MPH215

Limit tests
Ipratopium Bromide

Test Solution: Dissolve 20 mg of the sample in methanol and make up to 1.0 ml with
the same solvent. 20 mg/ml

Reference Solution (c): Dissolve 5 mg Impurity A in 100 ml methanol. Dilute 2 ml of

the resulting solution to 5 ml with methanol. 0.02 mg/ml

Apply 5 µl of each solution to a silica TLC plate and develop with a suitable solvent.
Any spot due to Impurity A in the test chromatogram is not more intense than the spot
from Reference Solution (c).

What is the permitted amount of Impurity A in Ipratopium Bromide BP? 0.1% w/w

Prilocaine

Test Solution: Dissolve 20 mg of the sample in ethanol and make up to 5.0 ml with
the same solvent. 4 mg/ml

Reference Solution (a): Dissolve 4 mg 2-chloro-N-(2-methylphenyl)propanamide in

100 ml ethanol. Dilute 2 ml of the resulting solution to 10 ml with methanol.
0.008 mg/ml

Reference Solution (b): Dissolve 1 mg 2-methylbenzenamine in 100 ml ethanol. Dilute

2 ml of the resulting solution to 50 ml with methanol. 0.0004 mg /ml

Apply 5 µl of each solution to a silica TLC plate and develop with a suitable solvent.
Any spot from 2-chloro-N-(2-methylphenyl)propanamide in the test chromatogram is
not more intense than the spot from Reference Solution (a).

Any spot from 2-methylbenzenamine in the test chromatogram is not more intense
than the spot from Reference Solution (b).

What is the permitted amount of impurities in Prilocaine BP?

0.2 %w/w 2-chloro-N-(2-methylphenyl)propanamide
100 ppm (0.01 %w/w) 2-methylbenzenamine
Diphenoxylate Hydrochloride

Test Solution: Dissolve 1.0 g of the sample in methanol/dichloromethane and make up

to 20 ml with the same solvent 50 mg/ml

Reference Solution (a): Dilute 1 ml Test Solution to 20 ml with

methanol/dichloromethane and then 1 ml of the resulting solution to 10 ml with the
same solvent. 0.25 mg/ml

Apply 5 µl of each solution to a silica TLC plate and develop with a suitable solvent.
No spot from the Test Solution apart from the principal spot is more intense than the
spot from Reference Solution (a).

What is the maximum permitted amount of impurities in this drug? 0.5 %w/w

Meprobamate

Test Solution: Dissolve 0.2 g of the sample in ethanol and make up to 10 ml with the
same solvent 20 mg/ml

Reference Solution (a): Dilute 1 ml Test Solution to 20 ml with ethanol and then 1 ml
of the resulting solution to 5 ml with the same solvent. 0.2 mg/ml

Reference Solution (b): Dilute 1 ml Test Solution to 20 ml with ethanol and then 1 ml
of the resulting solution to 10 ml with the same solvent.0.1 mg/ml

Apply 5 µl of each solution to a silica TLC plate and develop with a suitable solvent.
No spot from the Test Solution apart from the principal spot is more intense than the
spot from Reference Solution (a).

Not more than 1 spot from the Test Solution apart from the principal spot is more
intense than the spot from Reference Solution (b).

What is the maximum permitted amount of impurities in this drug?

No individual impurity more than 1 %w/w
Not more than 1 impurity more than 0.5 %w/w