LIBERATION OF HEXOSAMINE, HEXURONIC ACID, AND HYDROXYPROLINE FROM TISSUES BY RESIN HYDROLYSIS

1958 ◽  
Vol 36 (4) ◽  
pp. 413-424 ◽  
Author(s):  
P. A. Anastassiadis ◽  
R. H. Common
Keyword(s):  
Hydrochloric Acid ◽  
Tissue Samples ◽  
Hexuronic Acid ◽  
Polystyrene Resin ◽  
Hydrolysis Of ◽  
Separation Of Sugars

Excess sulphonated polystyrene resin (Dowex-50, 200–400 mesh) suspended in 0.05 N hydrochloric acid has been found suitable as a catalyst for the hydrolysis of tissue samples preparatory to the determination of hexosamine, hexuronic acid, and hydroxyproline. This technique protected hexuronic acid from destruction during hydrolysis sufficiently well to permit of its determination. The resin used in hydrolysis has been used also for separation of sugars and hexuronic acid from hexosamine and hydroxyproline by differential elution.

LIBERATION OF HEXOSAMINE, HEXURONIC ACID, AND HYDROXYPROLINE FROM TISSUES BY RESIN HYDROLYSIS

1958 ◽  
Vol 36 (1) ◽  
pp. 413-424 ◽  
Author(s):  
P. A. Anastassiadis ◽  
R. H. Common
Keyword(s):  
Hydrochloric Acid ◽  
Tissue Samples ◽  
Hexuronic Acid ◽  
Polystyrene Resin ◽  
Hydrolysis Of ◽  
Separation Of Sugars

Excess sulphonated polystyrene resin (Dowex-50, 200–400 mesh) suspended in 0.05 N hydrochloric acid has been found suitable as a catalyst for the hydrolysis of tissue samples preparatory to the determination of hexosamine, hexuronic acid, and hydroxyproline. This technique protected hexuronic acid from destruction during hydrolysis sufficiently well to permit of its determination. The resin used in hydrolysis has been used also for separation of sugars and hexuronic acid from hexosamine and hydroxyproline by differential elution.

A STUDY ON THE LIBERATION OF SUGARS, HEXURONIC ACID, AND HEXOSAMINE FROM BIOLOGICAL MATERIAL

1961 ◽  
Vol 39 (4) ◽  
pp. 671-681 ◽  
Author(s):  
W. Haab ◽  
P. A. Anastassiadis
Keyword(s):  
Hyaluronic Acid ◽  
Hydrochloric Acid ◽  
Biological Material ◽  
Dilute Hydrochloric Acid ◽  
Glucuronic Acid ◽  
Chondroitin Sulphate ◽  
Hydrolytic Cleavage ◽  
Hexuronic Acid ◽  
Polystyrene Resin ◽  
Hydrolysis Of

Sulphonated polystyrene resin suspended in dilute hydrochloric acid and 4 N hydrochloric acid were compared with respect to (a) efficiency as catalysts of hydrolytic cleavage of mucopolysaccharides and (b) rates of destruction of sugars, glucuronic acid, and glucosamine. Mannose, galactose, and glucose were not subject to serious destruction when heated with the resin suspension over a period that was sufficient to effect hydrolysis of mucopolysaccharides and glycoproteins. All these sugars were subject to serious destruction when heated with 4 N hydrochloric acid for a period sufficient to effect hydrolysis of mucopolysaccharides and glycoproteins. Under similar conditions, pentoses were destroyed more rapidly than hexoses but ribose withstood heating with the resin suspension for several hours. Heparin was found to be more resistant to hydrolysis than chondroitin sulphate or hyaluronic acid.

scholarly journals HIDROLISIS RUMPUT LAUT (Glacilaria sp.) MENGGUNAKAN KATALIS ENZIM DAN ASAM UNTUK PEMBUATAN BIOETANOL

