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 ◽  
...  

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.

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.


1996 ◽  
Vol 51 (5) ◽  
pp. 681-685 ◽  
Author(s):  
Max Herberhold ◽  
Guo-Xin Jin ◽  
Arnold L. Rheingold

The reactions of hydrido-tri(3,5-dimethyl-1-pyrazolyl)borate nitrosylmolybdenum diiodide, Tp*Mo(NO)I2 (2), with the oligochalcogenides (NH4)2S10 and (NEt4)2Se6 in THF solution lead to mononuclear cyclo-pentachalcogenido complexes, Tp*Mo(NO)(E5) (E = S (3a), Se (3b)). In the presence of either H2S or H2Se (generated by slow “in situ” hydrolysis of AI2E3 in moist THF solution) 2 is converted into binuclear chalcogenido-bridged products, Tp*2Mo2(NO)2(μ-E)2(E = S (4a), Se (4b)) which are more conveniently obtained from 3a,b by dechalcogenation with tri(″butyl)phosphane (1:4,5). The new chalcogen complexes 3a,b and 4a,b were characterized by IR, NMR and mass spectroscopy and compared with the related chalcogen compounds derived from pentamethylcyclopentadienyl nitrosylmolybdenum diiodide, Cp*Mo(NO)l2. The molecular structure of Tp*Mo(NO)(Se5) (3b) has been determined; the complex contains a sixmembered MoSe5; metallacycle in the chair conformation and a linearly coordinated nitrosyl ligand (angle Mo-N-O 178.9(17)°).


Author(s):  
Ahmed Iqbal ◽  
Peter Novodvorsky ◽  
Alexandra Lubina-Solomon ◽  
Fiona M Kew ◽  
Jonathan Webster

Summary Secondary amenorrhoea and galactorrhoea represent a common endocrine presentation. We report a case of an oestrogen-producing juvenile granulosa cell tumour (JGCT) of the ovary in a 16-year-old post-pubertal woman with hyperprolactinaemia amenorrhoea and galactorrhoea which resolved following surgical resection of the tumour. This patient presented with a 9-month history of secondary amenorrhoea and a 2-month history of galactorrhoea. Elevated serum prolactin at 7081 mIU/l and suppressed gonadotropins (LH <0.1 U/l; FSH <0.1 U/l) were detected. Serum oestradiol was significantly elevated at 7442 pmol/l with undetectable β-human chorionic gonadotropin. MRI showed a bulky pituitary with no visible adenoma. MRI of the abdomen showed a 4.8 cm mass arising from the right ovary with no evidence of metastatic disease. Serum inhibin B was elevated at 2735 ng/l. A right salpingo-oophorectomy was performed, and histology confirmed the diagnosis of a JGCT, stage International Federation of Gynaecology and Obstetrics 1A. Immunohistochemical staining for prolactin was negative. Post-operatively, oestrogen and prolactin levels were normalised, and she subsequently had a successful pregnancy. In summary, we present a case of an oestrogen-secreting JGCT with hyperprolactinaemia manifesting clinically with galactorrhoea and secondary amenorrhoea. We postulate that observed hyperprolactinaemia was caused by oestrogenic stimulation of pituitary lactotroph cells, a biochemical state analogous to pregnancy. To the best of our knowledge, this is the first report of hyperprolactinaemia as a result of excessive oestrogen production in the context of a JGCT. Learning points Hyperprolactinaemia with bilateral galactorrhoea and secondary amenorrhoea has a wide differential diagnosis and is not always caused by a prolactin secreting pituitary adenoma. Significantly elevated serum oestradiol levels in the range seen in this case, in the absence of pregnancy, are indicative of an oestrogen-secreting tumour. JGCTs are rare hormonally active ovarian neoplasms mostly secreting steroid hormones. Serum inhibin can be used as a granulosa cell-specific tumour marker. JGCTs have an excellent prognosis in the early stages of the disease.


