Procyclidine Tablets

Anticholinergic.

Procyclidine Tablets contain Procyclidine Hydrochloride.

The tablets comply with the requirements stated under Tablets and with the following requirements.

90.0  to 110.0% of the stated amount.

A.  Disperse a quantity of the powdered tablets containing 25  mg of Procyclidine Hydrochloride in 10  ml of water, shake with 20  ml of ether and discard the ether layer. Make the aqueous layer alkaline with 2m sodium hydroxide and extract with two 20-ml quantities of ether. Wash the combined ether extracts with two 10-ml quantities of water, dry by shaking with anhydrous sodium sulphate, filter and evaporate the filtrate to dryness. If necessary, induce crystallisation by scratching with a glass rod. The infrared absorption spectrum of the residue, Appendix II A, is concordant with the reference spectrum of procyclidine (RS 291).

B.  The powdered tablets yield the reactions characteristic of chlorides, Appendix VI.

Carry out the method for thin-layer chromatography, Appendix III A, using the following solutions in chloroform.

(1)  Shake a quantity of the powdered tablets containing 25  mg of Procyclidine Hydrochloride with 5  ml of chloroform and filter.

(2)  0.001% w/v of 1-phenyl-3-pyrrolidinopropan-1-one hydrochloride BPCRS.

(3)  Dilute 1  volume of solution (1) to 200  volumes.

(a)  Use as the coating silica gel GF₂₅₄.

(b)  Use the mobile phase as described below.

(c)  Apply 20 µl of each solution.

(d)  Develop the plate to 15 cm.

(e)  After removal of the plate, dry at 105° for 15  minutes and examine under ultraviolet light (254  nm).

(f)  Spray the plate with dilute potassium iodobismuthate solution.

1  volume of 13.5m ammonia and 100  volumes of ether.

When examined under ultraviolet light (254  nm) in the chromatogram obtained with solution (1):

any spot corresponding to 1-phenyl-3-pyrrolidinopropan-1-one is not more intense than the spot in the chromatogram obtained with solution (2) (0.2%).

When examined after spraying with dilute potassium iodobismuthate solution in the chromatogram obtained with solution (1):

any secondary spot is not more intense than the spot in the chromatogram obtained with solution (3) (0.5%).

Disregard any spot due to excipient on the line of application.

Weigh and finely powder 20  tablets. Record second-derivative ultraviolet absorption spectra of the following solutions, Appendix II B, in the range 220  to 280  nm. For solution (1) add 80  ml of 0.1m hydrochloric acid to a quantity of the powdered tablets containing 25  mg of Procyclidine Hydrochloride, mix with the aid of ultrasound for 15  minutes, cool, dilute to 100  ml with 0.1m hydrochloric acid and filter through a glass fibre paper having a maximum pore size of 0.7 µm (Whatman GF/F paper is suitable) discarding the first 10  ml of filtrate. Solution (2) contains 0.025% w/v of procyclidine hydrochloride BPCRS in 0.1m hydrochloric acid.

For each solution measure the amplitude from the largest trough at about 257  nm to the largest peak at about 254  nm. Calculate the content of C₁₉H₂₉NO,HCl using the declared content of C₁₉H₂₉NO,HCl in procyclidine hydrochloride BPCRS.