Jurnal Kimia ◽  
2016 ◽  
Author(s):  
Yohanes Armawan Sandi ◽  
Wiwik Susanah Rita ◽  
Yenni Ciawi
Keyword(s):  
Gas Chromatography ◽  
Hydrochloric Acid ◽  
Sulphuric Acid ◽  
Ethanol Concentration ◽  
Reducing Sugar ◽  
Optimum Concentration ◽  
Raw Material ◽  
Optimum Length ◽  
Hydrolysis Of

The aim of this research is to determine the effect of enzyme and acids concentration on the yield of glucose produced in the hydrolysis of Glacilaria sp. in the production of bioethanol. The concentrations of cellulase used were 200 units/mL, 400 units/mL, 600 units/mL, 800 units/mL and the concentration of sulphuric acid (H2SO4) and hydrochloric acid (HCl) used were 1%, 3%, 5%, 7% (w/v). The concentration of reduction sugar was determined using Anthrone and analyzed using UV-Vis spectrophotometry and the determination of ethanol concentration was carried out by using gas chromatography. The results showed that the contents of reducing sugar produced by sulphuric acid (H2SO4) hydrolysis were 26,19%; 36,69%; 41,40%; 45,0% (v/v), by hydrochloric acid (HCl) were 12,12%; 14,03%; 15,17%; 16,50% (v/v), and by cellulase enzyme were 46,15%; 46,73%; 47,68%; 48,25% (v/v). Optimum concentration of reducing sugar produced by hydrolysis using 800 units/mL cellulase was 48,25% (v/v). The optimum length of fermentation to produce bioethanol using Glacilaria sp. as raw material was 5 days. In the fermentation, inoculum with a concentrations of 5% and 10% (w/v) produced 0,85% and 1,51% (v/v) ethanol.

High Performance Liquid Chromatographic Quantitation of Aflatoxin Metabolites in Animal Tissues

1982 ◽  
Vol 65 (4) ◽  
pp. 869-875 ◽  
Author(s):  
Jesse F Gregory
Keyword(s):  
High Performance ◽  
High Performance Liquid Chromatographic ◽  
Water Soluble ◽  
Animal Tissues ◽  
Tissue Samples ◽  
Sample Extract ◽  
Liquid Chromatographic ◽  
Hydrolysis Of ◽  
Fluorescent Derivatives

Abstract A previously reported reverse phase high performance liquid chromatographic (HPLC) procedure was modified to permit the determination of the parent aflatoxins and various free and conjugated metabolites in animal tissues. The modified procedure was based on HPLC analysis of duplicate portions of a sample extract which had been prepared with and without treatment with trifluoroacetic acid (TFA). TFA catalyzes the conversion of aflatoxins G1, B1, M1, and Q1 to the fluorescent derivatives G2a, B2a M2a, and Q2a. Aflatoxicol, which exhibited a sharp fluorescent peak in its native state, eluted as a tailing peak with weaker fluorescence following TFA treatment. Acid hydrolysis of the aqueous phase of tissue samples permitted the analysis of water-soluble conjugated forms of the various aflatoxins. Analysis of fluorescence spectra of manually collected HPLC fractions qualitatively supported the accuracy of the method. Representative data on the distribution of aflatoxins in turkey liver following ingestion of an experimentally contaminated ration are presented.

The determination of mimosine and 3,4-dihydroxypyridine in biological material

1964 ◽  
Vol 15 (1) ◽  
pp. 168 ◽  
Author(s):  
MP Hegarty ◽  
RD Court ◽  
PM Thorne
Keyword(s):  
Hydrochloric Acid ◽  
Exchange Resin ◽  
Cation Exchange Resin ◽  
Ammonium Hydroxide ◽  
Mesityl Oxide ◽  
Specific Method ◽  
Fresh Material ◽  
First Time ◽  
Hydrolysis Of

