PRAC PRACTI TIC CAL NOT NOTE EBOOK BOOK INDUSTRIAL PHARMACY
COURSE NAME: INDUSTRIAL LAB
COURSE NO: PCU 610
SEMESTER: 8th PROGRAM:
PHARM-D
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PRAC PRACTI TIC CAL NOT NOTE EBOOK BOOK INDUSTRIAL PHARMACY
TABLE TABLE OF CONTENTS LIST OF PRACTICAL PERFORMED Cours: I!"ustr#$% Ph$r&$'( L$)or$tor(
Cours No* PCU-610
Cours I!'h$r+: Mr* H$roo! R$h#&
L$)or$tor(: T T'h!o 'h!o L$)
S* NO 1*
TITLE OF PRACTICAL PERFORMED
Preparation Of Starch Paste
,*
To Determine Determine The Angle of Repose of Given Sample
*
Preparation of Simple (White) Ointment
.*
Preparation of Sulphur Ointment
/*
Preparation of Cold Cream (WO !mulsion)
6*
Preparation of Paracetamol Granules
*
To determine determine moisture contents in Given Sample
8*
Preparation of Paracetamol Ta"lets
*
Weight We ight #ariation #ariation Test Test $or $o r Ta"lets
10* 11* 11*
$ria"ilit% Test $or Ta"lets To determine the Thic&ness of Ta"lets
1,*
To determine the Diameter of Ta"lets
1*
'ardness Test $or Ta"lets
1.*
Disintegration Test $or ncoated Ta"lets
1/*
Disintegration Test $or $ilm coated Ta"lets
PRACTICAL NO* 1 PREPARATION OF STARCH PASTE 2 | P a g e
PRACTICAL NOTEBOOK INDUSTRIAL PHARMACY THEOR2:
Starch is a car"oh%drate consisting of a large num"er of glucose units oined "% gl%cosidic "onds* This pol%saccharide is produced "% most green plants as an energ% store* +t is the most common car"oh%drate in human diets and is contained in large amounts in such staple food as potatoes, -heat, mai.e (corn) rice cassava* Pure starch is -hite, tasteless and odorless po-der that is insolu"le in cold -ater or alcohol* +t consists of t-o t%pes of molecules, the linear and helical am%lase and the "ranched am%lopectin* Depending on plant, starch generall% contains /01 to /21 am%lase and 321 to 401 am%lopectin "% -eight* RE3UIREMENTS:
Starch, Purified Water, Weighing 5alance, Stirrer, 5ea&ers FORMULA USED:
Starch666666666 3*0 gm Cold purified -ater666666 3*0 ml 'ot purified -ater6666666 20*0 ml PROCEDURE:
7* Weigh starch 03 gm "% -eighing "alance* /* Ta&e 03 ml of cold -ater* 8* Suspend mai.ecorn starch in pure -ater -ith continues stirring till smooth slurr% is o"tained* 9* Ta&e 20 ml of pure -ater in another "ea&er and heat it to "oil* 2* Add the slurr% to the "oiling -ater -ith stirring and maintaining heat for some time* :* Remove the heat and cool the starch paste 90;C -ith stirrer* USES:
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PRACTICAL NOTEBOOK INDUSTRIAL PHARMACY As ta"lets "inder* !mplo%ed in granulation of po-der*
PRECAUTIONS: Do not store the paste for prolong time as the chances of micro"ial gro-th* Do not store it in refrigerator*
PRACTICAL NO* , 4 | P a g e
PRACTICAL NOTEBOOK INDUSTRIAL PHARMACY TO DETRMINE THE ANGLE OF REPOSE OF GI4EN SAMPLE THEOR2: A!+% o5 Ros: The angle of repose is the ma
friction, cohesion and the shapes of the particles* When "ul& granular materials are poured onto a hori.ontal surface, a conical pile -ill form* The internal angle "et-een the surface of the pile and the hori.ontal surface is &no-n as the angle of repose and is related to the densit%, surface area, and coefficient of friction of the material*
F%o7 rort(
A!+% o5 ros "+rs9
!
