The synthesis, separation, and identification of the methyl ethers of arabinose and their derivatives

1967 ◽  
Vol 45 (3) ◽  
pp. 275-290 ◽  
Author(s):  
S. C. Williams ◽  
J. K. N. Jones
Keyword(s):  
Reducing Sugars ◽  
Reducing Sugar ◽  
The Other ◽  
Partition Chromatography ◽  
Ring Form ◽  
Optical Rotations ◽  
Layer Chromatography ◽  
Derivatives Of ◽  
Spray Reagents

A study has been made of various methods available for the identification and separation of the methyl ethers of arabinose. Gas–liquid partition chromatography has been used to separate the acetylated glycosides and the acetylated alditols of the methyl ethers of arabinose. All of the methyl ethers of arabinopyranose and arabinofuranose have been separated by paper chromatography. Several spray reagents have been used to distinguish between those methyl ethers with similar rates of movement. Thin-layer chromatography has been used to separate the methyl glycosides, acetylated methyl glycosides, and glycitols of the methyl ethers of arabinose, as well as the methyl ethers of the reducing sugar. The optical rotations of the reducing sugars and of the methyl glycosides of the methyl ethers of arabinose provide information about the ring form and, in the case of the glycosides, about the anomer present. The rotations of the acetylated and unacetylated O-methyl arabinitols aid in the determination of the position of the methyl substitutents. In connection with this study, all of the mono-O-methyl and tri-O-methyl, and most of the di-O-methyl ethers of arabinose have been synthesized. New syntheses have been devised for 4-O-methyl and 2,3-di-O-methyl arabinose, and the other sugars have been synthesized by known or partially revised syntheses. During this work, previously unreported derivatives of these sugars have been prepared.

THE SEPARATION, DETERMINATION, AND CHARACTERIZATION OF 2-AMINO-2-DEOXY-D-GLUCOSE (D-GLUCOSAMINE) AND 2-AMINO-2-DEOXY-D-GALACTOSE (D-GALACTOSAMINE) IN BIOLOGICAL MATERIALS BY GAS–LIQUID PARTITION CHROMATOGRAPHY

1964 ◽  
Vol 42 (4) ◽  
pp. 451-460 ◽  
Author(s):  
M. B. Perry
Keyword(s):  
Hyaluronic Acid ◽  
Chondroitin Sulphate ◽  
Chromatographic Determination ◽  
Partition Chromatography ◽  
Quantitative Analyses ◽  
Optical Rotations ◽  
Trimethylsilyl Derivatives ◽  
Quantitative Procedure

A method for the separation, determination, and characterization of 2-amino-2-deoxy-D-glucose (D-glucosamine) and 2-amino-2-deoxy-D-galactose (D-galactosamine) is presented. Treatment of 2-acetamido-2-deoxy-α-D-glucose and 2-acetamido-2-deoxy-α-D-galactose in pyridine solution with trimethylchlorosilane and hexamethyldisilazane results in a rapid conversion of the glycoses to their respective trimethylsilyl 3,4,6-tri-O-trimethylsilyl-2-acetamido-2-deoxy-α-D-glycosides which are sufficiently stable and volatile to allow their separation and quantitative analysis to be made by gas–liquid partition chromatography. The two trimethylsilyl derivatives, collected by preparative gas–liquid partition chromatography, were crystalline compounds which had sharp melting points and characteristic infrared spectra and specific optical rotations. Quantitative analyses of mixtures of 2-amino-2-deoxy-D-glucose hydrochloride and 2-amino-2-deoxy-D-galactose hydrochloride were made by gas chromatographic analysis of their trimethylsilyl derivatives formed after prior conversion to their N-acetyl derivatives.The analytical procedure was applied to the characterization of 2-amino-2-deoxy-D-glucose in hyaluronic acid and 2-amino-2-deoxy-D-galactose in chondroitin sulphate. The quantitative procedure was also successfully applied to the analysis of mixtures of hyaluronic acid and chrondroitin sulphate by the gas–liquid partition chromatographic determination of the 2-amino-2-deoxy-D-glucose and 2-amino-2-deoxy-D-galactose in the hydrolyzates prepared from synthetic mixtures of the two mucopolysaccharides.