1967 ◽  
Vol 55 (3) ◽  
pp. 401-414 ◽  
Author(s):  
S. Dell'Acqua ◽  
S. Mancuso ◽  
G. Eriksson ◽  
J. L. Ruse ◽  
S. Solomon ◽  
...  

ABSTRACT 16α-Hydroxy-dehydroepiandrosterone-7α-3H (16αHO-DHA), 16α-hydroxy-androstenedione-4-14C (16αHO-A) and 16α-hydroxy-testosterone-4-14C (16αHO-T) were synthesized. Human placentas were perfused in situ at midpregnancy with these steroids and the radioactive material recovered from the placentas and perfusates was analysed. In order to compare the aromatisation of 16α-hydroxylated and 16-desoxy precursors, in a second series of perfusions 16αHO-DHA was combined with differently labelled dehydroepiandrosterone (DHA) and 16αHO-T with testosterone (T). Following the perfusion of 16αHO-DHA, both 16αHO-A and oestriol (OE3) were isolated from the placentas and perfusates. No labelled androst-5-ene-3β,16α,17β-triol (Δ5-TRIOL) or 16αHO-T was detected in these sources. When 16αHO-A or 16αHO-T was perfused, OE3 was isolated from the placenta and perfusates. However, there was no interconversion between 16αHO-A and 16αHO-T. No oestrogenic ring D ketols were found in the placentas and perfusates in any of the experiments. The extent of aromatisation (judged from the amount of oestrogen isolated from the placenta and perfusate) was approximately the same following the perfusion of 16αHO-DHA, 16αHO-A, DHA and T, but was much lower when 16αHO-T was perfused. The low degree of aromatisation of 16αHO-T was associated with the presence of large amounts of unchanged 16αHO-T in the placentas as well as in the perfusates. The transfer of 16αHO-T to the maternal compartment was also much lower than that of the other precursors studied. It is concluded that the placental transfer and aromatisation of 16αHO-T is much lower than those of other oestrogen precursors. This condition might lead to the accumulation of this compound in the placenta. The placental metabolism of Δ5-TRIOL and 16αHO-DHA follow separate pathways with no interconversion until the stage of aromatisation, or possibly 19-hydroxylation.


RSC Advances ◽  
2016 ◽  
Vol 6 (25) ◽  
pp. 21261-21270 ◽  
Author(s):  
D. Nanda Kumar ◽  
Jaydeep Roy ◽  
S. A. Alex ◽  
N. Chandrasekaran ◽  
A. Mukherjee

A novel fluorimetric detection method for Hg2+ and Pb2+ based on in situ formation of AgNPs, where thiocholine (TCh), a product obtained by the hydrolysis of acetylcholine (ACh) by acetylcholinesterase (AChE), can act as a stabilizing agent.


Author(s):  
S. P. Sapers ◽  
R. Clark ◽  
P. Somerville

OCLI is a leading manufacturer of thin films for optical and thermal control applications. The determination of thin film and substrate topography can be a powerful way to obtain information for deposition process design and control, and about the final thin film device properties. At OCLI we use a scanning probe microscope (SPM) in the analytical lab to obtain qualitative and quantitative data about thin film and substrate surfaces for applications in production and research and development. This manufacturing environment requires a rapid response, and a large degree of flexibility, which poses special challenges for this emerging technology. The types of information the SPM provides can be broken into three categories:(1)Imaging of surface topography for visualization purposes, especially for samples that are not SEM compatible due to size or material constraints;(2)Examination of sample surface features to make physical measurements such as surface roughness, lateral feature spacing, grain size, and surface area;(3)Determination of physical properties such as surface compliance, i.e. “hardness”, surface frictional forces, surface electrical properties.


1978 ◽  
Vol 39 (C6) ◽  
pp. C6-1232-C6-1233 ◽  
Author(s):  
N. F. Pedersen ◽  
J. Mygind ◽  
O. H. Soerensen ◽  
B. Dueholm

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%.


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