A simple, specific method is described for the determination of mimosine and 3,4-dihydroxypyridine (DHP) in extracts of leaves and seeds of Leucaena glauca Benth. and in urine. Plant material is extracted with cold 0.1 N hydrochloric acid, and interfering substances are removed by chromatography on a cation-exchange resin. Organic cations are displaced from the resin with 2N ammonium hydroxide and the concentrated eluate chromatographed in one direction with the use of mesityl oxide : formic acid : water (41 : 7 : 6 by volume). The spots of mimosine and DHP, revealed with a ferric chloride spray, are cut out and the colour fully developed and measured. Urines are analysed in the same way except for a preliminary hydrolysis of the conjugated DHP. The method is satisfactory for estimating amounts of mimosine and DHP in the range 10–160 µg applied to the paper. Recoveries of these substances added to various extracts and to urine have varied between 98–102%. Appreciable destruction of mimosine, with the formation of some DHP, occurred when fresh L. glauca leaves were dried even under mild conditions. In fresh material no loss of mimosine occurred when it was placed immediately in 0.1 N hydrochloric acid. The ready hydrolysis of mimosine to DHP by boiling 0. I N hydrochloric acid has been demonstrated for the first time.

DETERMINATION OF MICRO-AMOUNTS OF 5β-PREGNAN-3α-OL-20-ONE IN URINE USING INFRARED-SPECTROMETRY

1962 ◽  
Vol 41 (2) ◽  
pp. 234-246 ◽  
Author(s):  
H. J. van der Molen
Keyword(s):  
Infrared Spectrum ◽  
Quantitative Determination ◽  
Acid Hydrolysis ◽  
Chromatographic Separation ◽  
Pure Form ◽  
Infrared Spectrometry ◽  
Hydrolysis Of

ABSTRACT A procedure for the quantitative determination of 5β-pregnan-3α-ol-20-one in urine is described. After acid hydrolysis of the pregnanolone-conjugates in urine, the free steroids are extracted with toluene. Pregnanolone is isolated in a pure form as its acetate; after chromatographic separation of the free steroids on alumina, the fraction containing pregnanolone is acetylated and rechromatographed on alumina. Quantitative determination of the isolated pregnanolone-acetate is carried out with the aid of the infrared spectrum recorded by a micro KBr-wafermethod. The reliability of the method under various conditions is discussed under the headings, specificity, accuracy, precision and sensitivity. It is possible to determine 30–40 μg pregnanolone in a 24-hours urine portion with a precision of 25%.

EINE CHEMISCHE METHODE ZUR BESTIMMUNG VON 16-EPI-ÖSTRIOL IM URIN DES MENSCHEN

1963 ◽  
Vol 44 (1) ◽  
pp. 47-66 ◽  
Author(s):  
W. Nocke ◽  
H. Breuer
Keyword(s):  
Melting Point ◽  
Phosphoric Acid ◽  
Aqueous Alkali ◽  
Percentage Error ◽  
Organic Layer ◽  
Maximum Percentage ◽  
Chemical Determination ◽  
Routine Assay ◽  
Hydrolysis Of

ABSTRACT A method for the chemical determination of 16-epi-oestriol in the urine of nonpregnant women with a qualitative sensitivity of less than 0.5 μg/24 h is described. The separation of 16-epi-oestriol and oestriol is accomplished by converting 16-epi-oestriol into its acetonide, a reaction which is stereoselective for cis-glycols and therefore not undergone by oestriol as a trans-glycol. Following partition between chloroform and aqueous alkali, the acetonide of 16-epi-oestriol is completely separated with the organic layer whereas oestriol as a strong phenol remains in the alkaline phase. 16-epi-oestriol is chromatographed on alumina as the acetonide and determined as a Kober chromogen. This procedure can easily be incorporated into the method of Brown et al. (1957 b) thus making possible the simultaneous routine assay of oestradiol-17β, oestrone, oestriol and 16-epi-oestriol from one sample of urine. The specificity of the method was established by separation of 16-epi-oestriol from nonpregnancy urine as the acetonide, hydrolysis of the acetonide by phosphoric acid, isolation of the free compound by microsublimation and identification by micro melting point, colour reactions and chromatography. The accuracy of the method is given by a mean recovery of 64% for pure crystalline 16-epi-oestriol when added to hydrolysed urine in 5–10 μg amounts. The precision is given by s = 0.24 μg/24 h. For the duplicate determination of 16-epi-oestriol the qualitative sensitivity is 0.44 μg/24 h, the maximum percentage error being ± 100% The quantitative sensitivity (±25% error) is 1.7 μg/24 h.