/2 = 80
Good
87 = 82
$air6aid not needed
8: = 90
Passa"le = ma% hang up
97 = 92
Poor = must agitate,
9: = 22
vi"rate #er% poor
2: = :2
#er%, ver% poor
>::
RE3UIREMENTS: $unnel, Sample, Weighing "alance, Clamp, Calculator 5 | P a g e
PRACTICAL NOTEBOOK INDUSTRIAL PHARMACY PROCEDURE: Angle of repose -as determined using funnel method* $unnel is adusted -ith the help of clamp to the stand and height of the funnel -as adusted in such a -a% that the tip of the funnel ust touches the heap of the "lends* The angle of repose is the angle formed "% the hori.ontal "ase of the "ench surface and the edge of a cone6li&e pile of granules* $unnel used -as a stainless steel funnel and the si.e of the orifice -as 70 mm and the height from the "eginning of funnel to end of orifice -as 777 mm* The funnel -as fi
PRACTICAL NO* 6 | P a g e
PRACTICAL NOTEBOOK INDUSTRIAL PHARMACY
PREPARATION OF SIMPLE HITE9 OINTMENT FORMULA USED: • • • •
Wool $at 666666666666666666666666666 2 grams 'ard Paraffin 666666666666666666666 2 grams Cetoster%l Alcohol 666666666666666 2 grams White Soft Paraffin 66666666666666 42 grams
PROCEDURE:
7* /* 8* 9*
Weighed accuratel% all the ingredients using a digital "alance* i< all the ingredients in a "ea&er* 'eat gentl% -ith constant stirring until a homogenous mi
PRECAUTIONS: $or !
USES: Simple ointment is use as Emollient. +t is used as base for medicated ointments*
PRACTICAL NO* . PREPARATION OF SULPHUR OINTMENT 7 | P a g e
PRACTICAL NOTEBOOK INDUSTRIAL PHARMACY FORMULA USED: • • •
Sulphur 666666666666666666666666666 70 grams ineral oil 666666666666666666666666 70 grams White Ointment 66666666666666666 40 grams
PROCEDURE:
7* /* 8*
Weight accuratel% all the ingredients using a digital "alance* i< Sulphur -ith mineral oil to form paste* Add the paste to -hite ointment and mi< until homogenous mi
PRECAUTIONS: $or !
+t should "e stored in -ell closed container* se -ithin one month*
USES OF SULPHUR OINTMENT:
+t is use for fungal infections. +t is used for skin infections li&e dermatitis, scabies and eczema*
PRACTICAL NO* / PREPARATION OF COLD CREAM ;O9 8 | P a g e
PRACTICAL NOTEBOOK INDUSTRIAL PHARMACY THEOR2: Cold cream is a WO t%pe of emulsion* INGREDIENTS: • • • •
M$str For&u%$
For&u%$ us"
ineral Oil 6666666666666666666666 200 parts 666666666666666666 20 grams 5ees Wa< 666666666666666666666666 790 parts 666666666666666666 3 grams Sodium 5ora< 6666666666666666666 32 parts 6666666666666666666 83*2 grams Purified Water 666666666666666666 82*8 parts 66666666666666666 73*:2 grams
PROCEDURE:
7* /* 8* 9*
Weighed all the ingredients accuratel% using a digital "alance* Com"ine the mineral oil and "ees -a< in a "ea&er* 'eat it at 30BC and stir the mi
a"sor"ed in the -ater* 2* o- put the "ora< solution slo-l% into the "ees-a< mi
USES OF COLD CREAM:
Cold Cream is use as Emollient. +t is used as base for medicated creams*
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PRACTICAL NOTEBOOK INDUSTRIAL PHARMACY
PRACTICAL NO* 6 PREPARATION OF PARACETAMOL GRANULES THEOR2: 10 | P a g e
PRACTICAL NOTEBOOK INDUSTRIAL PHARMACY t Gr$!u%$t#o!:
The Steps Involve in wet granulation are: 1 !eighing 2 "i#ing 3 $ranulation 4 S%reening The &a'p "ass 5 &r(ing RE3UIREMENTS:
Weighing "alance, esh, ortar, Oven, Paracetamol, Diluent, agnesium stearate* FORMUAL USED:
7* /* 8* 9*
Paracetamol (AP+)66666666/20 mg P#P80 (5inder)666 701 -Eactose (Diluent)6666(F*S) agnesium Stearate (Eu"ricant) 666666666608 mg
PROCEDURE:
The active ingredients of Paracetamol, diluents and disintegrants -ere mi
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PRACTICAL NOTEBOOK INDUSTRIAL PHARMACY
PRACTICAL NO* TO DETERMINE MOISTURE CONTENTS IN GI4EN SAMPLE PROCEDURE: 1* S-itch OH the mains* 12 | P a g e
