DULOXETINE HYDROCHLORIDE USP NOSCH LABS PVT.LTD.

COMMON TECHNICAL DOCUMENT HYDERABAD, INDIA

3.2.S.6 CONTAINER CLOSURE SYSTEM

Accurately weighed final drug substance is filled into a primary packaging, which consist of
transparent, virgin low density polyethylene bag. Bag is closed using nylon cable tie.

To protect the material from sunlight, the above is transferred into a non-functional secondary
packing consisting of a black colored virgin low-density polyethylene bag. This bag is also
closed using nylon cable tie.

The above pack is transfe!Ted in to a rigid functional secondary packaging container, consisting
of high molecular high-density polyethylene container, to withstand storage and transit strain.
This container is closed and sealed to avoid perforation.

Finally the API label is affixed on the container.

Choice of Material :

Polyolefins materials are safe for use in contact with pharmaceutical products. These materials
conform the required criteria for packing drug substances.

33~
DULOXETINE HYDROCHLORIDE USP NOSCH LABS PVT.LTD.
COMMON TECHNICAL DOCUMENT HYDERABAD, INDIA

3.2.S.6 CONTAINER CLOSURE SYSTEM

Compatibility of the materials of Construction

Suitability of primary packaging material

Suitability of Linear low density polyethylene (LLDPE) bags is established by testing as per
Phr.Eur. 3.1.3 for polyolefines.

Refer certificate of analysis in the following pages.

This material is obtained from the approved vendor and material will be tested as per Phr.Eur.
on annual basis.
 .
1 ; h

~
CHANDRA LABS ..L ..: 'l.i

·# 5-5-35/173, Plot No.10, 1•1 Floor, IDA, Prasanthi Nagar, Kukatpally, Hyderabad - 500 072.
Chcndrd Ldb~ Phone: 040-40113413.

.....

li1ii~!3~·l~51
..
Issued to: Registration No. CL/18-19/AS/0038
Mis .NOSCH LABS PVT LTb.
.sy No: 332,333&335;-Vliminedu (Village), Date of Receipt 07/05/2018
Chityal (Manda!) , Nalgonda (Dist)-508114, Customer Ref. No. 06/N GIAP/2012/B/R
T.S INDIA.
Report Date 22/05/2018

Sample Particulars I 30xsox400G WHITE POLYTHENE BAG

B.No PPL/A4/18/0NV35 Mfo.Dt APR/2018
B.Size 499 Ka Exp. Dt NIA
Mfg. By Nosch Labs Pvt.Ltd. Mfg.Lie No 06/NG/AP/2012/B/R
Supplier Name Nosch Labs Pvt.Ltd. Nature of Packing Poly Baa
Test Requested Tests mentioned below as per Sample Submitted 1
PH-EUR

RESULTS

.S. No. Test .. -. ._.Specification Result

I
Absorption maxima at Absorption maxima at
2920cm· 1, 2850cm· 1, 1465 2920.31cm- 1 1460.11cm·1
01 Identification-A PH-EUR
cm· 1, 1375cm·1,1170cm·1, 1379.00cm·1• 1178.61cm·1,
. 730cm· 1 & 720crrf 1 725.70cm·i.
An Orange Yellow Color An Orange Yellow Color
02 Identification C-PH-EUR
Shall develops was produced
03 Sulphated Ash- PH-EUR . NMT-1% 0.36%
NMT-1.5 ml of 0.01 M 0.9 ml of 0.01 M NaOH
04 Acidity or Alkalinity NaOH or NMT 1.0 Ml of
0.01 M HCL
05 Absorbance- PH-EUR NMT-0.2 <0.2
06 Extractable Aluminium- PH-EUR NMT-1 ppm 0.088 ppm
07 Extractable Titanium- PH-EUR NMT-1 ppm 0.04 ppm
08 Reducing Substances- PH-EUR NMT-3 ml 0.10 ml
Substances Soluble in Hexane-PH- 2.1%
09 NMT-5%
EUR
10 Extractable Heavy Metals- PH-EUR NMT-2.5 ppm 0.025 ppm
11 Extractable Zinc- PH-EUR NMT-1 ppm 0.995 ppm
Appearance of Solution 81-PH- The solution S1 should be The sol.ution S1 should be
12
EUR clear & colourless clear & colourless

