scholarly journals A Sulfuryl Group Transfer Strategy to Selectively Prepare Sulfated Steroids and Isotopically Labelled Derivatives

2021 ◽  
Vol 8 ◽  
Author(s):  
Jaber A. Alshehri ◽  
Daniel M. Gill ◽  
Alan M. Jones

The treatment of common steroids: estrone, estradiol, cortisol, and pregnenolone with tributylsulfoammonium betaine (TBSAB) provides a convenient chemoselective conversion of the steroids alcohol/phenol moiety to the corresponding steroidal organosulfate. An important feature of the disclosed methodology is the millimolar scale of the reaction, and the isolation of the corresponding steroid sulfates as their biologically relevant sodium salts without the need for ion-exchange chromatography. The scope of the method was further explored in the estradiol and pregnanediol steroid systems with the bis-sulfated derivatives. Ultimately, a method to install an isotopic label, deuterium (2H) combined with estrone sulfation is a valuable tool for its mass-spectrometric quantification in biological studies.

1975 ◽  
Vol 53 (1) ◽  
pp. 65-69 ◽  
Author(s):  
S. R. Philips ◽  
B. A. Davis ◽  
D. A. Durden ◽  
Alan A. Boulton

A procedure for the quantitative evaluation of m-tyramine in mammalian tissues is described. It involves isolation of the amine by ion-exchange chromatography, followed by conversion to the dansyl derivative, chromatographic separation, and quantitation by the mass spectrometric integrated ion current technique using an isotopically labelled internal standard. The concentrations of m-tyramine in some tissues of male Wistar rats were (mean ± S.D., nanograms per gram): brain 0.32 ± 0.03, heart 0.44 ± 0.13. kidney 12.6 ± 3.4, liver 0.27 ± 0.04, lung 0.33 ± 0.11, spleen 0.25 ± 0.07, and blood 0.15 ± 0.04.


2013 ◽  
Vol 10 (4) ◽  
pp. 1304-1311 ◽  
Author(s):  
Miguel Rodrigo ◽  
Natalia Cernei ◽  
Marketa Kominkova ◽  
Ondrej Zitka ◽  
Miroslava Beklova ◽  
...  

1974 ◽  
Vol 52 (5) ◽  
pp. 366-373 ◽  
Author(s):  
S. R. Philips ◽  
D. A. Durden ◽  
A. A. Boulton

A procedure for the quantitative evaluation of p-tyramine in mammalian tissues is described. It involves isolation of the amine by ion-exchange chromatography, followed by conversion to the dansyl derivative, chromatographic separation, and quantitation by the mass spectrometric integrated ion current technique using an isotopically labelled internal standard.The concentrations of p-tyramine in some tissues of male Wistar rats were (mean ± standard deviation (ng/g)): brain 2.0 ± 0.9, heart 3.4 ± 1.4, kidney 32.7 ± 13.1, liver 1.5 ± 0.5, lung 3.0 ± 1.2, and spleen 3.4 ± 1.2. In the brain, hypothalamus contained 11.3 ± 3.7, cerebellum 2.3 ± 1.7, stem 2.2 ± 1.0, caudate nucleus 19.2 ± 2.5, and the 'rest' 1.6 ± 0.4 ng/g, respectively.


1964 ◽  
Vol 42 (3) ◽  
pp. 599-604 ◽  
Author(s):  
J. G. Moffatt

The reaction between ribo- and deoxyribo-nucleoside-5′ phosphoromorpholidates and tributylammonium pyrophosphate in molecular sieve dried dimethyl sulphoxide has been found to give the nucleoside-5′ triphosphates in 81–84% yields. A convenient work-up of the triphosphates following ion exchange chromatography permits isolation of the triphosphates in overall yields of 73–80% as the pure sodium salts. A number of examples of the reaction are given.


1973 ◽  
Vol 30 (02) ◽  
pp. 414-424 ◽  
Author(s):  
Ulla Hedner

SummaryA procedure is described for partial purification of an inhibitor of the activation of plasminogen by urokinase and streptokinase. The method involves specific adsorption of contammants, ion-exchange chromatography on DEAE-Sephadex, gel filtration on Sephadex G-200 and preparative electrophoresis. The inhibitor fraction contained no antiplasmin, no plasminogen, no α1-antitrypsin, no antithrombin-III and was shown not to be α2 M or inter-α-inhibitor. It contained traces of prothrombin and cerulo-plasmin. An antiserum against the inhibitor fraction capable of neutralising the inhibitor in serum was raised in rabbits.


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