testing of packaging material


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TESTING OF PACKAGING MATERIAL Presented by: Mr. Sandip S. Herma M.Pharm.(sem-1),Q.A., Roll No:33 Year:2012-13 Guided by: Ms. Heena Bagada Assistant Professor & Ms. Aashka Jani Assistant Professor DEPARTMENT OF PHARMACEUTICAL SCIENCE SAURASHTRA UNIVERSITY, RAJKOT. 1

Why is it necessary? :

Why is it necessary? By testing of packaging material, we can check that this material is of required quality or not. Different tests are carried out based on the property of the material and purpose of its use. Packaging material is not only a protecting layer but also affect the stability and quality of the product. So it is necessary to qualify the packaging material as per standard data to maintain the throughout quality of the product. 2

The purpose of packaging:

The purpose of packaging

Hazard Encountered By The Package:

Hazard Encountered By The Package

Environmental Hazard:

Environmental Hazard

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Different type of packaging material used for pharmaceutical products: Glass Metal Plastic Rubber 6




GLASS Glass is one of the most widely used materials for parenteral products. So special care has to be taken in case of the glass. Each glass container has to be tested by following pharmacopoeial tests : Test for surface hydrolytic resistance Test for hydrolytic resistance of powdered glass Light transmission test for colored glass Test for resistance to thermal shock Test for Arsenic 8


HYDROLYTIC RESISTANCE TEST SurfaceHRT powder glassHRT PRINCIPLE: Amount of alkali leached from the glass is determined in the test. The container is filled with the pure water and maintained at specified autoclaving condition for specified time period. The leached alkali is titrated against the acid. So at neutralization point it will give the amount of alkali leached. 9

Test for surface hydrolytic resistance:

Test for surface hydrolytic resistance Nominal capacity of container (ml) Number of containers to be used Volume of test solution to be used for titration (ml) Up to 3 20 25 5 or less 10 50 6 to 30 5 50 More than 30 3 100 Take no. of container as specified below: 10

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Wash with CO 2 free water Fill it with CO 2 free water(up to maximum vol.) Autoclave(120 o C for 60 min. ) Take sample of water and titrate against 0.01N HCl Blank reading Amount of acid require must meet the specification of IP as given in next slide. 11

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Capacity of container [corresponding to cent average overflow volume (ml)] Volume of 0.01M hydrochloric acid per 100 ml of test solution Type I or II glass (ml) Type III glass (ml) NMT 1 2.0 20.0 MT 1 but NMT 2 1.8 17.6 MT 2 but NMT 5 1.3 13.2 MT 5 but NMT 10 1.0 10.2 MT 10 but NMT 20 0.80 8.1 MT 20 but NMT 50 0.60 6.1 MT 50 but NMT 100 0.50 4.8 MT 100 but NMT 200 0.40 3.8 MT 200 but NMT 500 0.30 2.9 MT 500 0.20 2.2 12

Test for hydrolytic resistance of powder glass:

Test for hydrolytic resistance of powder glass Hammer the container & collect 100g glass ( fragments should not be greater than 25mm) Powder it to obtain 20gm fragment on retain on 250 micron sieve but pass through 425 micron sieve(as per IP) Magnet passing to purify Now perform as per previous test by adding 100ml CO2 free water And Match the result with IP specifications 13

Light transmission test for colored glass:

Light transmission test for colored glass Break glass container with carborundum or diamond wheel Select wall section Put it in specimen holder of spectrometer with care Place test specimen in the spectrometer with its cylindrical axis parallel to the slit and in such a way light beam is perpendicular to the section Measure the transmission of specimen with reference to air in spectral region of the 290-450 nm continuously or with interval of 20 nm. 14

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The observed light transmission for colored glass should be not more than 10% at any wavelength in the range of 290-450 nm, irrespective of the type and capacity of container. 15

Test for resistance to thermal shock:

Test for resistance to thermal shock Particularly used for blood products or biological product Empty container in autoclave(140 o C for 30min) Place in oven(250 o C for 1 hr) Fill 70% container with 0.9% of NaCl and cool to the -20 o C for 1hr After restoring to room temperature the container must comply with test for resistance to centrifugation 16

Test for Arsenic:

