sop. validation. r2

7/25/2019 SOP. Validation. R2

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Standard Operating Procedure

PROCEDURE FOR CONCURRENT PROCESS VALIDATION

SOP NO. Dated Effective Reviion PageQD-3-PD-000 01 11

Rep!ace DatedAll previous SOPs in this context -

PREPARED"# C$EC%ED"# REVIE&ED"# APPROVED"#

A'(at A!i)PD

A*(ad S*e*r+arS)PD

&aee( S*a(iS),C

Dr. A-(a! NairEDT

Circu!ationEDT, EDQO, SM (PD, SM (Q! !M (Pro"uction

./ PURPOSETo "e#ine $n" "ocu%ent $ proce"ure #or !oncurrent Process &$li"$tion'

0./ SCOPEThis proce"ure is $pplic$le to concurrent process v$li"$tion o# ne) or revise" %$nu#$cturin*processes o# ph$r%$ceutic$l pro"uct'

1. / RESPONSI"ILITES

The "ele*$tion o# responsiilities re*$r"in* the concurrent process v$li"$tion $ctivit+ is *iven $s#ollo)s

PRODUCT DEVELOP)ENT

Prep$r$tion o# the v$li"$tion protocol $ccor"in* to the M. ($tch M$nu#$cturin* .ecor"

!o%%unic$tion )ith $ll the "ep$rt%ents involve" in the execution o# the v$li"$tion protocol

M$nu#$cturin* o# the $tches to e v$li"$te" /ointl+ )ith the Pro"uction te$%

.ecor"s *ener$tion, co%pil$tion o# "$t$ $n" prep$r$tion the v$li"$tion report

!ircul$tion o# the v$li"$tion report to $ll the concerne" "ep$rt%ent $n" personnel #or $pprov$l

PRODUCTION

Assist in the "evelop%ent o# v$li"$tion protocol

!hec $n" revie) the v$li"$tion protocol

M$nu#$cturin* o# the $tches to e v$li"$te" $n" #ollo)in* the controls "escrie" in the

protocol /ointl+ )ith Pro"uct Develop%ent Te$%

,UALIT# CONTROL AND )DV

Assist in the "evelop%ent o# the v$li"$tion protocol


Provi"in* $n$l+tic$l support + testin* the v$li"$tion $tches

!o%%unic$te the results to the Pro"uct Develop%ent Dep$rt%ent $#ter testin*

!$rr+ out the st$ilit+ stu"+ )ith the pro"ucts ot$ine" #ro% the v$li"$tion $tches $s per SOP

NO. QD-9-0018

IPC

Assist in the "evelop%ent o# the v$li"$tion protocol

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Over $ll %$n$*e%ent o# the in process control $n" checs "urin* the %$nu#$cturin* o# the

v$li"$tion $tches

EDT

Approves the v$li"$tion protocol

Approves the v$li"$tion report #or circul$tion

ED,O

Authorie the v$li"$tion protocol

Approves the v$li"$tion report #or circul$tion

2./ PROCEDURE

2. PREPARATION AND E3ECUTION OF T$E CONCURRENT VALIDATION PROTOCOLThe %$in contents o# the !oncurrent &$li"$tion Protocol $re2

Pro/ect "escription

Title p$*e

T$le o# contents

Protocol "escription

Approv$ls

Distriution list

.esponsiilities

- &$li"$tion te$%

- Execution te$%

&$li"$tion Protocol

ntro"uction

Purpose

Scope

Accept$nce criteri$

&$li"$tion $tches

4ist o# e5uip%ents $n" $re$s o# %$nu#$cturin*

6or%ul$tion "et$ils

M$nu#$cturin* process #lo) ch$rt

n process controls $n" checs )ith

- Accept$nce criteri$

- 6re5uenc+

- Environ%ent$l controls

Processes v$li"$tion

7r$nul$tion- Processin* step

- Purpose

- Tests

- S$%plin* pl$n


!o%pression

- Processin* step

- Purpose

- Tests

-S$%plin* pl$n

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!o$tin*

- Processin* step

- Purpose

- Tests

-

S$%plin* pl$n- Accept$nce criteri$

Det$il o# e$ch step o# the v$li"$tion protocol is *iven in the procee"in* sections' A speci%en

protocol is $lso $tt$che" #or re#erence'

6or li5ui" pro"ucts, v$li"$tion o# $ll the critic$l steps )ill e c$rrie" in the s$%e %$nner $s

