTERNATIONAL ◽

10.1093/jaoac/55.3.570 ◽

1972 ◽

Vol 55 (3) ◽

pp. 570-572

Author(s):

Damon Larry

Keyword(s):

Liquid Chromatography ◽

Quantitative Determination ◽

Collaborative Study ◽

Gas Liquid Chromatography ◽

Carbonated Beverage ◽

Made In

Abstract Six samples of carbonated beverage were spiked at levels from 0 to 400 p pm with foodgrade ammonium glycyrrhizinate and sent to 7 participating laboratories for collaborative study. To facilitate the analysis of samples containing microquantities of ammonium glycyrrhizinate, slight modifications were made in the published GLC method. Recoveries of ammon ium glycyrrhizinate were 116.4, 102.0, 93.4, 102.3, and 105.8% for 35, 100, 200, 300, and 400 ppm levels, respectively. The method has been adopted as official first action.

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