PRACTICAL NOTEBOOK INDUSTRIAL PHARMACY ,* Open the lid cover and put sample on the pan* * Spread the sample on the pan evenl% -ith the help of spatula* .* When -eight is more than 200 mg the instrument s%m"olicall% sho-s that it is read% for heating*
/* Close the lid cover* 6* +nstrument -ill start heating "% itself* * When the material start dr%ing, displa% unit -ill sho- automaticall% loss in -eight in 1age*
8* When dr%ing is over the result is displa%ed in 1age on displa% unit, note the reading* * Remove the pan and clean it* 10* S-itch O$$H the instrument -hen not in use*
PRACTICAL NO* 8 13 | P a g e
PRACTICAL NOTEBOOK INDUSTRIAL PHARMACY PREPARATION OF PARACETAMOL TABLETS B2 ET GRANUATION METHOD 1* P$r$'t$&o% API9 ,* A<#'% D#%u!t9
,/0 &+ 3*S
* St$r'h B#!"r9
10= ;9
.* Aros#% D#s#!t+r$!t9
= ;9
/* M$+!s#u& st$r$t Lu)r#'$!t9 6* $tr
1 to 1*/ = ;9 3*S
The steps involved in -et granulation -ere, Weighing, i
Starch -as ta&en in a "ea&er in /0 ml of hot -ater -as added and stirred -ell to ma&e suspension and heated in a "oiling -ater "ath -ith continues stirring until to translucent paste is formed* The active ingredients of paracetamol, diluents and disintegrants are mi
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PRACTICAL NOTEBOOK INDUSTRIAL PHARMACY The -et granulation is forced through a 7: mesh screen* The moist materials are placed on large sheets of paper on shallo- -ire tra%s and placed in dr%ing ca"inets -ith a circulating air current in thermostatic heat control* Particle si.e distri"ution can "e controlled "% var%ing the speed of rotation and dr%ing temperature* After dr%ing the granulation is reduced the particle si.e "% passing it through a smaller mesh screen* After dr%ing granulation the lu"ricants is such as agnesium Stearate -as added* Then the lu"ricated -ere compressed "% using the single punch machine* RESULT:
After passing through mesh o*7: and Dr%ing -e o"tained $ine granules of paracetamol for ta"leting*
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PRACTICAL NOTEBOOK INDUSTRIAL PHARMACY
PRACTICAL NO* EIGHT 4ARIATION TEST FOR TABLETS
THEOR2:
Weight variation or uniformit% of -eight is an official test in all current pharmacopoeias* Weight variation test is one of the +n6Process tests during production of ta"lets in an% pharmaceutical industr%* An% variation in -eight of ta"lets ultimatel% leads to variation in doses* RE3UIREMENTS:
Ta"lets
Anal%tical "alance
PROCEDURE:
7* /* 8* 9* 2*
Select 70 ta"lets randoml% and -eighed them all using a digital "alance* Determine the average -eight of ta"lets* o- each ta"let is -eighed individuall% (prescri"es limits alread% calculated) ot more than t-o ta"lets should "e deviated from the allo-ed limits* one of the ta"lets should deviate from t-ice the percentage limits*
USP #+ht <$r#$t#o! To%r$!'s 5or U!'o$t" T$)%ts S* No
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A<r$+ 7t* o5 t$)%t&+9
M$>* = "#55r!' $%%o7"
PRACTICAL NOTEBOOK INDUSTRIAL PHARMACY 7
780 or Eess
701
/
78068/9
3*21
8
ore than 8/9
21
B*P Br#t#sh Ph$r&$'o#$9 #+ht <$r#$t#o! To%r$!'s 5or U!'o$t" T$)%ts A<r$+ 7#+ht o5 t$)%t
D<#$t#o! $%%o7" 5ro& $<r$+ 7#+ht
>9
40 or J40 mg
701
406/20 mg
3*21
>/20mg
21
PRACTICAL NO* 10 FRIABILIT2 TEST FOR TABLETS OFFICIAL TEST9 17 | P a g e
PRACTICAL NOTEBOOK INDUSTRIAL PHARMACY THEOR2: +t is ph%sical parameter -hich indicates resistance of ta"lets against mechanical shoc& during pac&aging, transport or stripping*
RE3UIREMENTS:
$ria"ilator, Anal%tical "alance, Ta"lets ? Calculator PROCEDURE: 7* /* 8* 9* 2* :* 3*
$or ta"lets having -eight eIual or less than :20mg, ta&e sample of /0 ta"lets* $or ta"lets having -eight more than :20mg, ta&e sample of 70 ta"lets* De6dust the ta"lets -ith addition of air pressure or soft "rush* Accuratel% -eighed the ta"lets and placed in the drum of the $ria"ilator* Operate the $ria"ilator for 9 minutes at /2 rpm to complete 700 rotations* Collect, de6dust and -eighed the ta"lets again* The percentage fria"ilit% can "e determined "% using follo-ing formulaK 1 age $ria"ilit% @ W7 = W/ W7 Where, W7 @ initial -eight and W/ @ final -eight
