QualityGuidances

GENERAL MATERIAL INFORMATION
General Information	Procyclidine Hydrochloride uncoated tablets is consisting of Procyclidine Hydrochloride and Excipients.
Categories
Composition	Each film coated tablet contains: Procyclidine Hydrochloride IP …………2.5 mg & 5 mg
Reference	Indian Pharmacopoeia 2022
Sample Quantity	Chemical Analysis = 60 Tablets   Microbiology Analysis = 20 Tablets
Shelf Life	24 Months
Hazards and Precaution, If any	Use nose mask and hand gloves while sampling at bulk stage
Storage	Store protected from moisture at a temperature not exceeding 30°.

 

S.NO.	TESTS	SPECIFICATIONS			REFERENCE
1.	Description	White colored, round shaped, uncoated tablet having mid break line on one side and other side plain.			IH
2.	Average weight	190mg ± 3%			IH
3.	Uniformity of weight	Within ± 7.5% of the Average weight			IP
4.	Identification	Compare the spectrum with that obtained with procyclidine hydrochloride RS treated in the same manner or with the reference spectrum of procyclidine. B. The powdered tablets give the reactions of chlorides			IP
5.	Hardness	NLT 2.5 kg/cm2			IH
6.	Disintegration Time	NMT 15 minutes			IP
7.	Dimension				IH
8.	Friability	NMT 1.0%			IP
9.	Dissolution	NLT 75%			IP
10.	Leak Test	Should be Pass			IP
11.	Related Substance	Determine by thin-layer chromatography
12.	Assay:				IP
	Each uncoated tablet contains:	Limit
		Claim	In mg	In %
	Procyclidine Hydrochloride I.P.	2.5 mg	2.25 mg to 2.75 mg	90.0% to 110.0%
	Pack size:	10 x10 ( Alu-Alu Pack)
	Shelf life	24 months
Storage: Store in a cool, dark & dry place.
Reference: As per I.P.

 

 

SPECIFICATION OF STABILITY ANALYSIS

S.NO.	TESTS	SPECIFICATIONS			REFERENCE
1.	Description	White colored, round shaped, uncoated tablet having mid break line on one side and other side plain.			IH
2.	Average weight	190mg ± 3%			IH
3.	Uniformity of weight	Within ± 7.5% of the Average weight			IP
4.	Identification	Compare the spectrum with that obtained with procyclidine hydrochloride RS treated in the same manner or with the reference spectrum of procyclidine. B. The powdered tablets give the reactions of chlorides			IP
5.	Hardness	NLT 2.5 kg/cm2			IH
6.	Disintegration Time	NMT 15 minutes			IP
7.	Friability	NMT 1.0%			IP
8.	Dissolution	NLT 75%			IP
9.	Related Substance	Determine by thin-layer chromatography
10.	Assay:				IP
	Each uncoated tablet contains:	Limit
		Claim	In mg	In %
	Procyclidine Hydrochloride I.P.	2.5 mg	2.25 mg to 2.75mg	90.0% to 110.0%
	Pack size:	10 x10 ( Alu-Alu Pack)
	Shelf life	24 months
Storage: Store in a cool, dark & dry place.
Reference: As per I.P.

*Related Substance: once in a year.

*Microbial Limit Test: once in a year .

 

S.NO.	TESTS	SPECIFICATIONS			REFERENCE
1.	Description	White colored, round shaped, uncoated tablet having mid break line on one side and other side plain.			IH
2.	Average weight	190mg ± 3%			IH
3.	Uniformity of weight	Within ± 7.5% of the Average weight			IP
4.	Identification	Compare the spectrum with that obtained with procyclidine hydrochloride RS treated in the same manner or with the reference spectrum of procyclidine. B. The powdered tablets give the reactions of chlorides			IP
5.	Hardness	NLT 2.5 kg/cm2			IH
6.	Disintegration Time	NMT 15 minutes			IP
7.	Dimension				IH
8.	Friability	NMT 1.0%			IP
9.	Dissolution	NLT 75%			IP
10.	Leak Test	Should be Pass			IP
11.	Related Substance	Determine by thin-layer chromatography
12.	Assay:				IP
	Each uncoated tablet contains:	Limit
		Claim	In mg	In %
	Procyclidine Hydrochloride I.P.	5 mg	4.5 mg to 6.5 mg	90.0% to 110.0%
	Pack size:	10 x10 ( Alu-Alu Pack)
	Shelf life	24 months
Storage: Store in a cool, dark & dry place.
Reference: As per I.P.

