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Name of molecule

Study Title /Project Name


Sponsor
Original Manufacturer
Study Director
Study Personnel
Test facility Management
Sample Received Date
Batch No.
Mfg. Date
Expiry Date
Laboratory Code

Study Initiated date/Date


of analysis started

Study Completion date


Report date
Project Code Number
Report Code Number

Test Facility

Sponsor
Address/Customer Name
and address

Impurity standards No.

1 Active
2 Impurity Std -1
3 Impurity Std -2
4 Impurity Std -3
5 Impurity Std -4
6 Impurity Std -5
7 Impurity Std -6
8 Impurity Std -7
9 Impurity Std -8
10 Impurity Std -9
11 Impurity Std -10
12 Impurity Std -11
13 Impurity Std -12
14 Impurity Std -13
15
16
Sr. No.
1
2
4
3
5
6
7
8
9

Method No.
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
Boscalid
Analytical Test Report on Fenazaquin 18.3 % w/w SC (200 SC)
M/s UPL Limited, Mumbai
M/s UPL Limited, Mumbai
Mr. Iqbal Shaikh, M,Sc.
Mr. Sandeep Jagtap, M.Sc.
Kedar Deobhankar, Ph.D.
3/29/2017
BOS/R2/S1/086
11/25/2016
11/24/2018
C/1595/1

09 May 2017

07 November 2017
10 November 2017
RLS/TS/242/10/16/0011426
RLS/TS/242/10/16/0011426/2
Ross Lifescience Private Limited, Plot No. 96, Sector No. 10, PNTDA, Bhosari, Pune -
411026, Maharashtra, India.

M/s UPL Limited., UPL House, 610 B/2, Bandra Village, Off Western Express Highway,
Bandra (East), Mumbai 400 051

Impurity standard name

Boscalid
A
B
C
D
E
F
G
H
I
J
K
L
M
Moisture
Other impurities
Parameter Name
Description
a.i. content, percent by mass
Moisture content, percent by mass
pH (1% solution in water)
Material insoluble in acetone, percent by mass
Acidity (as H2SO4), percent by mass
Alkalinity (as NaOH), percent by mass
Melting Point ,°C
Ash content ,percent by mass

METHODS
DESCRIPTION
ACTIVE CONTENT (WITH IS)-BY HPLC
ACTIVE CONTENT (WITH IS)-BY GC
ACTIVE CONTENT (WITHOUT IS)-BY HPLC
ACTIVE CONTENT (WITHOUT IS) BY GC
MOISTURE (WATER) CONTENT BY IS
MOISTURE (WATER) CONTENT BY CIPAC
pH CONTENT
MATERIAL INSOLUBLE IN ACETONE
ACIDITY (as H2SO4)
ALKALINITY (as NaOH)
MELTING POINT
ASH CONTENT
IMPURITY CONTENT BY HPLC
IMPURITY CONTENT BY GC
Test Facility
Nature of Test Item Insecticide
Fungicide Before
Herbicide GLP 17 April 2017

12 February 2013
Sathiyanarayanan,S. Ph.D. 12 February 2015
NABL 24 September 2015
24 September 2017
06 December 2017

31 October 2011

01 April 2014
DSIR
01 April 2017
27 June 2017

25 June 2015
CIB&RC
19 May 2017

GI/019 For all dates

Impurity profile

% Purity of impurity Impurity


Standards Wt. in Sample Wt. in Volumetric Flask
Diluent
standards mg Dilution-1
mg
99.90 100.2 Acetonitrile 10
99.00 10.2 100.2 Acetonitrile 10
98.00 10.5 100.2 Acetonitrile 10
97.00 10.6 100.2 Acetonitrile 10
99.00 10.8 100.2 Acetonitrile 10
99.50 10.4 100.2 Acetonitrile 10
99.20 10.2 100.2 Acetonitrile 10
99.00 10.6 100.2 Acetonitrile 10
99.00 10.5 100.2 Acetonitrile 10
99.10 10.8 100.2 Acetonitrile 10
99.00 10.1 100.2 Acetonitrile 10
99.50 10.1 100.2 Acetonitrile 10
99.00 10.0 100.2 Acetonitrile 10
99.10 10.7 100.2 Acetonitrile 10
Specification Observation
White solid
White solid powder powder
Min. 95.00 97.52
Max. 1.00 0.52
4.00-6.50 5.20 (This yellow
marking value
Max. 0.50 0.20 should be linked to
Max. 0.50 0.25 Averarage or mean
average value of
Max. 0.50 0.15 respective tests)
121-125 123
Max. 2.00 1.02