Equipment Used: ICPMS (Make-Agilent, Model-7800)

ppm =parts per million

Test Method: As Per EP.

f"~v-- ..
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Authorised Signatory
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Note . This report 1s issued subject to the Terms and Cond1t1ons mentioned overleaf .
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DULOXETINE HYDROCHLORIDE USP NOSCH LABS PVT.LTD.
COMMON TECHNICAL DOCUMENT HYDERABAD, INDIA

3.2.S.6 CONTAINER CLOSURE SYSTEM

Non-functional Secondary Packaging Components:

Construction of material is black colored virgin grade linear low density polyethylene. Non-
functional secondary packaging is used to protect the drug substance from light.

Functional Secondary Packaging Component:

Construction of material is virgin grade high molecular high density polyethylene. It is light
blue in color and rigid in nature with wide opening closed with lid and clamped.

347
DULOXETINE HYDROCHLORIDE USP NOSCH LABS PVT.LTD.
COMMON TECHNICAL DOCUMENT HYDERABAD, INDIA

3.2.S.6 CONTAINER CLOSURE SYSTEM

Safety of Material of Construction

The polyolefin manufacturer undertakes that the material has been manufactured as per
requirements stipulated in IS 10146-1982 on " specification for polyethylene for safe us~ in
contact with foodstuff, pharmaceuticals and drinking water". Basic chemicals I additives
incorporated in the grade conform to the positive list of constituents as prescribed in IS 10141-
1982. Thus the grade is produced in line with FDA requirements laid down in FDA:CFR
Title 21,177.1520, Olefin polymers.

Declaration from the manufacturer is enclosed in the following pages.

Conclusion:

Based on the details referred above it is concluded that the material of construction of primary
packing material used for packing the drug substance is safe.

'"' I
.5'-1: 8
 Email: paran_polymers@redijfmail.com

Factory & Regd. Off : 77/A, IDA, Phase III, Patancheru - 502 319, Sangareddy Dist., Telangana
Tel: 08455 • 200034, 9247004560, Telefax: 08455 - 244267
Date: 08.06.2017

FQOD GRADE CERTIFICATE & ANALYSIS REPORT

Customer : NO SCH LABS PRIVATE LIMITED

Product : LDPE Polythene Liners
Quality : Food Grade Polythene Cover
Composition : RELIANCE 24 FS 040 Food Grade LDPE
: RELIANCE F 19010 Grade LLDPE
Organic Volatile Residue : Conforms to USP 661 Standards
Heavy Metals : Conforms to USP 661 Standards
Residue on Ignition : Conforms to USP 661 Standards
Other Qualities & Assurance: Easy Opening, Spots free & Proper Scaling
Invoice No. & Date 244 dated 08.06.2017
Raw material batch no : H 1720666& B1720186
~s1. Variety Size&g. Quantity Batch no
No
1 LDPE colourless 30x50x400 500 kgs PPUJ6/l7/ ONV42 dt 04-06-17
2 LDPEblack 30x50x400 500 kgs PPUJ6/17/ ONV43 dt 04-06-17

The LDPE (Low Density Polyethylene) & LLDPE (Low Low Density Polyethylene) inputs/additives used in production of
Polythene bags meets the requirements of Indian Standard IS: 10146: 2003 on Polyethylene for its safe use in contact with
food stuns, pharmaceuticals and drinking water.

The Above grade also conforms to positive list of constituents as approved in IS: 10141 The grade complies with FDA
regulation: CFR title 21,177,1520-olefin polymer.

The material complies with.EU directive EUil 0/2011. These grades also meet the regulations of Canadian food contact.

These grades also comply to clause# 3.2.2 and clause# 3.1.3 of European Pharmacopoeia 7.0 for level of various plastic
additives, phenolic antioxidant, non phenolic antioxidant and amides and sterates are well below prescribed level in the
Pharmacopeia.

