THE SEPARATION OF SOME TERPENOID COMPOUNDS BY GAS–LIQUID CHROMATOGRAPHY

1960 ◽  
Vol 38 (5) ◽  
pp. 631-640 ◽  
Author(s):  
E. von Rudloff
Keyword(s):  
Liquid Chromatography ◽  
Polyethylene Glycol ◽  
Liquid Phase ◽  
Diatomaceous Earth ◽  
Solid Support ◽  
Gas Liquid Chromatography ◽  
Polyphenyl Ether ◽  
Liquid Phases ◽  
Degree Of Separation ◽  
Separation Of Mixtures

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.

GAS–LIQUID CHROMATOGRAPHY OF TERPENES: PART III. THE USE OF OLEIC ACID ESTERS AS LIQUID PHASES

1961 ◽  
Vol 39 (6) ◽  
pp. 1190-1199 ◽  
Author(s):  
E. von Rudloff
Keyword(s):  
Liquid Phase ◽  
Rapeseed Oil ◽  
Hydroxyl Groups ◽  
Gas Liquid Chromatography ◽  
Retention Data ◽  
Geometrical Isomers ◽  
Potassium Oleate ◽  
Liquid Phases ◽  
Degree Of Separation ◽  
Poly Ethylene

The separation of several cyclic terpene hydrocarbons and some oxygenated derivatives was studied on a variety of triglyceride and dioleate ester columns. Use of rapeseed oil, partially hydrogenated rapeseed oil, olive oil, triolein, tristearin, methyl oleate, and potassium oleate as liquid phases led to the conclusion that the presence of an esterified mono-unsaturated long-chain acid is a desirable constituent of the liquid phase. Dioleate esters of 1,3-propanediol, 1,4-butanediol, 1,6-hexanediol, diethylene glycol, and polyethylene glycol showed useful differences in the degree of separation of both terpene hydrocarbons and oxygenated derivatives. Ether linkages, as in the di- and poly-ethylene glycol ester, also were associated with favorable separations. When the liquid phase contained free hydroxyl groups, the degree of separation of hydrocarbons and ketones was in general less favorable. The spacing of the ester groups was found to have some effect on retention data. The separation of such critical pairs of isomers as tricyclene and α-pinene, α-fenchene and camphene, and also geometrical isomers of oxygenated derivatives is facilitated by use of several of these liquid phases.

Quantitative Determination of Benzaldehyde in Flavors by Gas-Liquid Chromatography

1963 ◽  
Vol 46 (6) ◽  
pp. 950-951
Author(s):  
Richard L Brunelle ◽  
Glenn E Martin
Keyword(s):  
Liquid Chromatography ◽  
Liquid Phase ◽  
Benzoic Acid ◽  
Quantitative Determination ◽  
Solid Support ◽  
Specific Method ◽  
Gas Liquid Chromatography ◽  
Ultraviolet Spectrophotometry ◽  
Liquid Chromatography Separation

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.

Fusel Oil Determination by Gas-Liquid Chromatography

1963 ◽  
Vol 46 (2) ◽  
pp. 294-297
Author(s):  
Glenn E Martin ◽  
Gian Caggiano ◽  
Howard Schlesinger
Keyword(s):  
Liquid Chromatography ◽  
Liquid Phase ◽  
Isothermal Condition ◽  
Solid Support ◽  
Gas Liquid Chromatography ◽  
Fusel Oil ◽  
Liquid Chromatography Separation

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.

Gas-liquid chromatography of undervatized drugs after chromatographic extraction from blood.

1979 ◽  
Vol 25 (12) ◽  
pp. 2020-2025 ◽  
Author(s):  
M Werner ◽  
R J Mohrbacher ◽  
C J Riendeau
Keyword(s):  
Liquid Chromatography ◽  
Liquid Phase ◽  
Gas Liquid Chromatography ◽  
Gastric Aspirate ◽  
Chemical Derivatization ◽  
Integrated Method ◽  
Relative Retention ◽  
Liquid Phases ◽  
Precision And Accuracy ◽  
Chromatographic Extraction

Abstract We have developed an integrated method that overcomes the two main procedural difficulties of gas-liquid chromatography, namely, solvent-solvent extraction and chemical derivatization. Drugs are extracted from serum by column chromatography on granular diatomaceous earth (kieselguhr). Subsequent gas-liquid chromatography of underivatized samples can be performed on either of two liquid phases. A mixed liquid phase, used for quantitative gas-chromatographic assay on patients with a known therapeutic regimen, has enabled quantitation of 12 drugs in serum. Alternatively, a single liquid phase, used with the mixed liquid phase, permits the gas-chromatographic identification of unknown drugs on the basis of the characteristic pattern of the two relative retention times; by this approach more than 40 drugs have been identified in cases of suspected intoxication, both in serum and in gastric aspirate. Besides providing ease of performance and wide applicability, the proposed procedure offers a degree of precision and accuracy that compares favorably with established methods.

Gas—Liquid Chromatographic Measurement of Guanidino Acids

1975 ◽  
Vol 21 (7) ◽  
pp. 838-843 ◽  
Author(s):  
Harini Patel ◽  
Burton D Cohen
Keyword(s):  
Nuclear Magnetic Resonance ◽  
Liquid Chromatography ◽  
Liquid Phase ◽  
Magnetic Resonance ◽  
Gas Liquid Chromatography ◽  
Butyl Esters ◽  
Silicone Liquid ◽  
Chromatographic Measurement ◽  
Liquid Chromatographic

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.

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