L#&#ts:
*S*P @ not more than 71 5*P @
not more than 0*41*
PRACTICAL NO* 11 TO DETERMINE THIC@NESS OF TABLETS THEOR2:
Ta"let thic&ness is an important Iualit% control test for ta"let pac&aging* The thic&ness of ta"let can affect the therapeutic effectiveness of ta"lets* #er% thic& ta"let affects pac&aging either in 18 | P a g e
PRACTICAL NOTEBOOK INDUSTRIAL PHARMACY "lister or plastic container* Ta"let thic&ness is determined "% the die of the ta"leting machine and is generall% controlled to minimi.e appearance pro"lems* Thic&ness is an u!o55#'#$% tst*
+t can "e dimensionall% descri"ed L controlled* The thic&ness of a ta"let is onl% varia"le* Ta"let thic&ness can "e measured "% #ernier caliper or "% other device* Ta"let thic&ness should "e controlled -ithin a M21 variation of standard value as per *S*P specifications* Thic&ness of the ta"let is inversel% proportional to hardness i*e* increase in hardness
decrease the thic&ness L vice versa* Thic&ness of ta"let is measured "% #ernier caliper Digital tester* +t is determined for 70 ta"lets*
RE3UIREMENTS:
Ta"lets, #ernier caliper or Digital Tester
PROCEDURE: 1* Turn on the +nstrument* 70 ta"lets are selected and then the test for thic&ness is
carried out "% using the Digital Ta"let Testing +nstrument 'T60:03 "% clic&ing ode "utton and adusting operating mode to thic&ness* Turn O the hardness tester and set ,* * .* /*
its mode to the specifications as reIuired* Place the ta"let "et-een its a-s and start the apparatus* The a-s -ill appl% force on the ta"let till it "rea&s* The force -ill "e displa%ed on the screen of tester, note that value along -ith its unit* Repeat the same procedure for 70 ta"lets and note their readings and then average -as calculated*
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PRACTICAL NOTEBOOK INDUSTRIAL PHARMACY
PRACTICAL NO* 1, TO DETERMINE DIAMETER OF TABLETS THEOR2: RE3UIREMENTS: 1* Turn on the +nstrument 'T60:03* 70 ta"lets are selected and then the test for diameter
is carried out "% using the Digital Ta"let Testing +nstrument 'T60:03 "% clic&ing ode "utton and adusting operating mode to diameter* ,* Place the ta"let "et-een its a-s and start the apparatus* * The diameter -ill displa%ed on screen of tester, note that value along -ith its unit* .* Repeat the same procedure for 70 ta"lets and note their readings and then average -as calculated* 20 | P a g e
PRACTICAL NOTEBOOK INDUSTRIAL PHARMACY
PRACTICAL NO* 1 HARDNESS TEST FOR TABLETS (O6O$$+C+AE Test)
THEOR2: H$r"!ss 'rush#!+ str!+th9: +t is the load reIuired to crush the ta"let -hen placed on its edge* H$r"!ss #s &$sur": To determine the need for pressure adustments on the ta"leting machine*
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PRACTICAL NOTEBOOK INDUSTRIAL PHARMACY
'ardness can affect the disintegration* So if the ta"let is too hard, it ma% not disintegrate in the reIuired period of time* And if the ta"let is too soft, it -ill not -ithstand the handling during su"seIuent processing such as coating or pac&aging*
+n general, if the ta"let hardness is too high, -e first chec& its disintegration "efore
reecting the "atch* +f the disintegration is -ithin limit, -e accept the "atch*
+f 'ardness is high N disintegration is -ithin a time accept the "atch*
F$'tors A55't#!+ th H$r"!ss: •
Compression of the ta"let and compressive force*
•
Amount of "inder (ore "inder more hardness)*
•
ethod of granulation in preparing the ta"let (-et method gives more hardness than direct method, Slugging method gives the "est hardness)*
LIMITS: 2 &ilograms minimum and 70 &ilograms ma
