CHROMATOGRAPHIC SEPARATION OF URINARY CORTICOSTEROIDS

1960 ◽  
Vol XXXIV (III) ◽  
pp. 335-343 ◽  
Author(s):  
R. Emberland ◽  
K. F. Støa
Keyword(s):  
Propylene Glycol ◽  
Chromatographic Separation ◽  
Reducing Power ◽  
Phosphomolybdic Acid ◽  
Partition Chromatography ◽  
Chromatographic System ◽  
Specific Determination ◽  
The Right

ABSTRACT The usefulness of partition chromatography on cellulose columns has been tried in fractionation of urinary corticosteroids. As the chromatographic system toluene/propylene glycol has been used. During the first part of the experiments the determination of the corticosteroid content in the chromatographic fractions was carried out by measuring their reducing power against phosphomolybdic acid. Provided the right conditions were used, a satisfactory separation was obtained of the following steroids in mixture: 11-deoxycorticosterone, 11-dehydrocorticosterone, 11-deoxy-17-hydroxycorticosterone, corticosterone, cortisone, dihydrocortisone, tetrahydrocortisone, cortisol and tetrahydrocortisol. Aldosterone appeared in the same fractions as cortisone. By means of the borohydride-bismuthate reaction and a correction by the Allen formula in the subsequent spectrophotometry, an approximatively specific determination of a series of 17-hydroxycorticosteroids in urine extracts could be obtained.

COMPARISON OF VARIOUS METHODS FOR THE CHEMICAL ASSAY OF CORTICOIDS IN URINE

1955 ◽  
Vol 18 (4) ◽  
pp. 374-378
Author(s):  
Mogens Sprechler
Keyword(s):  
Calibration Curve ◽  
Periodic Acid ◽  
Reducing Power ◽  
Standard Technique ◽  
Phosphomolybdic Acid ◽  
Florisil Column ◽  
Chemical Assay ◽  
Chromatographic Procedure ◽  
Acid Reagent

SUMMARY Since 1949 about 10,000 urinary corticoid analyses have been performed routinely in our laboratory. The method used for this purpose was described in 1950 (Sprechler). We determine the corticoids which can be extracted from the urine with chloroform immediately after acidification to pH 1. The extract is washed with sodium hydroxide and water, a Girard separation is performed, and finally the reducing power of the ketonic fraction is measured by means of the phosphomolybdic acid reagent reaction. During the last few years two other chemical reactions have been used for comparison: The formaldehyde and the Porter-Silber method. After a thorough examination of the above methods a standard technique was followed. In the formaldehyde method a microdiffusion in a Conway unit was used instead of distillation of the formaldehyde following the oxidation with periodic acid. The calibration curve was corrected for loss of material by taking the standard doses of DOC through all the procedures of the method. A micromodification of the Porter-Silber method was chosen. Furthermore attempts were made to determine how specific the chromatographic procedure is in the determination of steroids in urinary extracts. For this purpose the Florisil column was used, and the technique described by Nelson & Samuels was followed. Finally we have investigated the glucuronide-bound corticoids in urine in a smaller series of objects.

Determination of Procaine and Related Local Anesthetics. I. Partition Chromatographic Separation and Assay of Mixtures of Procaine with Tetracaine and with Propoxycaine

1975 ◽  
Vol 58 (1) ◽  
pp. 88-92
Author(s):  
Thomas D Doyle ◽  
Joseph B Proctor
Keyword(s):  
Local Anesthetics ◽  
Chromatographic Separation ◽  
Ion Pair ◽  
Sodium Bromide ◽  
Chromatographic System ◽  
Extraction Constants ◽  
Bromide Ion ◽  
Selection Of

Abstract Determination of ionization and extraction constants for procaine, tetracaine, and propoxycaine led to selection of a simple partition chromatographic system for separation and assay of mixtures of these anesthetics. A 65% solution of chloroform in isooctane elutes tetracaine or propoxycaine from a pH 4:sodium bromide column; procaine is retained and subsequently eluted by chloroform as the bromide ion-pair. The anesthetics are then determined spectrophotometrically. Results of assay of standard and commercial formulations are presented.

ESTIMATION OF REDUCING SUGARS IN STARCH HYDROLYZATES BY PAPER CHROMATOGRAPHY

1950 ◽  
Vol 28b (9) ◽  
pp. 527-534 ◽  
Author(s):  
Ping Shu
Keyword(s):  
Quantitative Determination ◽  
Paper Chromatography ◽  
Chromatographic Separation ◽  
Reducing Sugars ◽  
Reducing Power ◽  
Probable Error

A method for quantitative determination of glucose, maltose, and reducing dextrins in starch hydrolyzates is described. The components are separated by paper chromatography and determined colorimetrically by measurement of their reducing power with alkaline copper and arseno-molybdate reagents. The probable error of the determinations with the use of this method is about 2%. A compact apparatus was designed, suitable for handling a large number of samples in the chromatographic separation. It is particularly useful for compounds with low Rf values.