scholarly journals Determination of conversion rate values to characterise the ethanol production of the Kluyveromyces marxianus CBS712 fungus branch

2010 ◽  
pp. 23-27
Author(s):  
Éva Erdei ◽  
István Pócsi ◽  
Mónika Molnár ◽  
Gyöngyi Gyémánt ◽  
János Nagy
Keyword(s):  
Thin Layer ◽  
Ethanol Production ◽  
Kluyveromyces Marxianus ◽  
Conversion Rate ◽  
The Other ◽  
Conversion Rates ◽  
Residual Glucose ◽  
Oxidase Enzyme ◽  
Layer Chromatography

The ethanol production of the Kluyveromyces marxianus CBS712 strain was investigated among different kind of condition. We defined the conversion rate in order to know the efficiency of the ethanol production. To determine this value, it is crucial to characterize the residual glucose concentracio. We chose two method to determine the amount of residual glucose. The first method is the thin layer chromatography (TLC) and the second method is the method of the glucose-oxidase enzyme. We found that the TLC method is reliable than the other method. The conversion rates were determined from these values and the ethanol values. The maximal ethanol production of the characterized Kluyveromyces marxianus CBS712 strain (5.6% (v/v) ethanol at 45 °C, 55.3% conversion rate) is comparable to those strains which are applied in industrial ethanol production nowadays.

Preservatives in Cosmetics: Partition Chromatography and Ultraviolet Spectrophotometry

1975 ◽  
Vol 58 (5) ◽  
pp. 937-940 ◽  
Author(s):  
E Patricia Sheppard ◽  
Clifton H Wilson
Keyword(s):  
Absorption Maximum ◽  
The Other ◽  
Uv Spectrophotometry ◽  
Chromatographic Technique ◽  
Partition Chromatography ◽  
Cosmetic Products ◽  
Ultraviolet Spectrophotometry ◽  
Broad Applicability

Abstract Separation by partition chromatography and determination by ultraviolet (UV) spectrophotometry have been applied to the analysis of 16 preservative chemicals used in cosmetic products. The method, adapted from the official first action method for hexachlorophene, 35.023–35.027, has broad applicability for the determination of preservatives in cosmetics. Among the chemical classes investigated, phenols, parabens, biphenyls, carbanilides, and salicylanilides are represented. The partition chromatographic technique does not separate 3,4’,5-tribromosalicylanilide (TBS) from hexachlorophene or Irgasan DP 300. However, the UV determination of these compounds was accomplished by utilizing an absorption maximum of TBS which does not coincide with that of the other 2 preservatives. Recoveries averaged 97% for all the compounds studied.

Determination of Matacil and Zectran by Fluorigenic Labeling, Thin Layer Chromatography, and In Situ Fluorimetry

1972 ◽  
Vol 55 (6) ◽  
pp. 1259-1264
Author(s):  
R W Frei ◽  
J F Lawrence
Keyword(s):  
Thin Layer ◽  
Thin Layer Chromatography ◽  
Sulfonyl Chloride ◽  
Relative Standard ◽  
Dansyl Derivatives ◽  
Layer Chromatography ◽  
Derivatives Of ◽  
Fluorescent Derivatives

Abstract The fluorigenic labeling of Matacil (4-dimethylamino- m-tolyl N-methylcarbamate) and Zectran (4-dimethylamino-3,5-xylyl Wmethylcarbamate) with dansyl chloride (1-dimethylamino- naphthalene-5-sulfonyl chloride) results in 3 fluorescent derivatives, and labeling with NBD-Cl (4-chloro-7-nitrobenzo- 2,1,3-oxadiazole) produces 2 fluorescent derivatives for each carbamate, all of which can be separated by thin layer chromatography (TLC). These derivatives are identified by nuclear magnetic resonance, infrared, and fluorescence spectroscopy, aided by TLC data. The carbamates are hydrolyzed in dilute base and the resulting amine or phenol hydrolysis products react with the labeling reagents. The derivatives are analyzed by TLC and in situ fluorimetry with a spectrophotometer in the fluorescence mode and a spectrophotofluorometer with the thin layer scanning accessory. Reactions, fluorescence phenomena, and chromatographic properties of the derivatives are investigated for evaluation of the method as a quantitative technique. A reproducibility of 3–5% relative standard deviation can be expected in the concentration range from 15 to 300 ng/spot for derivatives of the 2 labeling procedures. The dansyl derivatives are instrumentally detectable as low as 1 ng/spot while the NBD derivatives may be detected at concentrations of less than 0.5 mg/spot.

