scholarly journals A method for the determination of small quantities of mixed reducing sugars and its application to the estimation of the products of hydrolysis of starch by taka-diastase

1931 ◽  
Vol 25 (3) ◽  
pp. 863-879 ◽  
Author(s):  
Elsie May Widdowson
1964 ◽  
Vol 47 (4) ◽  
pp. 695-700
Author(s):  
Lester Hankin ◽  
Alphoxse F Wickroski

Abstract An enzymatic method is proposed to overcome the difficulties encountered with the AOAC yeast method for the determination of lactose in prepared meat products which also contain corn sirup solids in addition to nonfat dry milk. The AOAC method does not allow for complete hydrolysis of the corn sirup solids, and, when reducing sugars are calculated as lactose, inflated values are obtained since some of the unhydrolyzed reducing material from the corn sirup solids is measured. In the enzyme method, a combination of crude maltase and glucose oxidase are used to remove all reducing sugars except lactose. Preliminary yeast treatment is included either routinely or to remove sucrose, if present. Comparative values obtained on prepared frankfort samples showed that the enzyme method was superior to the AOAC method.


2018 ◽  
Vol 84 (10) ◽  
pp. 5-11 ◽  
Author(s):  
E. I. Kashcheyeva ◽  
V. V. Budaeva

An ever-growing scientific interest in the development of effective methods for transformation of various cellulosic resources into fermentable sugars necessitates development of a universal procedure for determination of the reactivity of cellulosic substrates towards enzymatic hydrolysis. The practical significance consists in maximum accessibility of the procedure for the labs of pilot-production enterprises engaged in testing and scaling up the biotech processes. The developed procedure fully complies with modern requirements and relies on measuring the concentration of reducing sugars (spectrophotometry and HPLC) in the enzymatic hydrolyzates obtained from pre-prepared substrates, the biocatalysis being run by a cocktail composed of available CelluLuxe-A and BrewZyme-BGX. On top of that, the procedure implies gravimetric analysis of the solid residues after hydrolysis of substrates. Cellulosic biomasses can usually be fermented for control without any pretreatment, however, commercial celluloses can be used as well. The use of the developed procedure is shown to provide prompt and high-quality assessment of the reactivity of a series of chosen substrates to enzymatic hydrolysis. In contrast to the methods of enzymatic hydrolysis discussed in literature for evaluation of the enzyme efficiency, the developed procedure allows arranging of chosen cellulosic raw materials in a descending order of their reactivity to hydrolysis using the same multi-enzyme cocktail and, moreover can demonstrate dependence of the reactivity of substrates on the pretreatment method. The results can be presented as a dependence of the concentration (yield) of reducing sugars on the duration of enzymatic hydrolysis of the substrate, and also in the form of the calculated hydrolysis rates, final yields of reducing sugars including pentoses, content of glucose component of reducing substances and decrease in mass. The procedure was repeatedly tested on a wide range of cellulosic substrates and provided reliable results regarding evaluation of their reactivity and forecasting of the scale-up results of enzymatic hydrolysis, including that in aqueous medium when preparing nutrient broths for microbiological synthesis.


1962 ◽  
Vol 41 (2) ◽  
pp. 234-246 ◽  
Author(s):  
H. J. van der Molen

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%.


1963 ◽  
Vol 44 (1) ◽  
pp. 47-66 ◽  
Author(s):  
W. Nocke ◽  
H. Breuer

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.


1961 ◽  
Vol 38 (4) ◽  
pp. 545-562 ◽  
Author(s):  
L. Kecskés ◽  
F. Mutschler ◽  
I. Glós ◽  
E. Thán ◽  
I. Farkas ◽  
...  

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.


2019 ◽  
Vol 85 (7) ◽  
pp. 16-21
Author(s):  
Liliya R. Mubarakova ◽  
German K. Budnikov

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.


1980 ◽  
Vol 45 (4) ◽  
pp. 1099-1108 ◽  
Author(s):  
Mikuláš Chavko ◽  
Michal Bartík ◽  
Evžen Kasafírek

A polarographic study of the hydrolysis of [8-lysine]vasopressin and some hormonogens of the vasopressin series with the blood serum of women in the last week of pregnancy was studied. The dependence of hydrolysis on pH (pH optimum: 7.4-7.50, substrate concentration (Km 1.2 . 10-5M), pH stability and thermal stability were determined. The rate of hydrolysis of individual vasopressin analogues decreases in the order: [8-lysine]vasopressin > Nα-glycyl-prolyl[8-lysine]-vasopressin > Nα-leucyl-[8-lysine]vasopressin > Nα-alanyl-[8-lysine]vasopressin > Nα-phenyl alanyl-[8-lysine]vasopressin > Nα-diglycyl-[8-lysine]vasopressin > Nα-prolyl-[8-lysine]vasopressin > Nα-triglycyl-[8-lysine]vasopressin > Nα-sarcosyl-glycyl-[8-lysine]vasopressin. The degree of hydrolysis gradually increases to a multiple with the length of the pregnancy in consequence of the presence of oxytocine. However, vasopressin is also hydrolysed to a small extent with the enzymes from the blood sera of non-pregnant women. Under similar analytical conditions oxytocin was not hydrolysed with the sera of non-pregnant women and therefore oxytocin is a more suitable substrate than vasopressin for polarographic determination of serum oxytocinase.


1980 ◽  
Vol 45 (7) ◽  
pp. 1959-1963 ◽  
Author(s):  
Dušan Joniak ◽  
Božena Košíková ◽  
Ludmila Kosáková

Methyl 4-O-(3-methoxy-4-hydroxybenzyl) and methyl 4-O-(3,5-dimethoxy-4-hydroxybenzyl)-α-D-glucopyranoside and their 6-O-isomers were prepared as model substances for the ether lignin-saccharide bond by reductive cleavage of corresponding 4,6-O-benzylidene derivatives. Kinetic study of acid-catalyzed hydrolysis of the compounds prepared was carried out by spectrophotometric determination of the benzyl alcoholic groups set free, after their reaction with quinonemonochloroimide, and it showed the low stability of the p-hydroxybenzyl ether bond.


1983 ◽  
Vol 29 (8) ◽  
pp. 1513-1517 ◽  
Author(s):  
M W McGowan ◽  
J D Artiss ◽  
B Zak

Abstract A procedure for the enzymatic determination of lecithin and sphingomyelin in aqueous solution is described. The phospholipids are first dissolved in chloroform:methanol (2:1 by vol), the solvent is evaporated, and the residue is redissolved in an aqueous zwitterionic detergent solution. The enzymatic reaction sequences of both assays involve hydrolysis of the phospholipids to produce choline, which is then oxidized to betaine, thus generating hydrogen peroxide. The hydrogen peroxide is subsequently utilized in the enzymatic coupling of 4-aminoantipyrine and sodium 2-hydroxy-3,5-dichlorobenzenesulfonate, an intensely red color being formed. The presence of a non-reacting phospholipid enhances the hydrolysis of the reacting phospholipid. Thus we added lecithin to the sphingomyelin standards and sphingomyelin to the lecithin standards. This precise procedure may be applicable to determination of lecithin and sphingomyelin in amniotic fluid.


2021 ◽  
Author(s):  
Yuxiao Dong ◽  
Dongshen Tong ◽  
Laibin Ren ◽  
Xingtao Chen ◽  
Hao Zhang ◽  
...  

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