Test for Arsenic Carry out the test on ampoules The inner and outer surfaces are washed five times with freshly distilled water. Prepare a test solution as described in the test for Hydrolytic resistance for an adequate number of ampoules to produce 50 ml. Pipette 10 ml of the test solution from the combined contents of all the ampoules into a flask, add 10 ml of nitricacid and evaporate to dryness on a water-bath. Dry the residue in an oven at 130° for 30 minutes. 17

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Cool, add to the residue 10.0 ml of hydrazine- molybdate reagent swirl to dissolve and heat under reflux on a water-bath for 20 minutes. Cool to room temperature. Determine the absorbance of the resulting solution at the maximum at about 840 nm using 10.0 ml of hydrazine- molybdate reagent as the blank. The absorbance of the test solution does not exceed the absorbance obtained by using 0.1 ml of arsenic standard solution (10 ppm As) in place of the test solution (0.1 ppm). 18

Non pharmacopoial tests for glass containers:

Non pharmacopoial tests for glass containers (1) Total height : tolerance 2 mm (2) Body diameter : tolerance 2 mm (3) Neck capacity : tolerance 2 mm (4) Overflow capacity : tolerance 2 ml 19




METAL CONTAINERS Select a sample of 50 tubes from the lot to be tested and clean each tube by vibration and/blowing. Fill the tubes with a suitable molten eye ointment base, close the open end of each tube by a double fold and allow the filled tubes to cool overnight at a temperature of 15º to 20º. A metal bacteriological filter with 4.25 cm filter paper of suitable porosity supported on suitable perforated plate H eat it above the melting range of the base. Remove the caps and apply uniform pressure to the closed end of each tube in turn, in such a manner that the time taken to express as much of the base as possible through each nozzle is not less than 20 sec. 21

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Collect the extruded base from the 50 tubes in the heated filter, applying suction . wash the walls of the filter and the filter paper with three successive quantities, each of 30ml, of chloroform, allow the filter paper to dry. Examine the filter paper under oblique lighting with the aid of magnifying glass with a graticule of 1 mm squares, one of which is sub-divided into 0.2 mm squares N ote (a) the number of all metal particles 1 mm in length and longer, (b) the number in the range 0.5 mm to less than 1 mm (c) the number in the range 0.2 mm to less than 0.5 mm. Carry out two further examinations & calculate the average number of metal particles 22

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Give each metal particle detected on the filter paper a score as follows and add the scores together: If total score is <100 comply If total score is >150 fail If score is 100-150 repeat Particles 1 mm and above 50 Particles 0.5 mm but less than 1 mm 10 Particles 0.2 mm but less than 0.5 mm 2 Particles less than 0.2 mm Nil 23

Plastic & Plastic containers:

Plastic & Plastic containers 24

Tests for Plastic & Plastic containers:

Tests for Plastic & Plastic containers Most widely used in pharma industries for aqueous parentral preparation. Container should be……… Withstand in sterilization condition Sterilize easily Resistance to enter microorganisms after closing Physically strong Transparent to provide visible observation of content. 25


PHARMACOPOEIAL TESTS :- Solution S :- Fill the container to its nominal capacity with water( R ) Close it ( with similar manner of closing or by aluminum sheet ) Heat in autoclave (Temperature 121 ° c for 30 min.) If deterioration of container at 121 ° c then heat at 100 ° c for 2 hr. Use this solution with in 4hr. 26

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Blank: - By heating water (R) in borosilicate flask cover with aluminum sheet at same temperature & time. Visual:- Appearance of the solution S must be clear and colorless . 27 Now by using blank and solution S, perform following tests

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Absorbance:- Absorbance of solution S at 230-360 nm should not more than 0.2 Oxydisable substances :- 20 ml solution S + 1 ml H 2 SO 4 + 20 ml 0.02M KMnO 4 Boil for 3 min. Cool and add 1gm potassium iodide & 0.25 ml starch as indicator Repeat operation for 20 ml blank Difference should not more than 1.5. 28

Resistance to centrifugation:-:

Resistance to centrifugation:- Acidify water with 2M HCl ↓ Fill the container with this water to its nominal capacity ↓ Envelope the container with absorbent paper impregnated with 5 fold dilution of bromophenol blue solution or any other indicator & dried ↓ Centrifuge at 5000 rpm for 10 min. ↓ No leakage should be detected on indicator paper 29


