GAS–LIQUID CHROMATOGRAPHY OF SOME FLAVONOID COMPOUNDS AND HYDROXY DIPHENYLS

1962 ◽  
Vol 40 (6) ◽  
pp. 1123-1129 ◽  
Author(s):  
N. Narasimhachari ◽  
E. Von Rudloff

Gas–liquid chromatography of the methyl ethers of 36 flavones, flavanones, isoflavones, and chalkones, 2 chromones, and 9 hydroxy diphenyls was carried out, using SE-30 silicone polymer as liquid phase. The results obtained show that this technique can be used for the separation, isolation, and identification of milligram amounts of these compounds. The influence of methylation, acetylation, and hydrogen bonding was demonstrated and is discussed. Dehydration of a 2-hydroxyisoflavanone to the corresponding isoflavone and isomerization between some flavanones and chalkones were encountered. No linear relationship between the number of substituents and retention time was obtained, indicating that substituents at different positions of a flavonoid nucleus influence the retention characteristics in a different manner. This was especially noticeable with some 3- and 5-substituted flavones, but in other instances the difference in retention times was also sufficient to differentiate between position isomers.

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.


1978 ◽  
Vol 61 (1) ◽  
pp. 68-71
Author(s):  
Dorothy K Wyatt ◽  
Lee T Grady

Abstract Gas-liquid chromatography (GLC) coupled with column chromatography was used to accurately determine as little as 25 ppm p-chloroacetanilide in acetaminophen. p-Chloroacetanilide was eluted from a pH 8 phosphate-buffered diatomite partition column by using purified tetrachloroethylene (acetaminophen was retained). This solution was concentrated, internal standard (docosane) was added, and p-chloroacetanilide was determined by using a 0.9 m × 2 mm glass column packed with 3% Poly A 103 on Supelcoport and a flame ionization detector with electronic integration. Standard curves were linear for 10–100 ppm p-chloroacetanilide. Various chromatographic materials were investigated for optimal retention characteristics. High pressure liquid chromatography (HPLC) was also evaluated as an alternative; however, lack of reproducibility of the HPLC column favored the GLC procedure.


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.


1973 ◽  
Vol 19 (4) ◽  
pp. 403-407 ◽  
Author(s):  
J. W. Carmichael ◽  
Awatar S. Sekhon ◽  
Lynne Sigler

Samples from dried colonies of 21 strains of Nannizzia and Arthroderma were analyzed by pyrolysis–gas–liquid chromatography. Characteristic peak patterns produced by all the strains were used as markers to correct random drift in retention time so that corresponding peaks in different pyrograms could be homologized. Variation in sample size was compensated for by comparing peaks on each pyrogram with a particular major component and scoring them simply as 0 (absent), 1 (small), or 2 (large). Proximities were calculated and analyzed for clusters by the TAXMAP procedure. The analysis always grouped replicate samples together in the same cluster. Opposite mating types of the same species were sometimes placed in the same cluster and sometimes in separate clusters. The (+) mating type of Arthroderma benhamiae was placed in a cluster with both mating types of Nannizzia gypsea and N. obtusa, while the (−) mating type replicates of A. benhamiae were placed in a cluster by themselves. Finding a greater difference between pyrograms of different mating types of one species than between pyrograms of different species was unexpected and requires further investigation.


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