These grades also comply with the European Guideline on plastic Immediate packing materials (CHMP/QWP/4359/03).
Reference should be made to the appropriate monograph(s) of the European Pharmacopoeia.

The material was processed under clean and hygienic room conditions while taking utmost care in process, sealing.
Packing, storing, and handling and is free from dust, contamination, and foreign particles and hence suitable in direct
contact to food, pharmaceuticals, and drinking water applications.

Thanking You
Yours faithfully
For PA

NW-lL f'..\0 ~ V~!\ oo t::>

rtf'-.r-.\0 ~~ 00~06\;tA

~o\tb\w\Pr
Mfrs. & Suppliers of: High Quality PP, HDPE, LDPE & LLDPE Packaging Materials with Multi-Colour Flexo Printing') I ._
..J "t 9
.'

..
Relia11ce
lndnslries.Limited

TO "'1l:IOMSOEVER IT MAY CONCERN

This is to certify that Relene Fl90l0 and Relene 24FS040 meet the requirements of Indian Standard IS:l0146: 1982 on
"Polyethylene for its. snfe use in contact with food stuffs, phannace11ticals and drinking water". Tiiese grades also conforms to the
positive list of constituents as approved in IS:l0141 The grade complies with FDA regulation: CFR title 21.177.1520, olefin
polymer and 21cfrl77.1010. These grades comply to the guidelines as depicted in 21cfr174.5 on Good Manufacturing Practices
and on substances the comes into contact with foodstuffs. Refiirencc to be made to relevant clauses a and d. Also the grade
comply with the guidelines given in 21cfrl 74.6 as tl\e migration to food-stuffs are very negligible. These grades also conform to
EC: Commission Directive 2002fl'l!EC of August 6, 2002, as amended by,2004/l/EC. 2004/19/EC, 2005179/EC, 2008/39/EC,
2007/19/EC. EU 7212002, 20041981 EC and 975/2009/EC of October 19th , 2009, 2023/2006 and also 1935/2004fEC,
1895/2005/EC and 10/2011. For contact with foodstuffs such as Tomato Paste, Diced Tomato, Fruit Concentrate, Musts, Fruit or
Vegetable Juices and Fruit Puree etc.These grades also conform to EU Regulation 128212011 amrnendcd from 10/2011 for
plastics intended to come to contact with foodstuffs. This grndc does not contain any such ingredients whose Specific
Migration Limit is mentioned in EU/l 0/2011.These grades also meets the regulations for Canadian Food Contact. These grades
also ~cct Kosher requirements.These grades also comp~y to clause ff. 3.2.2 and clause# 3.1.3 of E\lropean l'harmacopoeia
1.0 for level of'Various plastic additives, Phenolic antlo:ddant, non phenolic antioxidant and amides and stcarates are
well below prescribed level in the Pharmacopeia. The grade also complies to EN 71(3}. Accordin; to the reeipie in the
production of above grades , we do not intentionally use or add any hazardous substance like Lead (Pb), Mercury (Hg),
Cadmium (Cd), Hexnvalcnt Chromium (Cr 6+), Poly B"rominated Blphenyl (P.BB), Poly Broroinated Diphcnyl Ether
(PBDE), Polyvinyl Chloride and/or its compound and hence their traces arc not present.

These grades arc defined as a preparation under REACH. A!I components of this preparation arc compliant with the
pre·registratlon requirements of REACH. The product does not contain 'any or the chemicals proposed to be sµbstanccs of
very high concern as per REACH.
TI1cse grades also comply with the European Guideline on Plastic immediate Packaging Materials (CPMP/QWP/4359/03).
Reference should be:: made to the appropriate monograph(s} of the European Pharmacopoeia. This declaration ofRIL is restricted
to U1e material as it leaves the RIL facilities and does not !nclude any subst~ce subsequently added by the coiwerter.

l!.S1uulnrcsnn
l'l~Product lientl ('focllnlml}
Date:30.04.20l3

To : Mis Paran Polymers Prlvat~ Limited

Swastil\ Mill Compound, V.N. Pumv Marg, Chembur, Mumbai-400 071 Tel : 2,')267000 Fax: (022) 25267080 Registered Office: 3rd Floor,
MakerCbnmbers IV, 222, Narimal\ Point, Mumbai· 400 021, lndin.

