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Selenium disulfide

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Selenium disulfide

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Younes Dahmani
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Selenium disulfide EUROPEAN PHARMACOPOEIA 11.

ASSAY
To 0.100 g add 25 mL of fuming nitric acid R and heat on a
water-bath for 1 h ; a small insoluble residue may remain.
Cool and dilute to 100.0 mL with water R. To 25.0 mL of this
D. N-[(1R)-1-methyl-2-phenylethyl]prop-2-yn-1-amine solution add 50 mL of water R and 5 g of urea R and heat to
(desmethylselegiline), boiling. Cool, add 7 mL of potassium iodide solution R and
3 mL of starch solution R. Titrate immediately with 0.1 M
sodium thiosulfate. Carry out a blank titration.
1 mL of 0.1 M sodium thiosulfate is equivalent to 1.974 mg of
Se.

E. N-methyl-N-[(1S)-1-methyl-2-phenylethyl]prop-2-yn-1- 01/2017:0788
amine,

SERINE
G. (2EZ)-3-chloro-N-methyl-N-[(1RS)-1-methyl-2-
phenylethyl]prop-2-en-1-amine. Serinum
01/2008:1147

C3H7NO3 Mr 105.1
[56-45-1]
SELENIUM DISULFIDE DEFINITION
(2S)-2-Amino-3-hydroxypropanoic acid.
Selenii disulfidum Product of fermentation or of protein hydrolysis.
Content : 98.5 per cent to 101.0 per cent (dried substance).
SeS2 Mr 143.1
[7488-56-4] CHARACTERS
Appearance : white or almost white, crystalline powder or
DEFINITION colourless crystals.
Content : 52.0 per cent to 55.5 per cent of Se. Solubility : freely soluble in water, practically insoluble in
CHARACTERS ethanol (96 per cent).
Appearance : bright orange or reddish-brown powder. IDENTIFICATION
Solubility : practically insoluble in water. First identification : A, B.
IDENTIFICATION Second identification : A, C, D.
A. Gently boil about 50 mg with 5 mL of nitric acid R for A. Specific optical rotation (see Tests).
30 min. Dilute to 50 mL with water R and filter. To 5 mL of B. Infrared absorption spectrophotometry (2.2.24).
the filtrate add 10 mL of water R and 5 g of urea R. Heat to Comparison : serine CRS.
boiling, cool and add 1.5 mL of potassium iodide solution R. C. Thin-layer chromatography (2.2.27).
A yellow or orange colour is produced which darkens
rapidly on standing. This solution is used in identification Test solution. Dissolve 10 mg of the substance to be
test B. examined in a 1 per cent V/V solution of hydrochloric
acid R and dilute to 50 mL with the same solution.
B. Allow the coloured solution obtained under identification A
to stand for 10 min and filter through kieselguhr for Reference solution. Dissolve 10 mg of serine CRS in a 1 per
chromatography R. 5 mL of the filtrate gives reaction (a) cent V/V solution of hydrochloric acid R and dilute to
of sulfates (2.3.1). 50 mL with the same solution.
Plate : TLC silica gel plate R.
TESTS Mobile phase : glacial acetic acid R, water R, butanol R
Soluble selenium compounds : maximum 5 ppm, calculated (20:20:60 V/V/V).
as Se. Application : 5 μL.
To 10 g add 100 mL of water R, mix well, allow to stand for Development : over 2/3 of the plate.
1 h with frequent shaking and filter. To 10 mL of the filtrate Drying : in air.
add 2 mL of a 115 g/L solution of anhydrous formic acid R,
dilute to 50 mL with water R and adjust to pH 2.0-3.0 with an Detection : spray with ninhydrin solution R and heat at
115 g/L solution of anhydrous formic acid R. Add 2 mL of a 105 °C for 15 min.
5 g/L solution of 3,3′-diaminobenzidine tetrahydrochloride R. Results : the principal spot in the chromatogram obtained
Allow to stand for 45 min and then adjust to pH 6.0-7.0 with with the test solution is similar in position, colour and size
dilute ammonia R1. Shake the solution for 1 min with 10 mL to the principal spot in the chromatogram obtained with
of toluene R and allow the phases to separate. The absorbance the reference solution.
(2.2.25) of the upper layer measured at 420 nm is not greater D. To 1 mL of a 10 g/L solution of the substance to be
than that of a standard prepared at the same time and in examined in a test tube, add 5 mL of a 20 g/L solution of
the same manner beginning at the words “add 2 mL of an sodium periodate R. Heat on a water-bath and collect the
115 g/L solution of anhydrous formic acid R” and using 5 mL vapour on glass wool moistened with water R and inserted
of selenium standard solution (1 ppm Se) R instead of 10 mL in the opening of the test tube. After heating for 5 min,
of the filtrate. transfer the glass wool to a test tube containing 1 mL of

3948 See the information section on general monographs (cover pages)


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