  SPECIFICATION OF STABILITY ANALYSIS

 

S.NO.	TESTS	SPECIFICATIONS			REFERENCE
1.	Description	White colored, round shaped, uncoated tablet having mid break line on one side and other side plain.			IH
2.	Average weight	190mg ± 3%			IH
3.	Uniformity of weight	Within ± 7.5% of the Average weight			IP
4.	Identification	Compare the spectrum with that obtained with procyclidine hydrochloride RS treated in the same manner or with the reference spectrum of procyclidine. B. The powdered tablets give the reactions of chlorides			IP
5.	Hardness	NLT 2.5 kg/cm2			IH
6.	Disintegration Time	NMT 15 minutes			IP
7.	Friability	NMT 1.0%			IP
8.	Dissolution	NLT 75%			IP
9.	Related Substance	Determine by thin-layer chromatography
10.	Assay:				IP
	Each uncoated tablet contains:	Limit
		Claim	In mg	In %
	Procyclidine Hydrochloride I.P.	5 mg	4.5 mg to 6.5mg	90.0% to 110.0%
	Pack size:	10 x10 ( Alu-Alu Pack)
	Shelf life	24 months
Storage: Store in a cool, dark & dry place.
Reference: As per I.P.

*Related Substance: once in a year.

*Microbial Limit Test: once in a year .

 

 

 

 

STANDARD TESTING PROCEDURE

• Description: Visual

 

• Average Weight: Check weight of 20 tablets at randomly and calculate the average weight by formula.

Average weight (mg) =   wt of 20 tablets (gm) x 1000

20

• Uniformity of weight:

Weigh 20 tablets selected at random and calculate the average weight. Not more than two of the  individual weights deviate from the average weight by more than the percentage shown in table.

Tablets were weighed individually and the percentage of deviation of its weight from the average weight was determined for each tablet. Formula to calculate the percentage of deviation.

Deviation (%) =  Weight of each tablet – Average weight    x 100

Average weight

Average weight of tablets	Percentage deviation
More than 80mg but Less than 250mg	±7.5%

4.0)     Identification Test:

2. Dissolve a quantity of the powdered tablets containing about 25 mg of Procyclidine Hydrochloride in 10 ml of water, shake with 20 ml ofether and discard the ether layer. Make the aqueous layer alkaline with 2 M sodium hydroxide and extract with two quantities, each of 20 ml, ofether. Wash the combined ether extracts with two quantities, each of 10 ml, of water, dry by shaking with anhydrous sodium sulphate, filter and evaporate the filtrate to dryness. If necessary, induce crystallization by scratching with a glass rod. On the residue, determine by infrared absorption spectrophotometry (2.4.6). Compare the spectrum with that obtained with procyclidine hydrochloride RS treated in the same manner or with the reference spectrum of procyclidine.
3. The powdered tablets give the reactions of chlorides

5.0)     Hardness:

The standard method used for tablet hardness testing is compression testing. The tablet is placed between two jaws that crush the tablet. The machine measures the force applied to the tablet and detects when it fractures.

6.0)     Disintegration Time: 

Unless otherwise stated in the individual monograph, introduce one tablet into each tube and add a disc to each tube. The assembly is suspended in the liquid medium in a suitable vessel, preferably a 1-litre beaker. The volume of liquid is such that the wire mesh at its highest point is at least 15mm below the surface of the liquid, and at its lower point is at least 25mm above the bottom of the beaker. At no time should the top of the basket-rack assembly become submerged. There is a thermostatic arrangement for heating the liquid and maintaining the temperature at 37±2°.

If 1 or 2 tablets fail to disintegrate, repeat the test on 12 additional tablets; not less than 16 of the total of 18 tablets tested disintegrate.

If the tablets adhere to the disc and the preparation under examination fails to comply, repeat the test omitting the disc. The preparation complies with the test if all the tablets in the repeat test disintegrate.

7.0)     Dimension of Tablet:

Diameter and thickness are determined by vernier calliper in mm.