Method No.
4.1 3.1
4.2 3.2
4.3 3.3
4.4 3.4
4.5 3.5
4.6 3.6
4.7 3.7
4.8 3.8
4.9 3.9
4.10 3.10
4.11 3.11
4.12 3.12
4.13 3.13
4.14 3.14
4.15 3.15
Page No. 23 GLP

17 April 2017 Nil


17 April 2020 GLP certified (Chemistry including 5 batch analyses, and ecotoxicology)-GLP/C-098/

11 February 2015 ISO/IEC-17025-2005 accredited (NABL) - Chemical (Certificate No. T-2446) and Biological
23 September 2015 Nil
23 September 2017 ISO/IEC-17025-2005 accredited (NABL) - Chemical (Certificate No. T-2446) and Biological
05 December 2017 Nil
05 December 2019 ISO/IEC-17025-2005 accredited (NABL) - Chemical and Biological (Certificate No. TC-6633

31 March 2014 DSIR- recognized “in-house’ laboratory (TU/IV-RD/3310/2011). Valid till 31-March-2013

31 March 2017
DSIR- recognized “in-house’ laboratory (TU/IV-RD/3310/2014). Valid till 31-March-2017
26 June 2017 Nil
31 March 2020 DSIR- recognized “in-house’ laboratory (TU/IV-RD/3310/2017). Valid till 31-March-2020

18 May 2017 Approved by CIB&RC for registration data generation- as per 356th RC Meeting held on 25th J

18 May 2019 Approved by CIB&RC for registration data generation- as per 375th RC Meeting held on 19th M

Sponsored by Science and Technology Park promoted by NSTEDB- Govt of India and U

Pipette Dilution in ml Volumetric Flask Dilution factor Specification


into flask Dilution-2

96 Min.
1 50 0.02 1.0 Max.
1 50 0.02 0.5 Max.
1 50 0.02 0.5 Max.
1 50 0.02 0.3 Max.
1 50 0.02 0.3 Max.
1 50 0.02 0.3 Max.
1 50 0.02 0.2 Max.
1 50 0.02 0.2 Max.
1 50 0.02 0.2 Max.
1 50 0.02 0.2 Max.
1 50 0.02 0.2 Max.
1 50 0.02 0.2 Max.
1 50 0.02 0.2 Max.
0.2 Max.
0.2 Max.
and ecotoxicology)-GLP/C-098/2017-Valid -16-April 2020

tificate No. T-2446) and Biological (Certificate No. T-2447) valid till 11-February-2015

tificate No. T-2446) and Biological (Certificate No. T-2447) valid till 23-September-2017

Biological (Certificate No. TC-6633) valid till 05-December-2019

0/2011). Valid till 31-March-2013

0/2014). Valid till 31-March-2017

0/2017). Valid till 31-March-2020

per 356th RC Meeting held on 25th June 2015 (valid till May-2017)

per 375th RC Meeting held on 19th May 2017 (valid till April-2019)

NSTEDB- Govt of India and University of Pune (License no-Gl/019)

Observations
MATERIALS
CHEMICALS AND REAGENTS
Sr. No. Reagent /Chemicals
1 Acetonitrile (HPLC grade)
2 Methanol (HPLC grade)
3 Water (HPLC grade)
4 Distilled Water
5 Dried Methanol
6 Dried Acetone
7 Orthosphoric Acid (HPLC grade)
8 Acetone (HPLC grade)
9 Karl Fischer Reagents
10 0.05 Sodium Hydroxide solution
11 Methyl red indicator solution
12 Acetic Acid (HPLC grade)
13 Acetic Anhydride (AR grade)
14 Toluene (HPLC grade)
15 Hexane (HPLC grade)
16 Ethyl Acetate ((AR grade)
17 Methylene Chloride (AR grade)
18 Tetrahydrofuran (HPLC grade)
19 0.05Potassium Hydroxide
20 0.05 Hydrochloric acid solution
21 Formic Acid (HPLC grade)
22 Crystal Violet Indicator solution
23 0.1 N Silver nitrate solution
24 0.1 N Anmonium thiocyanate solution
25
26
27
28
29
30

