Zuclopenthixol Decanoate

EUROPEAN PHARMACOPOEIA 11.
0 Zuclopenthixol decanoate
Test solution. Dissolve 0.25 g of the substance to be examined

in ethylene chloride R, add 0.5 mL of the internal standard
solution and dilute to 5.0 mL with ethylene chloride R.
Reference solution. Dilute 4.5 mL of 2-propanol R to 100.0 mL
with ethylene chloride R. To 1.0 mL of the solution add 10.0 mL
of the internal standard solution and dilute to 100.0 mL with
ethylene chloride R. B. (7RS)-6-(5-chloropyridin-2-yl)-7-hydroxy-6,7-dihydro-
Column : 5H-pyrrolo[3,4-b]pyrazin-5-one,
– material : fused silica ;
– size : l = 10 m, Ø = about 0.53 mm ;
– stationary phase : styrene-divinylbenzene copolymer R (film
thickness 20 μm).
Carrier gas : helium for chromatography R.
Flow rate : 4 mL/min. C. 6-(5-chloropyridin-2-yl)-6,7-dihydro-5H-pyrrolo-
Temperature : [3,4-b]pyrazin-5-one.
Time Temperature
04/2021:1707
(min) (°C)
Column 0-5 50
5 - 10 50 → 70
10 - 14 70
14 - 20.5 70 → 200
ZUCLOPENTHIXOL DECANOATE
20.5 - 27.5 200 Zuclopenthixoli decanoas
Injection port 150
Detector 250
Detection : flame ionisation.

