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In process Quality Control, IPQC tests are mostly performed within the production
area.
They should not carry any risk for the quality of product.
In process testing enables easier identification of problems. It sometime identifies
a defective product batch that can be corrected by rework, whereas once that batch
has been completed, this may not be possible.
Failure to meet in process control specification indicates either that procedure were
not followed or some factor (S) out of control.
Disintegration apparatus
Dissolution apparatus
U.V Spectroscopy
Abbe Refractometer
T.L.C. kit
Official Tests
[1] Weight variation
[2] Disintegration
[3] Dissolution
Non-Official Tests
[1] Hardness
[2] Friability
Limit:
IP STANDARDS
Sr. No Average wt. of tablet(mg) Max. % difference allowed
1 84 or Less 10%
2 84-250 7.5%
3 More than 250 5%
of the 10 tablets must contain not less than 85 % and not more than 115 % of the labeled
drug content and the 10th tablet may not contain less than 75 % and more than125 % of the
labeled content. If these conditions are not met, remaining 20 tablet assayed individually
Water,
Simulated gastric fluid (pH = 1.2 HCl), or Simulated intestinal fluid (pH = 7.5,
KH2PO4 (phosphate buffer) + pancreatic enzyme + NaOH)
To remove or dissolve the coat, immerse the tablet in distilled water for 5min.
Put the tablet in the apparatus in water or HCL for 30 min at 37oC (according to the
U.S.P). If not disintegrated, put in intestinal fluid.
If one or two tablets fail to disintegrate, repeat on 12 tablets. So 16 tablets from the
18 must completely disintegrate within the time, if two or more not disintegrated
the batch is rejected.
Mechanism of Dissolution
Dissolution is a mass transfer process.
Sink condition The concentration of receptor compartment is maintain lower
level as compared to Donor compartment is known as sink condition.
Non sink condition The concentration of receptor compartment is not
maintain at lower level as compared to donor compartment.
USP apparatus
1. Apparatus 1 (rotating basket)
2. Apparatus 2 (paddle assembly)
3. Apparatus 3 (reciprocating cylinder)
4. Apparatus 4 (flow-through cell)
5. Apparatus 5 (paddle over disk)
6. Apparatus 6 (cylinder)
7. Apparatus 7 (reciprocating holder)
Procedure: The tablet was added into cylindrical vessel containing 1000 ml dissolution
media having rpm 75 and tem.370.5C. Dissolution of tablet was conducted 30 min,
in 5 min. of interval, after 5 min 5 mL sample was removed and appropriate quantity
of sample take absorbance by using U.V. spectroscopy technique and determine rate of
dissolution of tablet.
Procedure - The tablet was added into cylindrical vessel containing 1000 ml PH 1.2 Acidic
media having rpm 75 for next two hours and tem. 370.5C. Dissolution media was
changes tablet was added in to PH 6.8 Phosphate buffer for next five hour for 1 hr. of
interval. After 1 hr. 5 mL sample was removed and appropriate quantity of sample take
absorbance by using U.V. spectroscopy technique and determine rate of dissolution of
tablet.
Capsule
1. Dissolution apparatus Type 2 (USP)
2. Temperature - 370.5C
3. Time 5 hrs.
4. Media PH 1.2 Acidic Buffer, PH 6.8 Phosphate buffer.
5. Rpm 75 100.
6. Volume 900 ml.
Procedure - The Capsule was added into cylindrical vessel containing 1000 ml PH 1.2
Acidic media having rpm 75 for next two hours and tem. 370.5C. Dissolution media was
changes Capsule was added in to PH 6.8 Phosphate buffer for next three hour for 1 hr. of
interval. After 1 hr. 5 mL sample was removed and appropriate quantity of sample take
absorbance by using U.V. spectroscopy technique and determine rate of dissolution of
Capsule.
Procedure The Suppository was added into cylindrical vessel containing 1000 ml
dissolution media (PH 7.4 Phosphate buffer) having rpm 75 and tem.370.5C. Dissolution
of Suppository was conducted 60 min, in 10 min. of interval, after 10 min 5 ml sample was
removed and appropriate quantity of sample take absorbance by using U.V. spectroscopy
technique and determine rate of dissolution of Suppositories.
5. Hardness
Tablet requires a certain amount of strength or hardness and resistance to friability to
withstand mechanical shocks of handling in manufacture, packaging and shipping.
Hardness generally measures the tablet crushing strength.
Importance
To determine the need for pressure adjustments on the tableting machine.
Hardness can affect the disintegration.
So if the tablet is too hard, it may not disintegrate in the required period of time.
And if the tablet is too soft, it will not withstand the handling during subsequent
processing such as coating or packaging.
In general, if the tablet hardness is too high, we first check its disintegration before
rejecting the batch.
If the disintegration is within limit, we accept the batch.
IPQC Sagar Kishor Savale
If Hardness is high + disintegration is within a time accept the batch.
Limits
5 kilograms minimum and 8 kilograms maximum.
Make hardness test on 5 tablets and then take the average hardness.
Friability apparatus
Density
Density may influence compressibility, tablet porosity & dissolution.
Dense hard granules may require higher load to produce cohesive compact to
reduce free granules seen on the surface of tablets.
Compressibility DT, Dissolution, if DT is slower dissolution is indirectly
hampered.
Dense granules have less friability but cause a problem in releasing the drug.
Three Methods to determine density
Bulk Density
Bulk density is given by equation,
b = M / V b
Where,
b- bulk density of granules,
M is mass of granules in gm,
Vb volume of granules in measuring cylinder in ml.
More compressible bed of particulate - less flowable powder or granules.
If less dense/compressible - more flowable powder or granules.
True/tapped density
Tapped/true density is given by equation,
t = M / Vb
Where,
Hausner's Ratio
Hausners ratio was related to interparticulate friction and as such could be
used to predict powder flow characteristics.
It showed that powder with low particular friction such as coarse sphere had ratio
of approximately 1.2, whereas more as cohesiveness- less free flowing powders
such as flaks have Hausners ratio greater than 1.6.
Formula
Compressibility Index
It is directly related to the relative flow rate cohesiveness & particle size.
It is simple fast & popular method of presiding powder flow characters.
It can be obtained from bulk density measurements is the % Compressibility index (C).
% Compressibility index = Tapped density - Bulk density / Tapped density X 100.
OR
I = (1 V/ Vo) x 100
Where,
I % Compressibility index,
V Volume occupied by powder/ granules after tapping, Vo - volume of powder/granules
before tapping
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