8.0)      Friability:

The test is applicable to compressed tablets and is intended to determine the physical strength of tablets. Tablets with a unit weight equal to or less than 650 mg, take a sample of whole tablets corresponding as near as possible to 6.5 g. For tablets with a unit weight of more than 650mg, take a sample of 10 whole tablets. The tablets should be carefully dedusted prior to testing. Accurately weigh the tablet sample, and place the tablets in the drum. Rotate the drum 100 times and remove the tablets. Remove any loose dust from the tablets as before, and accurately weigh.

The test is run only once unless the results are difficult to interpret or if the weight loss is greater than the target value, in which case, the test is repeated twice and the mean of the three tests is determined.

% Friability = W₁ – W₂ X 100

                                                      W₁

W₁= Initial weight                  W₂= Final weight

            A maximum loss of weight (From a single test or from the mean of three tests) not greater than 1.0 percent is acceptable for most tablets.

If obviously cracked, chipped or broken tablets are present in the sample after tumbling, the sample fails the test.

9.0)      Dissolution:

            Apparatus: Paddle

            Medium: 900 ml of water

            Time: 45 minutes

            Speed: 50 rpm

            Withdraw a suitable volume of medium and pool the medium,filtter.Follow the procedure describe under assay with necessary modifications and calculate the content of Procyclidine Hydrochloride .

            Limit:

1. N.L.T. 75% of the stated amount of Procyclodine .

10.0)   Leak test:

The apparatus is used to test for the integrity of packed strips, blisters and Alu-Alu Blister pack containing tablets. Ensure apparatus bath is filled with purified water upto mark indicated and add 0.5% crystal violet solution in water. Samples are placed into the desiccators and the lid is placed in position. The pump starts to produce a vacuum 15inHg inside the desiccators and the vacuum is held for 1 minute. The sample remains at the required vacuum level for given time interval buzzer will sound after time is over and will cut off the vacuum pump. As the package is immersed in a colored dye solution the venting of the desiccators will allow any holes to be penetrated by the dye and the contents of the flexible packaging will also be stained with the same coloring material.

Examine all the strips for any leakage by opening the pockets manually. If anyone pocket shows evidence of leakage, reject the sample, stop the Blister / Strip machine and immediately take corrective action.

11.0)    Determine by thin-layer chromatography, coating the plate with silica gel GF254.

Mobile phase. A mixture of 100 volumes of ether and 1 volume of strong ammonia solution.

Test solution. Shake a quantity of the powdered table containing 25 mg of Procyclidine hydrochloride          with 5 ml chlorojiym and filter.

Reference solution (a). A 0.001 per cent w/v solution of 1-pheny1-3-pyrrolidinopropan-1-one hydrochloride IPRS in chloroform.

Reference solution (b). Dilute 1 volume of test solution to 200 volumes with chloroform.

Appy to the plate 20 µ of each solution. After development, dry the plate at 105° for 15 minutes and examine under

ultaviolet light at 254 nm. Any spot corresponding to l –phenyl  3_pyrrolidinopropan-l-one in the chromatogram obtained with

the test solution is not more intense than the spot in the chromatogram obtained with reference solution (a) (0.2 per cent). Spray the plate with dilute potassium iodohismuthate solution. Any secondary spot in the chromatogram obtained with the test solution is not more intense than the spot in the chromatogram obtained with reference solution (b) (0.5 per cent). Ignore any spot due to excipients on the line of  application .

12.0)     Assay: . Weigh and powder 20 tablets. Weigh a quantity of the powder containing about 2.5 mg of Procyclidine Hydrochloride, transfer to a 100-m1 volumetric flask, add 10.0 ml of water and mix, and dilute to volume with a 0.025 per cent w/v solution of bmmocresol Purple in 2 per cent v/v solution ofglacial acetic acid. Allow the undissolved particles to settle. Transfer 5.0 ml of the supernatant solution to a separating funnel, extract with 20.0 ml ofchlorolbrm and filter the extract, discarding the first 5 ml of the filtrate. Measure the absorbance of the filtrate at the maximum at about 405 nm (2.4.7), using as the blank a solution prepared by treating 0.5 ml of water and 4.5 ml of a 0.025 per cent w/v solution of bromocresol purple in the same manner beginning at the words extract with 20 ml of chloroform ……….’’

calculate the content of C 19H29NO.HCI from the absorbance obtained by repeating the operation using rocyclidine hydrochloride RS in place of the powdered tablets.