LIST OF IN
Sr .No. Instruments /Apparatus Make
1 HPLC Shimadzu
2 GC Agilent (7820 A)
3 Analytical Balance M/s. Contech India
4 Standard Lab Glasswares A Class
5 Karl fisher Autotitrator M/s. Metrohm
6 Microliter Syringe 0-50 µl Capacity
7 pH meter Eutech
8 Meling point/Boiling point apparatus Veego
9 Sonicator Upper India Scientific
10 Water Bath Met lab
11 Hot air Oven Met lab
12 Sintered Glass Filtering crucible porocity No.3 Borocilicate
13 250 ml Erlenmeyer flask Borocilicate
14 FT IR Agilent
15 UV -Visible Spectrophotometer Shimadzu
16 LCMS -MS Waters
17 GCMS Agilent
18 NMR Bruker
LIST OF INSTRUMENTS AND APPARATUS
Model
UV-1800 Series
Acquity- H Class with Xevo TQD Mass Detector Acquity
5977 E -MSD , 7820 A-GC
Software Detector
LC Solution software PDA
Ezchrome Elite /Open lab software FID
UVprobe2.52
Masslynx.4.1
Open lab 2.2
Desiccator
Mechanical Shaker
Stability Chamber Newtronics
4 RESULTS

4.1. DESCRIPTION
A white colour granules free from extraneous matter.

4.2. ACTIVE CONTENT (WITH IS)-BY HPLC


4.3 ACTIVE CONTENT (WITH IS)-BY GC
Table - 1 : Calculation results - Active content

Area of Active Area of Active Areathe


of IS in
Weight of Weight of in the standard in the sample standard
standard sample
Replicates solution solution solution
mg mg
M1 M2 A1 A2 A3
S1R1 35.2 35.7 17437785 17448562 6674256
S1R2 35.2 35.7 17437785 17562531 6674256
S2R1 35.2 35.5 17463281 17495842 6676954
S2R2 35.2 35.5 17463281 17452654 6676954

4.4 ACTIVE CONTENT (WITHOUT IS)-BY HPLC


4.5 ACTIVE CONTENT (WITHOUT IS) BY GC
Table - 2 : Calculation results - Active content

Area of Active Area of Active


Weight of Weight of in the standard in the sample %Standard
Purity of
standard sample
Replicates solution solution

mg mg
M1 M2 A1 A2 P
S1R1 35.2 35.7 17437785 17448562 99.90
S1R2 35.2 35.7 17437785 17562531 99.90
S2R1 35.2 35.5 17463281 17495842 99.90
S2R2 35.2 35.5 17463281 17452654 99.90

4.6 MOISTURE (WATER) CONTENT BY IS


Table-3 : Water equivalence factor

Water
Weight of KF Reading Mean Factor ,T
Sr.No. equivalence
water (mg) (ml) (mg/ml)
factor (T)

1 10.3 2.01 5.1244


2 10.2 2.00 5.1050 5.1016
3 10.1 1.99 5.0754
4.7 MOISTURE (WATER) CONTENT BY CIPAC
Table-5 : Water equivalence factor

Water
Weight of KF Reading Mean Factor E
Sr.No. equivalence
water (gm) W (ml) b (g/l)
factor (T)

1 0.0395 7.81 5.0576


2 0.0391 7.80 5.0128 5.0256
3 0.0390 7.79 5.0064

4.8. pH content
Table-7: pH results

Sample Avg. pH
Sample No. weight in gm pH observed observed

1 1.0052 5.50
5.54
2 1.0063 5.58

4.9 Material insoluble in acetone


Table-8: Material insoluble in acetone content results

Material
Weight of
Weight of empty Weight of Weight of insoluble in
Sample No. sample in gm crucible crucible + residue in gm acetone,
in
(M) residue in gm (m) percent by
gm mass

1 10.0325 65.3521 65.3572 0.0051 0.05


2 10.0852 65.3248 65.3313 0.0065 0.06

4.10 ACIDITY (as H2SO4)


Table-9: Acidity content results

Normality
Mass of the Blank Titration of 0.05N
sample taken reading Difference in
Sample No. for test in (v) reading(V) in Sodium
gm ml
in ml ml Hydroxide
(M) solution (N)

1 10.0141 0.1 0.5 0.4 0.0501


2 10.1027 0.1 0.7 0.5 0.0501

4.11 Alkalinity (as NaOH)


Table-10: Alkalinity content results

Normality
Mass of the Blank Titration of 0.05N
sample taken reading Difference in Hydrochlori
Sample No. for test in (v) reading(V) in
gm ml
in ml ml c acid
(M) solution (N)
Normality
Mass of the Blank Titration of 0.05N
sample taken reading Difference in Hydrochlori
Sample No. for test in (v) reading(V) in
gm ml
in ml ml c acid
(M) solution (N)