Leakage:- Place the container between two plates covered with absorbent paper impregnated with bromophenol blue solution or any other indicator ↓ Apply force to plate to press the container so that internal pressure of container reaches to 67 Kpa with in 10 min ↓ Should not any sign of leakage on indicator paper 30

Permeability to vapour:-:

Permeability to vapour:- Fill the container with 0.9% NaCl solution to its nominal capacity ↓ Weigh it & store at 4-6 ° c,45-55% relative humidity for 21 days ↓ At the end of period wt.loss should not more than 1% 31

Resistance to stress:-:

Resistance to stress:- Acidify water with 2M HCl ↓ Fill the container with this water to its nominal capacity ↓ Apply force to both end of container ↓ No break & deterioration occur. Resistance to temperature variation:- Place container in chamber having temp.20-23 ° c ↓ cool & rapidly maintain -80 ° c for 24 hr ↓ Raise temp.to 50 ° c & maintain it for 12 hr. ↓ cool at room temp. ↓ No break & deterioration occur 32

Test of pyrogen:-:

Test of pyrogen:- Rinse with WFI at 19-21 ° c then discard rinsing ↓ Fill container with 100 ml NaCl injection ↓ Close the container & heat in autoclave with 110 ° c for 30 min.(solution A) ↓ Take 10 ml solution B per kg body weight of rabbit ↓ Solution B complies with test of pyrogen 33

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Test of sterility:- Comply with sterility test as per IP/ BP. Transparency:- Fill the container with primary suspension to nominal capacity of container. ↓ The cloudiness of suspension should be perceptible when view through container. ↓ Dilution 1 in 200 for container made from polyethylene or polypropylene & 1 in 400 for other container. 34

Non pharmacopoeial tests:-:

Non pharmacopoeial tests:- Total Height Body diameter 35

Printed / Plain strip rolls of aluminum or plastic:

Printed / Plain strip rolls of aluminum or plastic 36

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Aluminum foil widely used for blister & strip packing Non pharmacopoeial tests:- Description:- Foil printed with …………. colours Dimension:- Text matter:- check 10 foil individually it must as per specification Cleanliness check Gram per square meter:- Cut square piece of 10 × 10 or 5 × 5 cm & weigh take 10 individual reading limit :-Not more than 50 gm per square meter 37

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38 Rubber closures

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When rubber closures come in contact with content it may absorb active ingredients,preservatives etc. So the quality of closures has to be control . PHARMACOPOEIAL TESTS:- Sample preparation:- wash the closures by agitation in 0.2% w/v solution of anionic surface active agents for 5 min.then rinse 5 time with water place number of washed closures (contain100 cm2 surface area) in suitable borosilicate glass container. 39

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Add 200 ml water per 100 cm 2 surface area of closures & weigh it Now,cover the mouth of container with aluminum foil & heat in autoclave & maintain temp.119°-123°c for 30min. Cool at room temp. for 30 min.& make up the original weight with water shake & immediately separate the solution from closures by decantation ( Solution A ) Dry the treated closure at 64°-66°c,at pressure not more than 0.7 Kpa for 24 hr. 40

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Prepared sample is used for the following tests : sterilization test : shall not become tacky or soften . Fragmentation test : The Test applicable to closure intended to be pierced by hypodermic needle. Result : count the number of fragments should not more than 10 except butyl rubber closures where total no of fragments should not more than 15. Aqueous preparations :place water in each of 12 vials, close vial allow to stand for 16 hour. volume is taken 4 minus. Carry out 4 times. Pass the liquid in the vial with nominal pore size 0.5 micro meter. For dry preparation same volume is taken for 12 vials. using hypodermic needle(0.8mm), inject 1 ml of water & remove same air.

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Clarity & color of aqueous extract : Not more opalescent & not more intensely colored than standard reference solution of IP. Heavy metal : 20 ml of solution complies with the limit test for heavy metals.

