Tagros Chemicals India Limited-Cuddalore

Limited Doc No: L3/SOP/QC/184

Integrated Management System Rev No: 00
Department: Quality Control Rev Date: 05.06.2008
Analysis Method of Cypermethrin Technical for
Title: Page No: Page 1 of 5
Assay and Related quality parameters

I. PURPOSE:
The purpose of the procedure is to define the analysis method of Cypermethrin Technical for Assay
and related quality parameters.
II. SCOPE:
This procedure is applicable
pplicable for analysis method of Cypermethrin Technical for Assay and related
quality parameters.
III. RESPONSIBILITY:
It is the responsibility of the officer / Junior officer to execute the operation and the Sr.Officer to
ensure that the operations are carried out as per the procedure.
IV. DOCUMENT REFRENCE:
Finished Goods Product Register – Technical (FOR/QC/42)
Finished Goods Worksheet – Cypermethrin Technical (FOR/QC/17).
V. PROCEDURE:
Wear all the personal protective equipments
1. Physical Appearance:
Take 20 ml of sample
ple in a test tube, physically check the colour and any visible foreign particles
present or not, compare with standard colour grade sample and fix the colour grade.
grade
2. 10%
% solution in Toluene Test:
Weigh about 10.0
.0 gm of sample in a 100 ml cone measuring cylinder
er and make upto the mark
with toluene (LR grade) and dissolve well. Physically check the clarity and foreign particle present
or not.
3. Procedure for Assay Analysis:
a) Internal Standard:
Di-Octylphthlate
Octylphthlate of purity (Min-98.00%)
(Min
b) Reference Standard:
Standard
Cypermethrin
ermethrin Technical of purity (Min – 95.00%)
c) Preparation of Internal stock solution:
Weigh about 8 gm of Di-Octylphthalate
Di Octylphthalate in a 150ml glass beaker. Dissolve the material
completely by using Chloroform (LR grade)) and transfer into 2 lits volumetric flasks. Then
dissolve the material by using chloroform (LR grade) and make upto the mark. Dissolve the
solution carefully or sonicate for 10minutes. Then allow the solution to retain and bring to
room temperature.

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Signature

Designation Sr. Officer Asst. Manager QA Head Factory Head

 Tagros Chemicals India Limited-Cuddalore
Limited Doc No: L3/SOP/QC/184
Integrated Management System Rev No: 00
Department: Quality Control Rev Date: 05.06.2008
Analysis Method of Cypermethrin Technical for
Title: Page No: Page 2 of 5
Assay and Related quality parameters

d) Standard Preparation:
Weigh about
out 0.26gm of homogenized Cypermethrin reference standard in a separate 50ml
volumetric flask. Then dissolve the reference standard by using internal stock solution and
make upto the mark. Dissolve the solution or sonicate for 10minutes. Then allow the solution
sol
to retain and bring to room temperature. Perform a duplicate standard solution.
e) Sample Preparation:
Weigh about 0.26gm of homogenized Cypermethrin sample in a separate 50ml volumetric
flask. Then dissolve the sample by using internal stock solution and
and make upto the mark.
Dissolve the solution or sonicate for 10minutes. Then allow the solution to retain and bring to
room temperature. Perform a duplicate sample solution.
f) Injection sequence:
Blank, Standard-1,
1, Sample-1,
Sample Sample-2, Standard-2, Sample-1, Sample-2.
Sample
g) Instrument Condition:
Instrument : Gas Liquid Chromatography
Detector : FID
Column : 5% Dexil 300 ss 2 mtrs.
Temperatures:
Oven Temp : 260°C
Injector Temp : 270°C
Detector Temp : 280°C
Gas Flow Rates:
Nitrogen Flow : 30 ml/min
Hydrogen flow : 30 ml/min
Zero Air flow : 300 ml/min
Run Time : 10 min
Retention Time:
Internal Standard : 2 - 3 min
Cypermethrin : 4 - 5 min
Calculation Method : Internal Standard Method
Calculation:
Calculate the Cypermethrin content for each sample injection, the following equation.
e

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Signature

Designation Sr. Officer Asst. Manager QA Head Factory Head

 Tagros Chemicals India Limited-Cuddalore
Limited Doc No: L3/SOP/QC/184
Integrated Management System Rev No: 00
Department: Quality Control Rev Date: 05.06.2008
Analysis Method of Cypermethrin Technical for
Title: Page No: Page 3 of 5
Assay and Related quality parameters

AxBxC
Relative response factor (F) =
DxExG

A = Area of Cypermethrin peak from the standard solution.