a&e hardness test on 2 ta"lets and then ta&e the average hardness*
RE3UIREMENTS:
Sample 6666 70 ta"lets 'ardness tester (Digital 'ardness Tester) PROCEDURE: 7* /* 8* 9* 2*
Turn O the hardness tester and set its mode to the specifications as reIuired* Place the ta"let "et-een its a-s and start the apparatus* The a-s -ill appl% force on the ta"let till it "rea&s* The force -ill "e displa%ed on the screen of tester, note that value along -ith its unit* Repeat the same procedure for 70 ta"lets and note their readings*
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PRACTICAL NOTEBOOK INDUSTRIAL PHARMACY NORMAL LIMITS: inimum limit 6666666666 2 &g a
PRACTICAL NO* 1. DISINTEGRATION TEST FOR UNCAOTED TABLETS THEOR2: +t is the time reIuired for the ta"let to "rea& into particles, the disintegration test is a measure onl% of the time reIuired under a given set of conditions for a group of ta"lets to disintegrate into particles* Disintegration test is an official test* +t is performed to identif% the disintegration of ta"let in particular time period* Disintegration test is not performed for controlled L sustained release ta"lets* 23 | P a g e
PRACTICAL NOTEBOOK INDUSTRIAL PHARMACY APPARATUS USED:
Disintegration apparatus consists of 5as&et rac& assem"l% supporting si< c%lindrical glass tu"es* The assem"l% is attached -ith a device for lo-ering and raising the assem"l% in the medium placed in a c%lindrical vessel having 7000 ml capacit%* This -hole apparatus is placed in a -ater "ath for maintaining the desired temperature o f 83BC M 7 BC* RE3UIREMENTS:
Sample 6666666 : ta"lets
Disintegration apparatus
PROCEDURE:
7* Turn O the apparatus and maintain the temperature at 83BC M 7 BC* /* Remove the 5as&et6rac& assem"l% from the -ater* 8* Select si< ta"lets randoml% from the sample and place one in each of the tu"es of the 5as&et6rac& assem"l%* 9* o- reset the assem"l% in the apparatus and set the machine in motion* 2* ote the disintegration time and compared it -ith that of prescri"e time* The ta"lets must disintegrate -ithin the prescri"ed time* :* Repeat the same procedure for coated and effervescent tablets. According to the test the ta"let must disintegrate and all particles must pass through the 70 mesh screen in the time specified* +f an% residue remains, it must have a soft mass* Liquids used in disintegration Water, Simulated gastric fluid (p' @ 7*/ 'Cl), or
Simulated intestinal fluid (p' @ 3*2, '/PO9 (phosphate "uffer) N pancreatic en.%me N aO')* U*S*P* &tho" 5or u!'o$t" t$)%ts:
Start the disintegration test on : ta"lets* +f one or t-o ta"lets from the : ta"lets fail disintegrate completel% -ithin 80min repeat the same test on another 7/ ta"let* (i*e* the -hole test -ill consume 74 ta"lets)* 24 | P a g e
PRACTICAL NOTEBOOK INDUSTRIAL PHARMACY ot less than 7: ta"lets disintegrate completel% -ithin the time if more than t-o ta"lets (from the 74) fail to disintegrate, the "atch must "e reected*
TABLETS Solu"le ta"lets ncoated ta"lets $ilm coated ta"lets Sugar coated ta"lets !nteric coated ta"lets
DISINTEGRATION TIME 8 minutes 8672 minutes 80 minutes 7 hour /68 hours
PRACTICAL NO* 1/ DISINTEGRATION TEST FOR FILM CAOTED TABLETS RE3UIREMENTS:
Ta"lets, Water, Disintegration Test Apparatus* PROCEDURE:
Start the disintegration test apparatus on : ta"lets*
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PRACTICAL NOTEBOOK INDUSTRIAL PHARMACY +f one or t-o ta"lets from the : ta"lets fail disintegrate completel% -ithin 80 min repeat the same test on another 7/ ta"let* (i*e* the -hole test -ill consume 74 ta"lets)* ot less than 7: ta"lets disintegrate completel% -ithin the time, if more than t-o ta"lets (from the 74) fail to disintegrate, the "atch must "e reected*
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