"escrie" $ove'

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A. INTRODUCTIONThe intro"uction covers the #ollo)in* points

Pro"uct

Ph$r%$colo*ic$l cl$ssi#ic$tion

n"ic$tion

M$nu#$cturin* histor+ (i# re5uire"

8usti#ic$tion #or v$li"$tion

St$ilit+ re5uire%ents ($s per SOP

&$li"$tion re5uire%ent ($s per SOP

". PURPOSE!oncurrent Process &$li"$tion o# the %$nu#$cturin* process is con"ucte" to ensure th$tthe *iven %$nu#$cturin* process is suit$le to %$nu#$cture the Ph$r%$ceutic$l Pro"uct'

C. SCOPEThis protocol covers $ll the oper$tions involve" in %$nu#$cturin* o# three consecutiveco%%erci$l $tches o# $ ph$r%$ceutic$l pro"uct, #ro% receivin* o# the r$) %$teri$ls to the$chieve%ent o# the ul Ph$r%$ceutic$l Pro"uct'

The #inishe" pro"ucts ot$ine" #ro% the v$li"$te" $tches $re su/ecte" to St$ilit+stu"ies'

D. ACCEPTANCE CRITEIASt$*e )ise suit$ilit+ re5uire%ent or $ccept$nce criteri$ $re %entione" un"er this he$"in*'6or ex$%ple2

7r$nul$tion 9 The *r$nul$tion %ust co%pl+ )ith the :;4 content uni#or%it+

speci#ic$tions

!o%pression 9 The t$lets %ust co%pl+ )ith the :;4 speci#ic$tion #or co%pression o#

th$t p$rticul$r pro"uct

!o$tin* 9 The co$te" t$lets %ust co%pl+ )ith the :;4 speci#ic$tion #or co$tin* o# th$t

p$rticul$r pro"uct .SD (.el$tive St$n"$r" Devi$tion li%its #or these processes $re

- .e$"il+ p$ss$le - M$r*in$ll+ p$ss$le

E. VALIDATION "ATC$ES

The #ollo)in* "et$ils re*$r"in* the three v$li"$tion $tches %ust e provi"e"

$tch nu%er

M$nu#$cturin* "$te

Expir+ "$te

Shel# li#e

$tch sie

F. LIST OF E,UIP)ENTS AND AREAS OF )ANUFACTRUIN4

The list consist o# the #ollo)in* in#or%$tion

E5uip%ent@ Are$

;u%er (Asset

Qu$li#ic$tion nu%er

4. FOR)ULATION DETAILS

Mention the #ollo)in* "et$il re*$r"in* the #or%ul$tion2

!o%ponent

M$teri$l co"e

Q! speci#ic$tion nu%er

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M$nu#$cturer

6unction

Percent$*e in the #or%ul$tion

%* per t$let

* per $tch

$. )ANUFACTURIN4 PROCESS FLO& C$ART The ch$rt sho)s the "i$*r$%%$tic over vie) o# the %$nu#$cturin* process'

I. IN PROCESS CONTROL AND C$EC%S &IT$ ACCEPTANCE CRITERIA ANDFRE,UENC#$' The v$rious control p$r$%eters $n" their speci#ic$tions $re "e#ine" $t e$ch section in the

experi%ent$l pl$n' n or"er to consi"er the process v$li"$te", the v$li"$tion $tches %ust co%pl+ )ith e$ch

$n" ever+ speci#ic$tion inclu"e" in the experi%ent$l pl$nc' An+ "$t$ outsi"e speci#ic$tions %ust e stu"ie" in"ivi"u$ll+ $n" recor"e" in the #in$l

report"' Environ%ent$l control shoul" $lso e %onitore" especi$ll+ in c$se o# sensitive pro"ucts

e'*' te%per$ture $n" hu%i"it+

5. PROCESSES TO "E VALIDATED An+ critic$l process or step th$t %$+ $##ect the 5u$lit+ o# the #in$l pro"uct %ust e v$li"$te"'

6or ex$%ple, #in$l %ixin*@luric$tion o# the *r$nul$te, o##ici$l $n" uno##ici$l t$lettin*p$r$%eters, co$tin* process p$r$%eters etc'