EXCRETION OF BILE ACIDS BY THREE MEN ON A FAT-FREE DIET

1966 ◽  
Vol 44 (6) ◽  
pp. 957-969 ◽  
Author(s):  
S. S. Ali ◽  
A. Kuksis ◽  
J. M. R. Beveridge
Keyword(s):  
Liquid Chromatography ◽  
Thin Layer ◽  
Bile Acids ◽  
The Other ◽  
Total Output ◽  
Gas Liquid Chromatography ◽  
Fecal Bile Acids ◽  
Layer Chromatography ◽  
Total Excretion

A combination of thin-layer chromatography and gas–liquid chromatography was used for the separation and determination of fecal bile acids in three middle-aged men during the last 4 days of three 8-day periods on a fat-free diet. The range of the total output was 130–650 mg/day. Lithocholic and deoxycholic acids were the major components and accounted for 65–80% of the total excretion of bile acids. Other common bile acids were present in considerably smaller quantities (0.5–11% each). In addition, evidence was obtained for the presence of a number of as yet unreported fecal bile acids. These were tentatively identified as 3α,12β-dihydroxy-, 3β,12β-dihydroxy-, 3α,7β-dihydroxy-, 3α-monohydroxy-7-keto-, 12α-monohydroxy-3-keto-, and 7β-monohydroxy-cholanic and cholanic acids. The latter three acids occurred in traces only, but the other uncommon fecal bile acids each accounted for 0.5–7% of the total excretion of bile acids. Significant variations were found in the concentrations of several of the bile acids both between different samples from the same subject and between samples from different subjects.

scholarly journals The distribution of polyphenols in the tea plant (Camellia sinensis L.)

1969 ◽  
Vol 113 (5) ◽  
pp. 741-755 ◽  
Author(s):  
G. I. Forrest ◽  
D S Bendall
Keyword(s):  
Tea Plant ◽  
Steady Increase ◽  
Protective Layers ◽  
Mature Leaves ◽  
High Concentrations ◽  
Root Apices ◽  
Layer Chromatography ◽  
Derivatives Of ◽  
Ring Hydroxylation

1. Methods for the separation and determination of the polyphenolic components of the tea plant by thin-layer chromatography and colorimetric reactions have been devised. 2. High concentrations of catechins, flavonols and depsides were found to be restricted to the young vegetative and floral shoots, whereas leucoanthocyanins or flavylogens were characteristic of the more bulky axial tissues of the plant. 3. In the young shoots cell growth was correlated with an increasing degree of flavonoid B-ring hydroxylation. 4. Maximal flavylogen concentrations occurred in the outer protective layers of stem and of seed coat. 5. Mature leaves were shown to contain derivatives of the flavones apigenin and luteolin. 6. Developing seedlings showed a steady increase in polyphenol complexity; flavylogens were concentrated at shoot and root apices and accumulated at the stem base. 7. It is postulated that the flavanols (leucoanthocyanins and catechins), because they can co-polymerize, are of use to the plant for protection of wood and bark against infection and decay.

Moire´ Patterns of Partial Derivatives of Displacement Components

1966 ◽  
Vol 33 (4) ◽  
pp. 901-906 ◽  
Author(s):  
V. J. Parks ◽  
A. J. Durelli
Keyword(s):  
Nonlinear Deformation ◽  
Strain Tensor ◽  
Strain Analysis ◽  
The Other ◽  
Partial Derivatives ◽  
Moire Patterns ◽  
Derivatives Of ◽  
Moiré Patterns

The knowledge of the partial derivatives of displacement components is essential in strain analysis. Two methods of determining these partial derivatives using moire´ effects are presented in this paper. One consists of superposing two shifted copies of the same deformed grating of lines. The other consists of superposing two shifted copies of moire´ patterns of displacement components. Explanations of the phenomena, based on the parametric properties of superposed families of lines, are given. Applications to the determination of the nonlinear deformation and strain tensor are included.