350
DULOXETINE HYDROCHLORIDE USP NOSCH LABS PVT.LTD.
COMMON TECHNICAL DOCUMENT HYDERABAD, INDIA

3.2.S.6 CONTAINER CLOSURE SYSTEM

Specifications for Polythene bags (Transparent)

SI.No. Test Specifications

1.0 Description Transparent low density polythene bag with two

seals on one side, free from foreign matter.

2.0 Identification by IR The Spectrum of the material to be examined

shows maximum at 2920 cm- 1, 2850 cm- 1,
1475 cm- 1 ,1465 cm- 1, 1380 cm- 1, 1170 cm- 1,
735 cm- 1 and 720 cm- 1•

3.0 Dimensions Height ± 10 mm and - 0 mm from the seal.

Width± 10 mm and- 0 mm.

4.0 GSM 400 gauge - 108±10%

5.0 Seals Seal intact and shows no apparent defect.

6.0 Quality of granules Bags are made of virgin granules. Certificate to

be obtained on annual basis from polythene
bag manufacturer(s).

351
DULOXETINE HYDROCHLORIDE USP NOSCH LABS PVT.LTD.
COMMON TECHNICAL DOCUMENT HYDERABAD, INDIA

3.2.S.6 CONTAINER CLOSURE SYSTEM

Method of analysis for Polythene bags (Transparent)

1.0 Description:

All bags should be free from foreign matter and two seals at the bottom of the bags.
Examine physically.

2.0 Identification by IR:

Take about 0.25 g of polyethelene bag peace add 1Oml of Toluene and boil under a
Reflux condenser for about l 5min , place a few drops of the solution obtained on a
Sodium Chloride Slide and evaporate the solution in an oven at 80°C

Scan the slide and observe the maximum wave numbers at 2920 cm- 1,2850cm- 1,1475
cm- 1, 1465 cm- 1, 1380cm- 1,1170 cm- 1, 735 cm- 1 and720 cm- 1•

3.0 Dimensions:

Measure with an SS tape or SS scale with in 1 mm accuracy from the seal upwards and
record the results on a minimum of 5 bags.

4.0 GSM:

Weigh 5 bags balance and record the weights. From the dimensions and the weight
calculate GSM as follows.

Calculation:

Weight of 5 bags in gms

CJSM == ------------------------------
5x2 x W x H

Where:

W == Width of the bag in mtrs

H == Height of the bag in mtrs.

2 == Number of sides of the bag

DULOXETINE HYDROCHLORIDE USP NOSCH LABS PVT.LTD.
COMMON TECHNICAL DOCUMENT HYDERABAD, INDIA

3.2.S.6 CONTAINER CLOSURE SYSTEM

Method of analysis for Polythene bags (Transparent)

5.0 Seals:

Pour sufficient quantity of water into the bag and hang the same for 1-2 hours. If there
is any leakage the water will leak.

6.0 Quality of granules:

The bags should be made of virgin LDPE granules as verified from manufacturer's
certificate.
DULOXETINE HYDROCHLORIDE USP NOSCH LABS PVT.LTD.
COMMON TECHNICAL DOCUMENT HYDERABAD, INDIA

3.2.S.6 CONTAINER CLOSURE SYSTEM

Specifications for Polythene bags (Black)

SI.No. Test Specifications

1.0 Description Black low density polythene bag with two

seals on one side, free from foreign matter.

2.0 Identification by IR The Spectrum of the material to be examined

shows maximum at 2920 cm- 1, 2850 cm- 1,
1475 cm- 1 ,1465 cm- 1, 1380 cm- 1, 1170 cm- 1,
735 cm- 1 and 720 cm- 1•

3.0 Dimensions Height ± 10 mm and - 0 mm from the seal.

Width± 10 mm and - 0 mm.