7r$nul$tion

!o%pression

!o$tin*

Other (#or other "os$*e #or%s

%. SA)PLIN4 PLAN A step)ise s$%plin* pl$n shoul" e "esi*ne" $n" i%ple%ente" in or"er to ensure reli$ilit+

in the v$li"$tion proce"ure' The %$in co%ponents o# the s$%plin* pl$n $re $s #ollo)s

S$%plin* techni5ue

S$%plin* loc$tions

S$%plin* tools

;u%er o# s$%ples

S$%ple 5u$ntit+

S$%plin* #re5uenc+

here $ppropri$te, expl$in the s$%plin* pl$n usin* sche%$tic "i$*r$%%es'

L. ASSOCIATED DOCU)ENT

A co%prehensive $pprove" protocol

!o%plete" M.s o# $ll the v$li"$tion $tches (Bncontrolle" copies c$n e use" #or the

recor" $n" re#erence .esult #or%$ts

- 7r$nul$tion- !o%pression- !o$tin*- Other (#or other "os$*e #or%s

!erti#ic$te o# An$l+sis ( )ith An$l+tic$l Metho" ;u%er

Microiolo*ic$l !ontrol (!erti#ic$te o# An$l+sis )ith An$l+tic$l Metho" ;u%er

2.0 C$EC%S AND CONTROLS )ONITORED DURIN4 )ANUCTURIN4 PROCESSDurin* the %$nu#$cturin* process, the elo) %entione" controls $n" tests $pplic$le tothe pro"ucts @ processes $re c$rrie" out' The protocol, testin* $n" result #or%$ts $n"reports $re co%pile" )hile #ollo)in* the re5uire%ents *iven $s #ollo)s

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2.0. C$EC%S AND CONTROLS )ONITORED DURIN4 TA"LET )ANUCTURIN4 PROCESSThe #ollo)in* p$r$%eters $re %onitore" $n" teste" "urin* "i##erent st$*es o# the t$lettin*process'

PARA)ETERS )ONITORED AND TESTED DURIN4 4RANULATION

The #ollo)in* p$r$%eters $re %onitore" "urin* 7r$nul$tion- E5uip%ent

- $tch sie

- Appe$r$nce o# the *r$nul$tion- len"er, $u*er or chopper spee"- A%ount o# *r$nul$tin* #lui" ()et *r$nul$tion- 6ee" r$te o# *r$nul$tion #lui"- 7r$nul$tion ti%e

The #ollo)in* tests $re per#or%e" $t the *r$nul$tion st$*e- 4oss on Dr+in* or $ter !ontent + C6 (C$rl 6ischer (i# re5uire"- Ass$+ o# the %ixe" po)"ers (i# re5uire"

PARA)ETERS )ONITORED AND TESTED DURIN4 FLUID "ED DR#IN4

The #ollo)in* p$r$%eters $re %onitore" "urin* 6lui" e" Dr+in*

- o)l T+pe $n" ch$r*e

- nlet@exh$ust $ir te%p'- Pro"uct Te%p'- Tot$l "r+in* Ti%e- nlet Air &olu%e- :u%i"it+ o# inco%in* $n" Exh$ust $ir- Porosit+ o# #ilter $*

The #ollo)in* tests $re per#or%e" $t 6lui" e" Dr+in* st$*e- P$rticle sie @ sie "istriution (i# re5uire"- ul "ensities, 4oose $n" t$ppe" (i# re5uire"- Po)"er 6lo) (i# $pplic$le (i# re5uire"- 4oss on Dr+in* or $ter !ontent + C6-

Ass$+ o# the %ixe" po)"ers (i# re5uire"

PARA)ETERS )ONITORED AND TESTED DURIN4 )ILLIN4

The #ollo)in* p$r$%eters $re %onitore" "urin* Millin*- E5uip%ent- Screen Sie- Mill (l$"e, t+pe, spee" $n" orient$tion- 6ee" .$te

The #ollo)in* tests $re per#or%e" $t Millin* st$*e- P$rticle sie @ sie "istriution- ul "ensities, 4oose $n" t$ppe"

PARA)ETERS )ONITORED AND TESTED DURIN4 LU"RICANT "LENDIN4The #ollo)in* p$r$%eters $re %onitore" "urin* 4uric$nt len"in*- len"er T+pe- len"er 4o$"- len"er Spee"- len"in* Ti%e

The #ollo)in* tests $re per#or%e" $t 4uric$nt len"in* st$*e- P$rticle sie @ sie "istriution (i# nee"e"- ul "ensities, 4oose $n" t$ppe"(i# nee"e"- 6lo) Properties(i# nee"e"- !ontent Bni#or%it+ (i# nee"e"