B = Weight of Di-Octylphthalate
Octylphthalate (IS) stock solution
C= Purity of Di-Octylphthalate.
Octylphthalate.
D = Area of Di-Octylphthalate
Octylphthalate peak of the standard solution.
E = Weight of Cypermethrin in standard solution.
G = Purity of the Cypermethrin reference standard.
HxBxC
Total Cypermethrin content (%
( w/w) = ___________
IxJxF

Where,
H = Area of Cypermethrin peak in the sample solution.
I = Area of the Di-Octylphthalate
Octylphthalate peak in the sample solution
B = Weight of Di-Octylphthalate
Octylphthalate (IS) stock solution.
J = Weight of sample.
C = Purity of Di-Octylphthalate.
Octylphthalate.
F = Relative response factor.
factor

4. Procedure for Cis-Trans

Trans Isomer Analysis:
a) Standard Preparation:
Weigh about 100mg of Cypermethrin standard (known cis + trans isomer ratio) in a 10ml
volumetric flask and make upto the mark by using Mobile Phase. Dissolve the solution or
sonicate for 10minutes. Then allow the solution to retain and bring to room temperature.
b) Sample Preparation:
Weigh about 100mg of sample in a 10ml volumetric flask and make upto the mark by using
Mobile Phase. Dissolve the solution or sonicate for 10minutes. Then allow solution to retain
and bring to room temperature.

Prepared By Reviewed By Approved By Authorized By

Signature

Designation Sr. Officer Asst. Manager QA Head Factory Head

 Tagros Chemicals India Limited-Cuddalore
Limited Doc No: L3/SOP/QC/184
Integrated Management System Rev No: 00
Department: Quality Control Rev Date: 05.06.2008
Analysis Method of Cypermethrin Technical for
Title: Page No: Page 4 of 5
Assay and Related quality parameters

c) Instrument condition:
condition
Instrument : HPLC
Column : Hypersil Silica 5micron (NP),, 250mm x 4.6 mm ID.
Mobile Phase : Hexane: Di-Ethyl ether
Ratio : 98 :02
Flow : 1.50 ml / min
Detector : UV 280 nm
Injection size : 20µl
Retention time : 7.0 – 12.0 min (CIS + Trans Isomers)

Calculation:

A+B
Cis Isomer = ------------------ x 100
A+B+C+D

Trans Isomer = 100 - Cis Isomer

First peak (A) : First peak of Cis Isomer.

Second peak (B) : Second peak of Cis Isomer.
Third peak (C) : First peak of Trans Isomer.
Fourth peak (D) : Second peak of Trans Isomer
Procedure for Moisture Content:
Procedure:
Take about 5 ml of sample in a glass beaker (W 1). Then transfer the sample into KFR vessel and
reweight the beaker again (W 2). Then titrate against KFR solution. Note down the volume as T.V
(Titrate Value). Conduct the duplicate test to get concordance value.
Calculation:

T.V x water equivalent

Moisture content = ________________
___________________
10 x (W 1 - W 2)

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Signature

Designation Sr. Officer Asst. Manager QA Head Factory Head

 Tagros Chemicals India Limited-Cuddalore
Limited Doc No: L3/SOP/QC/184
Integrated Management System Rev No: 00
Department: Quality Control Rev Date: 05.06.2008
Analysis Method of Cypermethrin Technical for
Title: Page No: Page 5 of 5
Assay and Related quality parameters

Procedure for Acidity:

Reagents Required:
0.02N Sodium Hydroxide Solution
Methyl red indicator
Procedure:
Weigh accurately 10 gm of sample in a conical flask. Then add 25ml of acetone and 75ml of distilled
water and few drops of methyl red indicator and titrate against 0.02N NaOH up to orange to yellow
color change. Note
e down the burette volume as T.V
Calculation:

T.V x Normality of 0.02N NaOH x 49

Acidity (as H2SO4) = ______________________________
10 x Wt. of sample

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Signature

Designation Sr. Officer Asst. Manager QA Head Factory Head