Injection : 1 μL.
Calculate the percentage content m/m of 2-propanol taking its
density to be 0.785 g/mL at 20 °C.
C32H43ClN2O2S Mr 555.2
Limit :
[64053-00-5]
– 2-propanol : maximum 0.7 per cent m/m.
Sulfated ash (2.4.14) : maximum 0.1 per cent, determined on DEFINITION
1.0 g. 2-[4-[3-[(9Z)-2-Chloro-9H-thioxanthen-9-ylidene]propyl]-
piperazin-1-yl]ethyl decanoate.
ASSAY Content : 98.0 per cent to 102.0 per cent (dried substance).
Dissolve 0.300 g in a mixture of 10 mL of anhydrous acetic
acid R and 40 mL of acetic anhydride R. Titrate with 0.1 M CHARACTERS
perchloric acid, determining the end-point potentiometrically Appearance : yellow, viscous, oily liquid.
(2.2.20). Solubility : very slightly soluble in water, very soluble in
1 mL of 0.1 M perchloric acid is equivalent to 38.88 mg ethanol (96 per cent) and in methylene chloride.
of C17H17ClN6O3.
IDENTIFICATION
STORAGE Infrared absorption spectrophotometry (2.2.24).
Protected from light. Comparison : Ph. Eur. reference spectrum of zuclopenthixol
decanoate.
IMPURITIES
Specified impurities : B. TESTS
Other detectable impurities (the following substances would, Appearance of solution. The solution is clear (2.2.1).
if present at a sufficient level, be detected by one or other of Using an ultrasonic bath, dissolve 1.0 g in ethanol (96 per
the tests in the monograph. They are limited by the general cent) R and dilute to 20.0 mL with the same solvent.
acceptance criterion for other/unspecified impurities and/or Related substances. Liquid chromatography (2.2.29). Carry
by the general monograph Substances for pharmaceutical use out the test protected from light and prepare the solutions
(2034). It is therefore not necessary to identify these impurities immediately before use.
for demonstration of compliance. See also 5.10. Control of Solution A. Dissolve 8.89 g of docusate sodium R in water
impurities in substances for pharmaceutical use) : A, C. for chromatography R, stirring for about 6-8 h, and dilute to
1000 mL with the same solvent.
Test solution. Dissolve 25.0 mg of the substance to be
examined in acetonitrile R and dilute to 100.0 mL with the
same solvent.
Reference solution (a). Dilute 1.0 mL of the test solution to
100.0 mL with acetonitrile R.
Reference solution (b). Dissolve 5.0 mg of zuclopenthixol
A. (5RS)-6-(5-chloropyridin-2-yl)-7-oxo-6,7-dihydro- impurity B CRS in acetonitrile R and dilute to 100.0 mL with
5H-pyrrolo[3,4-b]pyrazin-5-yl 4-methylpiperazine-1- the same solvent. Dilute 5.0 mL of this solution to 100.0 mL
carboxylate 4-oxide (zopiclone oxide), with acetonitrile R.
General Notices (1) apply to all monographs and other texts 4439
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Zuclopenthixol decanoate EUROPEAN PHARMACOPOEIA 11.0
Reference solution (c). Dissolve the contents of a vial – disregard limit : 0.05 times the area of the principal peak
of zuclopenthixol for system suitability CRS (containing in the chromatogram obtained with reference solution (a)
impurities A, B and C) in 1 mL of methanol R. (0.05 per cent).
Column : Loss on drying (2.2.32) : maximum 0.5 per cent, determined
– size : l = 0.25 m, Ø = 4.6 mm ; on 1.000 g by drying in vacuo at 60 °C for 3 h.
– stationary phase : end-capped octadecylsilyl silica gel for Sulfated ash (2.4.14): maximum 0.1 per cent, determined on
chromatography R (5 μm) ; 1.0 g.
– temperature : 40 °C.
Mobile phase : mix 25 volumes of solution A and 75 volumes ASSAY
of anhydrous ethanol R, then add 0.1 volumes of phosphoric Dissolve 0.250 g in 50 mL of anhydrous acetic acid R. Titrate
acid R. with 0.1 M perchloric acid, determining the end-point
Flow rate : 1.0 mL/min. potentiometrically (2.2.20).
Detection : spectrophotometer at 270 nm. 1 mL of 0.1 M perchloric acid is equivalent to 27.76 mg
Injection : 20 μL. of C32H43ClN2O2S.
Run time : twice the retention time of zuclopenthixol STORAGE
decanoate.
Under an inert gas in an airtight container, protected from
Identification of impurities : use the chromatogram supplied light, at − 20 °C or below.
with zuclopenthixol for system suitability CRS and the
chromatograms obtained with reference solutions (b) and (c) IMPURITIES
to identify the peaks due to impurities A, B and C.
Specified impurities : A, B, C.
Relative retention with reference to zuclopenthixol decanoate
(retention time = about 12 min): impurity C = about 0.4 ;
impurity B = about 0.5 ; impurity A = about 1.1.
System suitability : reference solution (c) :
– peak-to-valley ratio : minimum 2.0, where Hp = height
above the baseline of the peak due to impurity C and
Hv = height above the baseline of the lowest point of the
curve separating this peak from the peak due to impurity B ;
and minimum 2.5, where Hp = height above the baseline A. 2-[4-[3-[(9E)-2-chloro-9H-thioxanthen-9-ylidene]propyl]-
of the peak due to impurity A and Hv = height above the piperazin-1-yl]ethyl decanoate,
baseline of the lowest point of the curve separating this
peak from the peak due to zuclopenthixol decanoate.
Limits :
– impurity A : not more than 1.3 times the area of the
principal peak in the chromatogram obtained with
reference solution (a) (1.3 per cent) ;
– impurity B : not more than 0.2 times the area of the
reference solution (b) (0.2 per cent) ; B. 2-chloro-9H-thioxanthen-9-one,
– impurity C : not more than 0.3 times the area of the
reference solution (a) (0.3 per cent) ;
– unspecified impurities : for each impurity, not more than
0.1 times the area of the principal peak in the chromatogram
obtained with reference solution (a) (0.10 per cent) ;
– total : not more than 1.5 times the area of the principal peak
in the chromatogram obtained with reference solution (a) C. 2-[4-[3-[(9Z)-2-chloro-9H-thioxanthen-9-ylidene]propyl]-
(1.5 per cent) ; piperazin-1-yl]ethanol.
4440 See the information section on general monographs (cover pages)

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EUROPEAN PHARMACOPOEIA 11.

Test solution. Dissolve 0.25 g of the substance to be examined

Detection : ﬂame ionisation.

4440 See the information section on general monographs (cover pages)

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