PARA)ETERS )ONITORED AND TESTED DURIN4 TA"LET CO)PRESSION

The #ollo)in* p$r$%eters $re %onitore" "urin* T$let !o%pression

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- T$let Press- T$let Press Spee"- Toolin*- 6ixe" ;o' o# st$tions- Pre-co%pression 6orce- !o%pression 6orce- 6ee" 6r$%e (Open @ !lose"

The #ollo)in* tests $re per#or%e" "urin* T$let !o%pression- ei*ht !ontrol- :$r"ness- Thicness- 6ri$ilit+- Disinte*r$tion- Dissolution- Ass$+@ Dose Bni#or%it+- Ele*$nce ($ppe$r$nce "e#ects- ul hol"in* testin*, i'e' ul "ru* st$ilit+ (i# $pplic$le

PARA)ETERS )ONITORED AND TESTED DURIN4 TA"LET COATIN4

The #ollo)in* p$r$%eters $re %onitore" "urin* T$let !o$tin*- E5uip%ent- P$n 4o$"- nlet Air &olu%es- nlet @ Exh$ust :u%i"ities (# re5uire"- nlet @ Exh$ust Te%per$tures- P$n Spee"- Spr$+ ;ole Sie $n" nu%er- Ato%iin* Air pressure- Spr$+ r$te $n" spr$+ c+cle- 7un to e" "ist$nce- !o$tin* suspension viscosit+- !o$tin* e##icienc+

The #ollo)in* tests $re per#or%e" $t T$let !o$tin* st$*e- Percent )ei*ht *$in- Ele*$nce ($ppe$r$nce "e#ects- Dissolution- Ass$+- De*r$"$tion 4evel

2.0.0 C$EC%S AND CONTROLS )ONITORED DURIN4 CAPSULE )ANUCTURIN4The #ollo)in* p$r$%eters $re %onitore" $n" teste" "urin* "i##erent st$*es o# !$psuleM$nu#$cturin* Process'

PARA)ETERS )ONITORED AND TESTED DURIN4 CAPSULE PO&DER

"LENDIN4The #ollo)in* p$r$%eters $re %onitore" "urin* !$psule Po)"er len"in*- len"er - %$e, %o"el, sie- len"er lo$"- len"er Spee"- len"in* Ti%e

The #ollo)in* tests $re per#or%e" $t !$psule Po)"er len"in* st$*e- len" Bni#or%it+- Ass$+ o# the len"e" po)"ers (i# re5uire"- Dissolution on h$n" #ille" c$psules (# $ppropri$te- 4oss on Dr+in* or $ter !ontent + C6- ul "ensities, 4oose $n" t$ppe"- 6lo) Properties

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PARA)ETERS )ONITORED AND TESTED DURIN4 ENCAPSULATION

The #ollo)in* p$r$%eters $re %onitore" "urin* Enc$psul$tion- !$psule #illin* M$chine Bse"- ;u%er o# st$tion- M$chine Spee"- Po)"er e" :ei*ht- !o%p$ction Pressure

- Dos$tor &olu%e Settin*

- &$cuu% 4evel

The #ollo)in* tests $re per#or%e" $t Enc$psul$tion st$*e- Dose Bni#or%it+- ei*ht !ontrol- Ele*$nce o# 6ille" !$psules- !$psule closure (6it $n" len*th o# c$psule- Ass$+- Dissolution- Microi$l !ount-

2.0.1 C$EC%S AND CONTROLS )ONITORED DURIN4 LI,UID )ANUCTURIN4

The #ollo)in* p$r$%eters $re %onitore" $n" teste" "urin* "i##erent st$*es o# 4i5ui"%$nu#$cturin*'

PARA)ETERS )ONITORED AND TESTED AFTER LI,UID CO)POUNDIN4

The #ollo)in* p$r$%eters $re %onitore" "urin* #or%ul$tion @ !o%poun"in* o# 4i5ui""os$*e #or%s- T+pe o# &essel- Mixer t+pe- Mixin* Ti%e- Mixer spee"- Mix volu%e- Dissolvin* solvent 5u$ntit+- 6ilter t+pe, 6iltr$tion ti%e