scholarly journals DETERMINATION OF LUPEOL FROM MAKHAEN AT THAILAND AND TAIWAN BY HIGHPERFORMANCE LIQUID CHROMATOGRAPHY

2019 ◽  
pp. 49-51
Author(s):  
SURACHAI TECHAOEI ◽  
KHEMJIRA JARMKOM ◽  
NAKUNTWALAI WISIDSRI ◽  
SURADWADEE THUNGMUNGMEE ◽  
WARACHATE KHOBJAI
Keyword(s):  
Experimental Study ◽  
Antimicrobial Activity ◽  
Liquid Chromatography ◽  
Chemical Compounds ◽  
Bioactive Compound ◽  
The Other ◽  
Chiang Mai ◽  
Highperformance Liquid Chromatography ◽  
Layer Chromatography

Objective: The objective of this research was to investigate the extraction and isolation of chemical compounds of Zanthoxylum limonella Alstonextracts which selected from Chiang Mai and Pa Yao province, Thailand and Taiwan.Method: There are 3 locations of medicinal plant, Z. limonella Alston was collected, two provinces of northern Thailand, Chiang Mai and Phayao,including the other country, Taiwan. All of extractions were carried out by methanol. In this experimental study, thin-layer chromatography (TLC) andhigh-performance liquid chromatography (HPLC) were measured.Results: The result was found that the best organic solvent for extraction is methanol. The suitable of extraction was methanol and toluene in the ratioof 9:1 when developed with TLC and gradient methanol and water when analyzed with HPLC. The potential bioactive compound from crude extractedwas lupeol. Crude extracted from leaf at Chiang Mai was highest lupeol as 5655.72 μg/mg extraction whereas crude extracted from leaf at Phayaoshowed this compound as 16, 98.81 μg/mg extraction. In addition, the crude extraction from root and bark of both areas showed the amount of lupeolless than leaf crude extracted. The further study will focus on antimicrobial activity and biological activity in the near future.Conclusion: The bioactive compound, lupeol was found in all part of Makhaen in Thailand but did not found in Taiwan seed.

Determination of Vitamins D2 and D3 in Pharmaceuticals by Gas-Liquid Chromatography

1968 ◽  
Vol 51 (4) ◽  
pp. 839-840
Author(s):  
T K Murray ◽  
P Erdody ◽  
T Panalaks
Keyword(s):  
Vitamin D ◽  
Liquid Chromatography ◽  
Vitamin A ◽  
Coefficient Of Variation ◽  
Internal Standard ◽  
Antimony Trichloride ◽  
The Other ◽  
Gas Liquid Chromatography ◽  
Partition Chromatography

Abstract A method is described for determining vitamin D in multivitamin preparations; in the method, vitamins D2 and D3 are isomerized with antimony trichloride and separated by GLC. Vitamins D,2 and D3 are differentiated and measured separately and one vitamin may be used as an internal standard for the other. Vitamin A is largely removed by partition chromatography but can be tolerated in the final dilution in a ratio of 1:1 with vitamin D. When the method was used for the assay of multivitamin preparations, the coefficient of variation was 3.2%.

scholarly journals Alkylresorcinols in rye (Secale cereale L.) grains. I. Micromethod for determination of alkyl derivatives of resorcinol in rye grain

2015 ◽  
Vol 44 (4) ◽  
pp. 479-489 ◽  
Author(s):  
W. Mejbaum-Katzenellenbogen ◽  
F. Tłuścik ◽  
A. Kozubek ◽  
A. Sikorski
Keyword(s):  
Preparative Thin Layer Chromatography ◽  
Uv Spectrum ◽  
Selective Determination ◽  
Alkyl Derivatives ◽  
Secale Cereale L ◽  
Spectrum Characteristic ◽  
Acetone Extracts ◽  
Layer Chromatography ◽  
Derivatives Of

A pure preparation of alkylresorcinol from rye grains was obtained by preparative thin-layer chromatography, which gave a UV spectrum characteristic for 5-n-alkylresorcinols and orcinol. This preparation served as standard in the elaboration of a micro method (for alkylresorcinols determination in acetone extract from rye grain. It was found that this method is suitable for selective determination of 5-n-alkylrezorcinols in acetone extracts from rye grains.

Sign in / Sign up

Export Citation Format

Share Document