Constitutional Court of Romania: The Constitutionality of the Citizens’ Initiative for the Revision of Article 48 (1) of the Constitution (‘Family’)

ICL Journal ◽  
2017 ◽  
Vol 11 (2) ◽  
Author(s):  
Marieta Safta
Keyword(s):  
Family Life ◽  
Family Relations ◽  
Original Form ◽  
Constitutional Court ◽  
Marriage And Family ◽  
Biological Sex ◽  
Specific Determination ◽  
The Right

AbstractThe Constitutional Court found that Article 48 of the Constitution of Romania enshrines and guarantees the right to marriage and family relations resulting from marriage, apart from the right to family life/respect for and protection of family life, a concept with a much broader legal content, which is also embodied and protected by Article 26 of the Constitution. Insofar the analysis is limited solely to the scope of the right to marriage, the proposed amendment of Article 48 of the Constitution, ie replacement of the words ‘of the spouses’ with the words ‘between a man and a woman’, constitutes a mere indication as regards the exercise of the fundamental right to marriage, namely the specific determination of the fact that marriage is concluded between partners of different biological sex. The amendment proposed is not likely cause the disappearance, removal, deletion or cancellation of the concept of marriage. Furthermore, the safeguards of the right to marriage, as enshrined in the constitutional text of reference in its original form, remain unchanged. Therefore, the initiative for revision of the Constitution is constitutional in respect of the provisions of Article 152 of the Constitution, as it does not remove the right to marriage or the safeguards thereof and it does not bring into question any other limit on matters of revision.

Collaborative Study of a Method for the Determination of Antipyrine and Benzocaine in Glycerol and Propylene Glycol Bases

1968 ◽  
Vol 51 (3) ◽  
pp. 624-626
Author(s):  
Richard T Krause
Keyword(s):  
Hydrochloric Acid ◽  
Propylene Glycol ◽  
Ferric Chloride ◽  
Infrared Spectra ◽  
Collaborative Study ◽  
Potassium Bromide ◽  
Reference Standards ◽  
Partition Chromatography ◽  
Average Recovery

Abstract A method for antipyrine and benzocaine, This Journal 50, 685-688 (1967), was studied by ten collaborators on five simulated commercial preparations at levels of 49—54 mg antipyrine/ml and 10—51 mg benzocaine/ml. The antipyrine and benzocaine are separated by column partition chromatography: antipyrine is retained on a ferric chloride column, and benzocaine is retained on a hydrochloric acid column. Maximum absorbances are determined on chloroform eluates at 272 and 283 mμ for antipyrine and benzocaine, respectively. Infrared spectra of the residues are determined in potassium bromide for identification of the drugs. The average recovery for antipyrine was 99.3 ± 1.80%, and for benzocaine, 99.0 ± 1 . 6 0 % . Infrared spectra submitted by collaborators corresponded to the reference standards and showed no interfering peaks. The method, with a slight change in the preparation of the standard solutions, is recommended for adoption as official, first action.

Quantitative Determination of Antioxidants, after a Chromatographic Separation on Completely Acetylated Filter Paper. II. Determination of Some p-Phenylenediamine Derivatives

1957 ◽  
Vol 30 (4) ◽  
pp. 1172-1174
Author(s):  
J. W. H. Zijp
Keyword(s):  
Quantitative Determination ◽  
Filter Paper ◽  
Chromatographic Separation ◽  
Oxidation Products ◽  
Partition Chromatography ◽  
Rubber Compound

Abstract In this paper methods are given for the quantitative determination of three antioxidants, viz., N,N′-diphenyl-p-phenylenediamine, N,N′-di-2-naphthyl-p-phenylenediamine and N-phenyl-N′-cyclohexyl-p-phenylenediamine. According to these methods the antioxidants are extracted from the rubber compound, separated by partition chromatography on completely acetylated filter paper and oxidized to the corresponding p-quinonediimines, after which these oxidation products are determined colorimetrically.

Quantitative Determination of Antioxidants after Chromatographic Separation on Completely Acetylated Filter Paper. I. Determination of Phenyl-1-Naphthylamine and of Phenyl-2-Naphthylamine

1957 ◽  
Vol 30 (4) ◽  
pp. 1168-1171
Author(s):  
J. W. H. Zijp
Keyword(s):  
Quantitative Determination ◽  
Filter Paper ◽  
Chromatographic Separation ◽  
Sulfanilic Acid ◽  
Partition Chromatography ◽  
Rubber Compound ◽  
Detailed Procedure ◽  
Whatman Paper ◽  
General Method

Abstract In this paper a general method for the quantitative determination of antioxidants is described. After isolation from the rubber compound the antioxidants are separated by partition chromatography, using completely acetylated Whatman paper No. 1. A detailed procedure is given for the quantitative determination of phenyl-1-naphthylamine and of phenyl-2-naphthylamine. These antioxidants are coupled with diazotized sulfanilic acid and determined colorimetrically.

THE FACTORS OF CAREER SELF-DETERMINATION OF STUDENTS OF HIGHER EDUCATION INSTITUTIONS

2019 ◽  
Vol 7 (1) ◽  
pp. 9-20
Author(s):  
Inna Yeung
Keyword(s):  
Higher Education ◽  
Higher Education Institutions ◽  
Well Being ◽  
Young Person ◽  
Self Determination ◽  
Full Time ◽  
Actual Problem ◽  
The Third ◽  
The Right

Choice of profession is a social phenomenon that every person has to face in life. Numerous studies convince us that not only the well-being of a person depends on the chosen work, but also his attitude to himself and life in general, therefore, the right and timely professional choice is very important. Research about factors of career self-determination of students of higher education institutions in Ukraine shows that self-determination is an important factor in the socialization of young person, and the factors that determine students' career choices become an actual problem of nowadays. The present study involved full-time and part-time students of Institute of Philology and Mass Communications of Open International University of Human Development "Ukraine" in order to examine the factors of career self-determination of students of higher education institutions (N=189). Diagnostic factors of career self-determination of students studying in the third and fourth year were carried out using the author's questionnaire. Processing of obtained data was carried out using the Excel 2010 program; factorial and comparative analysis were applied. Results of the study showed that initial stage of career self-determination falls down on the third and fourth studying year at the university, when an image of future career and career orientations begin to form. At the same time, the content of career self-determination in this period is contradictory and uncertain, therefore, the implementation of pedagogical support of this process among students is effective.

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%.

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