The #ollo)in* tests $re per#or%e" $t #or%ul$tion @ !o%poun"in* st$*e o# 4i5ui" $n"Se%i-soli" "os$*e #or%s- Mix Bni#or%it+- Ass$+ o# the Solution- p:- Densit+- &iscosit+- $ter !ontent

6./. "UL% P$AR)ACEUTICAL ANAL#SISQu$lit+ !ontrol 4$ per#or%s the $n$l+ses liste" elo) usin* $ represent$tive $tchs$%ple' The result o# the $n$l+ses shoul" co%plies )ith the P, BSP, Eur Ph' 4i%its or

4i%its %entione" in the St$n"$r" Pro"uct Speci#ic$tion'

Stu"+ p$r$%eters #or Soli" Dos$*e 6or%s $re

Para(eter App!ica7!e to

!h$r$cteristics T$lets, !$psules, 7r$nules

"enti#ic$tion T$lets, !$psules, 7r$nules

Aver$*e )ei*ht T$lets, !$psules

ei*ht uni#or%it+ T$lets

Disinte*r$tion T$let, !$psules

6ri$ilit+ T$lets

Ass$+ T$lets, !$psules, 7r$nules

:$r"ness T$lets

Dissolution T$lets, !$psules, 7r$nules

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Moisture T$lets, !$psules, 7r$nules

.esi"u$l solvent T$lets, !$psules, 7r$nules

.el$te" sust$nces T$lets, !$psules, 7r$nules

Stu"+ p$r$%eters #or 4i5ui" $n" Se%i-Soli" Dos$*e 6or%s $re

Para(eter App!ica7!e to

!h$r$cteristics 4i5ui"s, Se%isoli"s"enti#ic$tion 4i5ui"s, Se%isoli"s

Densit+ 4i5ui"s, Se%isoli"s

&iscosit+ 4i5ui"s, Se%isoli"s

Ass$+ 4i5ui"s, Se%isoli"s

$ter !ontent 4i5ui"s, Se%isoli"s

.el$te" sust$nces 4i5ui"s, Se%isoli"s

Sterilit+ Test 4i5ui"s, Se%isoli"s

!opies o# the correspon"in* An$l+sis !erti#ic$tes $re $tt$che" )ith the v$li"$tion report#or recor"'

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8./ )ICRO"IOLO4ICAL CONTA)INATION CONTROL

Qu$lit+ !ontrol "eter%ines %icroi$l cont$%in$tion )ith the #ollo)in* p$r$%eters

PARA)ETERS SPECIFICATIONS

- Tot$l $eroes

$cteri$ !o%plies BSP, P, or Eur' Ph' 4i%its 6un*i !o%plies BSP, P, or Eur' Ph' 4i%its

- E. coli !o%plies BSP, P, or Eur' Ph' 4i%its

Microiolo*ic$l !ontrols $re c$rrie" out on the 6inishe" Ph$r%$ceutic$l Pro"uct' !opies o# thecorrespon"in* An$l+sis !erti#ic$tes $re $tt$che" )ith the v$li"$tion report #or recor"'

9./ VALIDATION REPORTOn co%pletion o# the $ctivities "escrie" in the protocol, Pro"uct Develop%ent Dep$rt%ent issuesthe correspon"in* &$li"$tion .eport conclu"in* $s to )hether the results ot$ine" #ro% the$tches teste" $re repe$t$le $n" "o not present si*ni#ic$nt v$ri$tions $*$inst the p$r$%eters$ssi*ne" in the &$li"$tion Protocol'

The &$li"$tion report inclu"es $nnexes )ith t$les "ul+ co%pilin* the "$t$ collecte" "urin* theexecution o# the Protocol'

The v$li"$tion report is si*ne" + $ll the persons involve" in the v$li"$tion process $n" + thehe$"s o# the concerne" "ep$rt%ents'

:./ RE VALIDATION POLIC#.ev$li"$tion )ill c$rrie" out onl+ in c$se o# ch$n*e o#

6or%ul$tion

M$nu#$cturin* process

$tch sie (i# extre%es $re not v$li"$te" "urin* initi$l v$li"$tion

E5uip%ents (i# the )orin* principle is "i##erent #or% the previous ones

Reference;

6DA, 7ui"$nce #or n"ustr+, Po)"er len"s $n" 6inishe" Dos$*e Bnits Str$ti#ie" n-Process Dos$*e Bnit S$%plin* $n"Assess%ent

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ANNE3

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sop. validation. r2

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