4.0 GSM 400 gauge - 108±10%

5.0 Seals Seal intact and shows no apparent defect.

6.0 Quality of granules Bags are made of virgin granules. Certificate to be

obtained on annual basis from polythene bag
manufacturer(s).

351r
DULOXETINE HYDROCHLORIDE USP NOSCH LABS PVT.LTD.
COMMON TECHNICAL DOCUMENT HYDERABAD, INDIA

3.2.S.6 CONTAINER CLOSURE SYSTEM

Method of analysis for Polythene bags (Black)

1.0 Description:

All bags should be free from foreign matter and two seals at the bottom of the bags.
Examine physically.

2.0 Identification by IR:

Take about 0.25 g of polyethelene bag peace add lOml of Toluene and boil under a
Reflux condenser for about 15min , place a few drops of the solution obtained on a
Sodium Chloride Slide and evaporate the solution in an oven at 80°C

Scan the slide and observe the maximum wave numbers at 2920 cm- 1, 2850 cm- 1, 1475
cm- 1, 1465 cm- 1, 1380 cm- 1, 1170 cm- 1, 735 cm- 1 and720 cm- 1•

3.0 Dimensions:

Measure with an SS tape or SS scale with in 1 mm accuracy from the seal upwards and
record the results on a minimum of 5 bags.

4.0 GSM:

Weigh 5 bags on balance and record the weights. From the dimensions and the weight
calculate GSM as follows.

Calculation:

Weight of 5 bags in gms

GSM = ------------------------------
5x2 x W x H

Where:

W = Width of the bag in mtrs

H = Height of the bag in mtrs.

2 =Number of sides of the bag

355
DULOXETINE HYDROCHLORIDE USP NOSCH LABS PVT.LTD.
COMMON TECHNICAL DOCUMENT HYDERABAD, INDIA

3.2.S.6 CONTAINER CLOSURE SYSTEM

Method of analysis for Polythene bags (Black)

5.0 Seals:

Pour sufficient quantity of water into the bag and hang the same for 1-2 hours. If there
is any leakage the water will leak.

6.0 Quality of granules:

The bags should be made of virgin LDPE granules as verified from manufacturer's
certificate.

356
DULOXETINE HYDROCHLORIDE USP NOSCH LABS PVT.LTD.
COMMON TECHNICAL DOCUMENT HYDERABAD, INDIA

3.2.S.6 CONTAINER CLOSURE SYSTEM

Specifications for HDPE Container

SI.No. Test Specifications

1.0 Appearance Should be clean and dust free from inside.

2.0 Description Container made of high density polyethylene.

3.0 Inner dimensions Diameter ± 3 mm and - 0 mm

Height ± 5 mm and - 0 mm

4.0 Top lid Screw type lid made of black HDPE.

5.0 Clamps (where applicable) Galvanized and rust proof.

6.0 Handles (where applicable) One handle on either side.

7.0 Drop test No damage takes place when the test is

performed.

357
DULOXETINE HYDROCHLORIDE USP NOSCH LABS PVT.LTD.
COMMON TECHNICAL DOCUMENT HYDERABAD, INDIA

3.2.S.6 CONTAINER CLOSURE SYSTEM

Method of analysis for HDPE Container

1.0 Appearance:

Open the lids and see the drums from inside and conclude.

2.0 Description:

Refer to manufacturer certificate.

3.0 Inner Dimensions:

Measure height and inner diameter with the SS tape or SS scale with in 1 mm accuracy
in at least 5 containers.

4.0 Top Lid:

Check the colour of the lid.

5.0 Clamps:

Galvanization is uniform and free from rust when examined physically.

6.0 Handles:

Number of handles are two, one on either side. Observe physically.

7.0 Drop test:

Fill the container to its capacity with any product, put the lid and fix the clamps. Lift
the drum and drop from height of four feet. Examine for damage to the container. No
damage should take place.

358