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.

C24H44BCuF4N4O4
[103694-84-4]
DEFINITION
(T-4)-Tetrakis[1-(isocyano-κC)-2-methoxy-2-
methylpropane]copper(I) tetrafluoroborate.
Content : 10.04 per cent to 11.04 per cent of Cu (Ar 63.5)
(anhydrous substance).
CHARACTERS
Appearance : white or almost white, crystalline powder.
Solubility : slightly soluble in water, freely soluble in anhydrous 80-120 per cent of the expected concentration of copper in
ethanol.
IDENTIFICATION
Infrared absorption spectrophotometry (2.2.24).
Comparison : copper tetramibi tetrafluoroborate CRS.
TESTS
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
colourless (2.2.2, Method I).
pH (2.2.3): 4.5 to 5.5 for solution S.
Related substances. Liquid chromatography (2.2.29). Prepare
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
100.0 mL with the mobile phase. Dilute 1.0 mL of this solution
to 10.0 mL with the mobile phase.
Column :
– size : l = 0.25 m, Ø = 4.6 mm ;
– stationary phase : strong cation-exchange silica gel for
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.
Flow rate : 1.0 mL/min.
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.
Mr 603 Copper stock solution (1 mg/L). To 50 mL of water R in a
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
cent Cu) for ICP R and dilute to 100.0 mL with water R.
Scandium internal standard (10 mg/L). To 50 mL of water R
in a 100 mL plastic volumetric flask add 1.0 mL of heavy
metal-free nitric acid R and 1000 μL of scandium standard
solution (0.1 per cent Sc) for ICP R and dilute to 100.0 mL
with water R.
Reference solutions. Dilute the copper stock solution (1 mg/L)
with water R to prepare a range of reference solutions spanning
the substance to be examined.
Procedure. To 50 μL of the digested sample solution and each
of the reference solutions, add 1.0 mL of the scandium internal
standard (10 mg/L) and 1.0 mL of heavy metal-free nitric
acid R and dilute to 100.0 mL with water R.
Detection :
– copper m/z = 63 ;
STORAGE
In an airtight container, protected from light, at a temperature
of 2 °C to 8 °C.
07/2017:2351
IOBENGUANE SULFATE FOR
RADIOPHARMACEUTICAL
PREPARATIONS
Iobenguani sulfas ad radiopharmaceutica
C16H22I2N6O4S Mr 648
[87862-25-7]

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