1 10.0654 0.1 0.6 0.5 0.0505


2 10.0748 0.1 0.7 0.6 0.0505

4.12 Melting Point


Table-11: Melting point results

point Avg.point
Melting
Sample No. Melting
observed °C observed °C

1 105.0
105.5
2 106.0

4.13 Ash content


Table-12: Ash content results
Weight of
Weight of
Weight of empty Weight of residue
silica silica crucible +cruccible (M2-M1 ) in
Sample No sample in gm crucible gm
(M) (M2) in gm + sample in gm after ignition
(M1) in gm
1 1.0065 37.8546 38.8611 38.8752 1.0206
2 1.0087 37.8985 38.9072 38.9285 1.0300

4.14 IMPURITY CONTENT BY HPLC


4.15 IMPURITY CONTENT BY GC
Table-13: IMPURITY PROFILE CALCULATION
A1 A2 M1 M2 D

Impurity Peak area of Peak area of


No. /Name Impurity in the Impurity in Wt. of STD Wt. of sample Dilution
Standard the Sample (mg) (mg) factor
solution solution

A
Impurity-1 8716307 10.2 100.2 0.02
B
Impurity-2 34118980 2525211 10.5 100.2 0.02
C
Impurity-3 71034 12562 10.6 100.2 0.02
D
Impurity-4 241731 10.8 100.2 0.02
E
Impurity-5 19708539 10.4 100.2 0.02
F
Impurity-6 27645144 10.2 100.2 0.02
G
Impurity-7 14939068 1254723 10.6 100.2 0.02
H
Impurity-8 18520074 1256544 10.5 100.2 0.02
I
Impurity-9 11968959 1442291 10.8 100.2 0.02
J
Impurity-10 7705078 1631071 10.1 100.2 0.02
K
Impurity-11 7705078 1631072 10.1 100.2 0.02
L
Impurity-12 7705078 1631073 10.0 100.2 0.02
M
Impurity-13 7705078 1631078 10.7 100.2 0.02
on results - Active content
Active
Area of IS in % Purity of Mean Avg.
Content, Avg. Active
the sample Active
Standard percent by Content,
solution Content,
mass percent by percent by
mass mass
A4 P
6647512 99.90 98.96
99.15
6665284 99.90 99.34
99.26
6651247 99.90 99.62
99.37
6669282 99.90 99.11

ve content
Active
Content, Mean Avg.
Avg. Active
percent by Active
Content,
mass Content,
percent by percent by
mass mass

98.56
98.88
99.21
99.00
99.24
99.12
99.00

Table-4 : Water content results

Water Average
Moisture
equivalent of Weight of Volume of the Moisture
Sample content
Karl Fischer Sample in g Karl Fischer content
No. ,percent by
reagent (T) (E) reagent (B) ,percent by
mass
(mg/ml) mass

1 5.1016 1.0050 0.21 0.11


0.12
2 5.1016 1.0256 0.25 0.12
Table-6: Water content results

Water Volume
equivalence mass of Moisture
required for
Sample of Karl sample Moisture content,
the sample content ,g/kg percent
No. Fischer taken (g) by
determination
reagent (E) (w) mass
(ml) (t)
(g/l)

1 5.0256 5.0125 10.1 10.13 1.01


2 5.0256 5.0136 10.3 10.32 1.03

Avg.
Material
insoluble in
acetone,
percent by
mass

0.06

Acidity (as Avg. Acidity


H2SO4), (as H2SO4),
percent by percent by
mass mass

0.02
0.02
0.02

Alkalinity Avg.Alkalinity
(as NaOH), (as NaOH),
percent by percent by
mass mass
Alkalinity Avg.Alkalinity
(as NaOH), (as NaOH),
percent by percent by
mass mass

0.02
0.02
0.02

Ash Avg. Ash


content, content,
percent by percent by
mass mass

1.01
1.02
1.02

ILE CALCULATION
P

Retention
Impurity time Retention time
% Purity of content, observed of observed of
Impurity percent by impurity in impurity in
standard
mass standard sample solution
solution

99.00 0.00 2.52

98.00 0.02 2.89 2.94

97.00 0.04 3.51 3.56

99.00 0.00 3.79


99.50 0.00 4.25

99.20 0.00 4.65

99.00 0.02 5.40 5.42

99.00 0.01 5.98 6.02

99.10 0.03 7.62 7.68

99.00 0.04 8.52 8.55

99.50 0.04 9.12 9.16

99.00 0.04 10.45 10.47

99.10 0.04 10.25 10.25


Avg. Moisture
content ,percent
by mass

1.02