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Self sealability: Take vial fill with nominal volume of water Close the vial secure with cap Pierce the closure with needle 10 times at different sites Immerse the vial in 0.1W/V% solution of methylene blue at pressure of 27 Kpa Restore the normal atmospheric pressure and leave vials for 30 mins

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Light absorption Filter the test solution by 0.5 micron filter Measure abs. at 220 -360 nm Abs. NMT 2.0 44

Volatile sulphides:

Volatile sulphides Place closures cut if necessary, with a total surface area of 20±2 cm 2 in a 100 ml clonical flask + 50 ml of 2% W/V solution of citric acid. Place a piece of lead acetate paper over the mouth of flask + Heat in an autoclave for 30 min. Result : A black stain on paper is not more intance than that of standard prepared at same time in same manner using 0.154 mg of NaS & 50 ml of 2% W/V solution of citric acid.

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Oxydisable substances:- Carry out this test with in 4 hr of preparing of solution A Take 20ml solution A + 1ml 1M H2So4 + 20 ml 0.02M KMnO4 Boil for 3 min. Cool,add 1gm potassium iodide & 0.25 ml starch solution,added toward end point of titration,as indicator Repeat operation using 20 ml blank prepared in light absorption test Difference should not more than 7. 46

This type of tests are generally used for secondary packaging materials:

This type of tests are generally used for secondary packaging materials Like…… Paper board Wooden ply Etc…… 47 Transportation test

Transport packaging testing:

Transport packaging testing Transport packaging and their contents are influenced by the modes of transport. Depending on which transport mode that is used, packages will be exposed to different kind of stresses. The main stresses are; Mechanical Strains - The most common mechanical strains on transported goods are force stresses like, stacking pressure and shocks and energy stresses like vibration and dropping. Climatic Stresses - Climate plays a vital part for the durability and performance of the packaging during the transport. Testing Methods Packaging is tested in two ways; 1) regarding their material performance 2) how they perform during the actual transportation. 48

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Drop Test, ISO 2248 - The test simulates actual shocks by dropping the package and its content freely against a rigid plane surface from a predetermined height. For example, a drop test can be conducted so that the package hits the surface diagonally against one corner, as in the picture beside. 49

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The Compression and Stacking Tests, ISO 12048 and 2234 - This test is performed to assess the ability of a transport package to withstand compressive forces and to protect its contents during compression. The test may also be used as a stacking test to investigate the performance of i.e. the bottom package in a stack during storage in a warehouse. 50

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The Vibration Test, ISO 2247 and 8318 - Various forms of transportation vibrations can be simulated in a laboratory through a vibration test. The test-bench can be made to swing and vibrate in almost any direction with a number of frequencies and amplitudes to emulate the transportation being used. 51

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The Horizontal Impact Test, ISO 2244 - Horizontal shocks are simulated by applying a horizontal velocity to the test specimen and bringing it to halt by impact with a vertical impact surface. 52

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The Water-Spray Test, ISO 2875 - The test is designed so that each area of the top surface of the package is sprayed with water maintained at a constant temperature at a specified rate for a specified period. The test package shall be filled with its intended contents and closed normally, as if ready for distribution 53

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The Rolling and Toppling Test, ISO 2876 AND 8768 - In a rolling test the package is placed on a horizontal impact surface with the resting surface down. The package is tilted until the point of balance on this edge is reached. Then it is permitted to overbalance without thrust so as to impact on the surface. This procedure shall be repeated until all six sides have been impacted. 54

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Bending Test-EPU: 4/86:89 - the ability of the package to withstand compression is based on the bending strength and bending stiffness of the sheet material. Therefore this is a vital test to perform in order to get the best possible packaging. 55

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Moisture Absorption Test - In order to determine the plywood box’s capability to protect the goods from moisture and to establish how moisture resistant the actual box will be a moisture absorption test is performed on the different batches of plywood used. 56

Bye Bye Thought:

Bye Bye Thought To secure the quality of product from external environment , protector must be also quality bonded And the same way………… “Quality of a person is highly dependent on the quality of surrounding people.” 57


REFERENCE Indian Pharmacopoeia, 2007, Government of Indian ministry of health and family welfare, The Indian Pharmacopoeia commission, Ghaziabad,volume-1, 6.1, 6.2, 6.3, 599-609. .Carter S.J., “Packaging”; Cooper & Gunn’s Tutorial Pharmacy, sixth edition, CBS publicashers & distributors, New Delhi, 2005, 133-136 & 139-140 www.nefab.com 58

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59 Thank you

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