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Haloperidol decanoate
nitric acid R and filter. To 1 ml of the filtrate add 1 ml of water R. The solution gives reaction (a) of chlorides TESTS
Appearance of solution. Dissolve 2.0 g in methylene
chloride R and dilute to 20 ml with the same solvent. The solution is clear (2.2.1) and not more intensely coloured than reference solution B (2.2.2, Method II).
Related substances. Examine by liquid chromatography
(2.2.29). Prepare the solutions immediately before use and D. 4-[4-(4-chlorophenyl)-4-hydroxypiperidin-1-yl]-1-[4-[4-(4- Test solution. Dissolve 0.100 g of the substance to be chlorophenyl)-4-hydroxypiperidin-1-yl]phenyl]butan-1-one, examined in methanol R and dilute to 10.0 ml with the same solvent.
Reference solution (a). Dissolve 2.5 mg of bromperidol decanoate CRS and 2.5 mg of haloperidol decanoate CRS in methanol R and dilute to 50.0 ml with the same solvent.
Reference solution (b). Dilute 5.0 ml of the test solution to 100.0 ml with methanol R. Dilute 1.0 ml of this solution to 10.0 ml with methanol R.
The chromatographic procedure may be carried out using: E. R = H, R′ = Cl: 4-[4-(4′-chlorobiphenyl-4-yl)-4- — a stainless steel column 0.1 m long and 4.0 mm in internal hydroxypiperidin-1-yl]-1-(4-fluorophenyl)butan-1-one, diameter packed with base-deactivated octadecylsilyl silica gel for chromatography R (3 µm), F. R = Cl, R′ = H: 4-[4-(3′-chlorobiphenyl-4-yl)-4- — as mobile phase at a flow rate of 1.5 ml/min the following hydroxypiperidin-1-yl]-1-(4-fluorophenyl)butan-1-one.
linear gradient programme:Mobile phase A. A 27 g/l solution of tetrabutylammonium 01/2005:1431
hydrogen sulphate R,Mobile phase B. Acetonitrile R, HALOPERIDOL DECANOATE
Mobile phase A
Mobile phase B
(per cent V/V)
(per cent V/V)
— as detector a spectrophotometer set at 230 nm.
Equilibrate the column for at least 30 min with acetonitrile R and then equilibrate at the initial eluent composition for at M 530.1 Adjust the sensitivity of the system so that the height of the principal peak in the chromatogram obtained with 10 µl of reference solution (b) is at least 50 per cent of the full scale Haloperidol decanoate contains not less than 98.5 per cent and not more than the equivalent of 101.0 per cent of 4-(4- Inject 10 µl of reference solution (a). When the chromatogram chlorophenyl)-1-[4-(4-fluorophenyl)-4-oxobutyl]piperidin-4-yl is recorded in the prescribed conditions the retention times decanoate, calculated with reference to the dried substance.
are: haloperidol decanoate about 24 min and bromperidol decanoate about 24.5 min. The test is not valid unless the resolution between the peaks due to haloperidol decanoate A white or almost white powder, practically insoluble in and bromperidol decanoate is at least 1.5. If necessary, water, very soluble in alcohol, in methanol and in methylene adjust the gradient or the time programme for the linear Inject 10 µl of methanol R as a blank, 10 µl of the test solution and 10 µl of reference solution (b). In the chromatogram obtained with the test solution: the area of A. Examine by infrared absorption spectrophotometry any peak apart from the principal peak, is not greater than (2.2.24), comparing with the spectrum obtained with the area of the principal peak in the chromatogram obtained haloperidol decanoate CRS. Examine the substances with reference solution (b) (0.5 per cent); the sum of the prepared as mulls in liquid paraffin R.
areas of all the peaks apart from the principal peak, is not B. To 0.1 g in a porcelain crucible add 0.5 g of anhydrous greater than three times the area of the principal peak in sodium carbonate R. Heat over an open flame for 10 min. the chromatogram obtained with the reference solution (b) Allow to cool. Take up the residue with 5 ml of dilute (1.5 per cent). Disregard any peak due to the blank and See the information section on general monographs (cover pages) Halothane
any peak with an area less than 0.1 times the area of the principal peak in the chromatogram obtained with reference solution (b).
Loss on drying (2.2.32). Not more than 0.5 per cent,
determined on 1.000 g by drying in vacuo at 30 °C.
Sulphated ash (2.4.14). Not more than 0.1 per cent,
determined on 1.0 g in a platinum crucible.
ASSAYDissolve 0.425 g in 50 ml of a mixture of 1 volume of anhydrous acetic acid R and 7 volumes of methyl ethyl ′ = Cl: 4-(4′-chlorobiphenyl-4-yl)-1-[4-(4- fluorophenyl)-4-oxobutyl]piperidin-4-yl decanoate, ketone R. Titrate with 0.1 M perchloric acid using 0.2 ml of naphtholbenzein solution R as indicator.
F. R = Cl, R′ = H: 4-(3′-chlorobiphenyl-4-yl)-1-[4-(4- fluorophenyl)-4-oxobutyl]piperidin-4-yl decanoate, 1 ml of 0.1 M perchloric acid is equivalent to 53.01 mg of STORAGEStore at room temperature below 25 °C, protected from light.
IMPURITIESSpecified impurities: A, B, C, D, E, F, G, H, I, J, K.
Other detectable impurities: L. H. n = 5: 4-(4-chlorophenyl)-1-[4-(4-fluorophenyl)-4- I. n = 6: 4-(4-chlorophenyl)-1-[4-(4-fluorophenyl)-4- J. n = 8: 4-(4-chlorophenyl)-1-[4-(4-fluorophenyl)-4- K. n = 9: 4-(4-chlorophenyl)-1-[4-(4-fluorophenyl)-4- A. R1 = F, R2 = R3 = R4 = H: 1-[4-(4-fluorophenyl)-4- oxobutyl]-4-phenylpiperidin-4-yl decanoate, B. R1 = R2 = H, R3 = F, R4 = Cl: 4-(4-chlorophenyl)-1-[4-(2- fluorophenyl)-4-oxobutyl]piperidin-4-yl decanoate, 01/2005:0393
C. R1 = F, R2 = C H , R3 = H, R4 = Cl: 4-(4-chlorophenyl)- HALOTHANE
1-[4-(3-ethyl-4-fluorophenyl)-4-oxobutyl]piperidin-4-yl DEFINITIONHalothane is (RS)-2-bromo-2-chloro-1,1,1-trifluoroethane to which 0.01 per cent m/m of thymol has been added.
CHARACTERSA clear, colourless, mobile, heavy, non-flammable liquid, slightly soluble in water, miscible with ethanol and with D. 4-(4-chlorophenyl)-1-[4-[4-[4-(4-chlorophenyl)-4- hydroxypiperidin-1-yl]phenyl]-4-oxobutyl]piperidin-4-yl A. It complies with the test for distillation range (see Tests).
General Notices (1) apply to all monographs and other texts

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