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EUROPEAN PHARMACOPOEIA 9.

2 Iobenguane sulfate for radiopharmaceutical preparations

07/2017:2547 Detection : spectrophotometer at 230 nm.


Injection : 20 μL.
Run time : twice the retention time of copper tetramibi.
Retention time : copper tetramibi = about 5 min.
System suitability : reference solution :
COPPER TETRAMIBI
– symmetry factor : maximum 1.35 for the principal peak.
TETRAFLUOROBORATE FOR Calculation of percentage contents :
RADIOPHARMACEUTICAL – for each impurity, use the concentration of copper tetramibi
PREPARATIONS in the reference solution.
Limits :
Cupri tetramibi tetrafluoroboras ad – unspecified impurities : for each impurity, maximum
radiopharmaceutica 0.10 per cent ;
– total : maximum 0.2 per cent ;
– reporting threshold : 0.05 per cent.
Water (2.5.32) : maximum 0.5 per cent, determined on 0.100 g.
Use direct sample introduction.

ASSAY
Inductively coupled plasma-mass spectrometry (2.2.58).
Test solution. Place 20.0 mg of the substance to be examined
in a polytetrafluoroethylene tube for microwave digestion and
add 4.5 mL of heavy metal-free nitric acid R and 1.5 mL of
strong hydrogen peroxide solution R. Treat by digestion in a
microwave oven and dilute to 25.0 mL with water R.
C24H44BCuF4N4O4 Mr 603 Copper stock solution (1 mg/L). To 50 mL of water R in a
[103694-84-4] 100 mL plastic volumetric flask add 1.0 mL of heavy metal-free
nitric acid R and 100 μL of copper standard solution (0.1 per
DEFINITION cent Cu) for ICP R and dilute to 100.0 mL with water R.
(T-4)-Tetrakis[1-(isocyano-κC)-2-methoxy-2- Scandium internal standard (10 mg/L). To 50 mL of water R
methylpropane]copper(I) tetrafluoroborate. in a 100 mL plastic volumetric flask add 1.0 mL of heavy
Content : 10.04 per cent to 11.04 per cent of Cu (Ar 63.5) metal-free nitric acid R and 1000 μL of scandium standard
(anhydrous substance). solution (0.1 per cent Sc) for ICP R and dilute to 100.0 mL
with water R.
CHARACTERS Reference solutions. Dilute the copper stock solution (1 mg/L)
Appearance : white or almost white, crystalline powder. with water R to prepare a range of reference solutions spanning
Solubility : slightly soluble in water, freely soluble in anhydrous 80-120 per cent of the expected concentration of copper in
ethanol. the substance to be examined.
Procedure. To 50 μL of the digested sample solution and each
IDENTIFICATION of the reference solutions, add 1.0 mL of the scandium internal
Infrared absorption spectrophotometry (2.2.24). standard (10 mg/L) and 1.0 mL of heavy metal-free nitric
Comparison : copper tetramibi tetrafluoroborate CRS. acid R and dilute to 100.0 mL with water R.
Detection :
TESTS
– copper m/z = 63 ;
Solution S. Dissolve 25 mg in carbon dioxide-free water R and – scandium m/z = 45.
dilute to 10.0 mL with the same solvent.
Appearance of solution. Solution S is clear (2.2.1) and STORAGE
colourless (2.2.2, Method I). In an airtight container, protected from light, at a temperature
pH (2.2.3): 4.5 to 5.5 for solution S. of 2 °C to 8 °C.
Related substances. Liquid chromatography (2.2.29). Prepare 07/2017:2351
the solutions immediately before use.
Test solution. Dissolve 50.0 mg of the substance to be
examined in the mobile phase and dilute to 10.0 mL with the
mobile phase.
Reference solution. Dilute 1.0 mL of the test solution to IOBENGUANE SULFATE FOR
100.0 mL with the mobile phase. Dilute 1.0 mL of this solution
to 10.0 mL with the mobile phase.
RADIOPHARMACEUTICAL
Column : PREPARATIONS
– size : l = 0.25 m, Ø = 4.6 mm ;
– stationary phase : strong cation-exchange silica gel for
Iobenguani sulfas ad radiopharmaceutica
chromatography R (5 μm) ;
– temperature : 20 °C.
Mobile phase : mix 40 volumes of acetonitrile R1 and
60 volumes of a 20.4 g/L solution of potassium dihydrogen
phosphate R, previously adjusted to pH 6.0 with a 56.1 g/L
solution of potassium hydroxide R. C16H22I2N6O4S Mr 648
Flow rate : 1.0 mL/min. [87862-25-7]

General Notices (1) apply to all monographs and other texts 4435