Fusel Oil Determination by Gas-Liquid Chromatography

1963 ◽  
Vol 46 (2) ◽  
pp. 294-297
Author(s):  
Glenn E Martin ◽  
Gian Caggiano ◽  
Howard Schlesinger

Abstract A method was developed for the determination of fusel oil by gas-liquid chromatography. Separation is effected in a ¼” column containing 20% Ucon polar as the liquid phase, on a solid support of Gas Chrom P at isothermal condition 90° C. The method is simple and expeditious, and the amount of each component alcohol can be determined individually.

1963 ◽  
Vol 46 (6) ◽  
pp. 950-951
Author(s):  
Richard L Brunelle ◽  
Glenn E Martin

Abstract A rapid and specific method is given for determination of benzaldehyde in the presence of interfering substances by gas-liquid chromatography. Separation is effected on a ¼ column containing 2 5% Apiezon M as the liquid phase on a solid support of Chromoport XXX (60—80 mesh) at isothermal conditions, 100°C. The determination can be performed in the presence of benzoic acid and other interfering substances. Results are compared with those obtained by ultraviolet spectrophotometry on a variety of almond and cherry flavors.


1960 ◽  
Vol 38 (5) ◽  
pp. 631-640 ◽  
Author(s):  
E. von Rudloff

A study has been made of the degree of separation of mixtures of some terpene hydrocarbons, some of their oxygenated derivatives, two sesquiterpene alcohols, and three monophenols on a variety of columns. Temperature and sample size affected the degree of separation and the solid support Chromosorb W, a calcined diatomaceous earth, was found to combine the advantages of Celite and C-22 firebrick without causing decomposition of the sample at higher temperatures. When Craig polyesters were used as liquid phases, separations equal to those obtained on polyethylene glycol were realized with the added advantage that these produced columns which are stable at 190 to 220 °C. Consequently, sesquiterpene alcohols and monophenols were also separated successfully. Another useful liquid phase for both low and high temperatures was found in a meta-linked polyphenyl ether. Squalene was found to be an efficient liquid phase for the separation of terpene hydrocarbons at 130 °C and lower. The possible application of the present findings for preparative work is discussed.


1975 ◽  
Vol 21 (7) ◽  
pp. 838-843 ◽  
Author(s):  
Harini Patel ◽  
Burton D Cohen

Abstract We present a method for separating and measuring guanidino acids by gas—liquid chromatography. Compared to ion-exchange techniques, this system is faster, more sensitive, requires smaller sample volumes, is independent of colorimetric reactions, and permits simultaneous determination of both amino and guanidino acids. N-Trifluoroacetyl-n-butyl esters are formed and then are separated by using a column containing a mixed silicone liquid phase coated on Chromosorb W-HP. Analytical recoveries from plasma ranged from 86 to 112% and were optimal when purification and derivatization were done without prior protein precipitation. Speculations as to the cause of this interference by protein include coprecipitation, protein-binding, and cyclization of the guanidines in the acids used for denaturation. Evidence presented suggests that all three occur: ultrafiltrability is diminished in the presence of protein and nuclear magnetic resonance demonstrates cyclization of some of these esters.


1968 ◽  
Vol 51 (4) ◽  
pp. 915-921
Author(s):  
Richard L Brunelle

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.


1983 ◽  
Vol 2 (2) ◽  
pp. 391-393 ◽  
Author(s):  
D. Martinez ◽  
M.P. Gimenez

1 A method for determining amphetamine and methylamphetamine in urine by gas-liquid chromatography is described. 2 Chromatography is performed on a 10% Apiezon L, 10% KOH column with alkali-flame detection (NPD). This method avoids the losses of these volatile substances which are known to occur when solvent extraction is used. An alkalinized urine sample (1 ml) is introduced into a sealed vial which is heated in a water bath at 70°C for 20 min. A 1 ml portion of the gas phase in equilibrium with the liquid phase is chromatographed. 3 Amphetamine and methylamphetamine can be detected and measured in urine samples after single therapeutic doses of the drugs.


1967 ◽  
Vol 50 (2) ◽  
pp. 322-329
Author(s):  
Richard L Brunelle

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.


1974 ◽  
Vol 57 (4) ◽  
pp. 954-956
Author(s):  
Robert G Parker

Abstract In the method described, anethole is extracted from the liqueur sample with chloroform, which eliminates interference from the large amount of sugar present, and is determined by gas-liquid chromatography, using 10% K-20M Carbowax as stationary phase on Chromosorb W (AWDMCS) as solid support. Anethole concentrations were measured in 8 different bottle samples, consisting of 4 different brands produced by 3 different manufacturers. There is a significant difference in the anethole concentration for the 4 brands tested.


1971 ◽  
Vol 67 (2) ◽  
pp. 303-315 ◽  
Author(s):  
A. J. Moolenaar ◽  
A. P. van Seters

ABSTRACT The 17-oxosteroids were estimated in the urine of 27 patients with Cushing's syndrome by gas-liquid chromatography (G. L. C.). The values of the various steroid fractions are compared with those of normal subjects, patients with thyrotoxicosis and obese subjects. The effect of the age of the patients on the diagnostic value of the invidual 17-oxosteroids and their ratios is discussed.


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