INDIREKTE PAPIERCHROMATOGRAPHISCHE METHODE ZUR BESTIMMUNG DER HARNOESTROGENE

1961 ◽  
Vol 38 (4) ◽  
pp. 545-562 ◽  
Author(s):  
L. Kecskés ◽  
F. Mutschler ◽  
I. Glós ◽  
E. Thán ◽  
I. Farkas ◽  
...  
Keyword(s):  
Pregnant Women ◽  
Granulosa Cell ◽  
Iron Content ◽  
List Type ◽  
Granulosa Cell Tumour ◽  
Hydrolysis Of ◽  
Phenol Fraction ◽  
Qualitative Determination

ABSTRACT 1. An indirect paperchromatographic method is described for separating urinary oestrogens; this consists of the following steps: acidic hydrolysis, extraction with ether, dissociation of phenol-fractions with partition between the solvents. Previous purification of phenol fraction with the aid of paperchromatography. The elution of oestrogen containing fractions is followed by acetylation. Oestrogen acetate is isolated by re-chromatography. The chromatogram was developed after hydrolysis of the oestrogens 'in situ' on the paper. The quantity of oestrogens was determined indirectly, by means of an iron-reaction, after the elution of the iron content of the oestrogen spot, which was developed by the Jellinek-reaction. 2. The method described above is satisfactory for determining urinary oestrogen, 17β-oestradiol and oestriol, but could include 16-epioestriol and other oestrogenic metabolites. 3. The sensitivity of the method is 1.3–1.6 μg/24 hours. 4. The quantitative and qualitative determination of urinary oestrogens with the above mentioned method was performed in 50 pregnant and 9 non pregnant women, and also in 2 patients with granulosa cell tumour.

Determination of δ-hexadecansultone in sodium α-olefinesulphonates and liquid detergents using gas chromatography-mass spectrometry (GC/MS)

2019 ◽  
Vol 85 (7) ◽  
pp. 16-21
Author(s):  
Liliya R. Mubarakova ◽  
German K. Budnikov
Keyword(s):  
Multicomponent Mixture ◽  
Operating Mode ◽  
Complete Separation ◽  
Gas Chromatography Mass Spectrometry ◽  
Liquid Detergent ◽  
Cyclic Esters ◽  
Alcohol Water ◽  
Household Chemicals ◽  
Hydrolysis Of

Sultones are cyclic esters of hydroxysulfonic acids, which are formed in the process of sulfonation of α-olefins with sulfur trioxide gas. More stable sultones may be present in the final product — an anionic surfactant — sodium α-olefin sulfonate (AOC-Na). AOC-Na is widely used in the production of household chemicals and cosmetic products, including liquid dishwashing detergents. Sultones are strong skin sensitizers, their level in AOC-Na should be strictly controlled and not exceed 5 ppm. Operational and strict control of the sultone content upon AOC-Na production allows timely adjustment at the stage of hydrolysis, which leads to a more complete disclosure of the sultone cycle with the formation of the corresponding olefin sulfonates and hydroxyalkanesulfonates. We propose a method for determining δ-hexadecansultone in liquid dishwashing detergents and sodium α-olefinsulfonates obtained on the basis of α-olefins of C14 – C16 fractions using GC/MS, which provides shortening of sample preparation and keeps the sensitivity with a detection limit of 0.02 mg/kg. The effect of various weakly polar and non-polar organic solvents used for Sultone extraction from AOC-Na and liquid detergent on liquid extraction based on the dispersion of the extractant in an alcohol/water phase is studied. When selecting the solvent we have shown that the use of diethyl ether provided the best extraction of the analyte. Determination of the analyte extraction recovery was performed using the reaction of hydrolysis of the extracted mixture. We specified the operating mode of the device which provided complete separation of the components of the analyzed compounds including the samples of liquid detergent for dishes being a multicomponent mixture of complex composition.

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