Page No. 1/3
FC-PF-254215
PESTICIDE FORMULATION & RESIDUE ANALYTICAL CENTRE, PMD, NIPHM, HYDERABAD
Sr. No. in Scope
NABL/ NON NABL
Flow Chart for Analysis of Deltamethrin and Buprofezin in Formulation
Date of Analysis
SI.
No.
1.
2.
3.
3.1
3.1.1
3.1.2
3.1.3
3.1.4
3.2
3.2.1
3.2.2
3.2.3
3.2.4
3.3
3.3.1
3.3.2
3.3.3
3.4
3.4.1
3.4.2
3.4.3
3.4.4
3.4.5
3.4.6
3.4.7
3.4.8
3.4.9
3.4.10
3.5
3.5.1
3.5.2
Execution
Step
Sample No.
Name of Sample
Procedure
Preparation of Mobile Phase
Mix Isooctane and 1,4-dioxane (0.15% water) in
the proportion of 95:5 (v/v)
Pass through membrane filter under vacuum
Homogenize the mixture using a magnetic stirrer
Allow to attain room temperature
Preparation of Make up Phase
Mix Isooctane : 1,4-dioxane in the proportion of
80:20 (v/v)
Pass through membrane filter under vacuum
Homogenize the mixture using a magnetic stirrer
Allow to attain room temperature
Preparation of Internal Standard Solution
Weigh 5 g of Di-butyl phthalate (DBP) in 100 ml
volumetric flask
Add 40 ml of make up phase(3.2.4) and mix well
Dilute up to the mark with make up phase (3.2.4)
Preparation of Standard Solution
Note the Purity of Deltamethrin standard
Weigh0.040 g a.i. of the standard Deltamethrin
accurately in a 50 ml volumetric flask
Note the serial No. of the balance log book
Make up the volume with Make-up phase (3.2.4)
(stock A).
Note the Purity of Buprofezin standard
Weigh 0.032 g a.i. of the standard Buprofezin
accurately in a 50 ml volumetric flask.
Note the serial No. of the balance log book
Add to it 5 ml of Internal standard solution (3.3.3)
Add to it 5 ml of Deltamethrin stock A solution
(3.4.4) and mix well
Make up the volume with Make-up phase (3.2.4)
Preparation of Sample Solution
Note the percent active ingredient contents
declared on the sample for Deltamethrin and
Buprofezin respectively.
Weigh 0.560 g of sample in 50 ml volumetric flask
R1
Executed
By
R2
g
g
ml
ml
%
g
%
g
%
g
%
g
%
%
g
g
Name of the Laboratory : Pesticide Formulation & Residue Analytical Centre, PMD, NIPHM, Hyderabad
Flow Chart for Analysis of Deltamethrin and
Document No.
: FC-PF-254
Document Name
:
Buprofezin, % by mass
Revision No.
: 02
Issue Date
:
04/08/2013
Revised Date
: 26/03/2014
Next Revision Date
:
26/03/2016
Prepared By
Checked By
Approved & Issued By
Mrs. C. Vijaya Lakshmi
(Assistant Plant Protection Officer)
Mr. C. V. Rao
(Technical Manager)
Dr. Abhay Ekbote
(Director PM & Quality Manager)
Page No. 2/3
FC-PF-254215
PESTICIDE FORMULATION & RESIDUE ANALYTICAL CENTRE, PMD, NIPHM, HYDERABAD
3.5.3
3.5.4
3.5.5
3.5.6
4.
4.1
4.1.1
4.1.2
4.1.3
4.1.4
4.2
4.2.1
4.2.2
4.3
4.4
4.5
5.
Note the serial No. of the balance log book
Add to it 10 ml of makeup phase (3.2.4) and mix
well.
Add to it 5 ml of Internal Standard solution
(3.3.3)and mix well
Dilute up to the mark with solvent mixture (3.2.4)
HPLC Parameters
Column
Stainless Steel Packed with Silica
Length:
250 mm
I.D.:
4.6 mm
Particle Size :
5µ
Mobile Phase
Isooctane : 1,4-dioxane (0.15% water) (95 : 5)
Flow Rate:
0.8 ml/min
Detector:
UV
Wave Length:
254 nm
Injection Volume:
20 µl
Result
Sample chromatogram no.
Standard chromatogram no.
6. Calculation:
Deltamethrin content, % by mass =
A1 x A ‘IS’1 x M1 x 1
-------------------------- XP
A’IS’2 x A2 x M3 x 10
Where,
A1
=
A’IS’2 =
A’IS’1 =
A2
=
M1
=
M3
=
P
=
10
=
Peak area of Deltamethrin in the sample solution
Peak area of internal standard in the sample solution
Peak area of internal standard in the standard solution
Peak area of Deltamethrin in the standard solution
Mass in ‘g’ of Deltamethrin in the standard solution
Mass in ‘g’ of sample taken for test
Percentage purity of Deltamethrin standard
Dilution Factor
Name of the Laboratory : Pesticide Formulation & Residue Analytical Centre, PMD, NIPHM, Hyderabad
Flow Chart for Analysis of Deltamethrin and
Document No.
: FC-PF-254
Document Name
:
Buprofezin, % by mass
Revision No.
: 02
Issue Date
:
04/08/2013
Revised Date
: 26/03/2014
Next Revision Date
:
26/03/2016
Prepared By
Checked By
Approved & Issued By
Mrs. C. Vijaya Lakshmi
(Assistant Plant Protection Officer)
Mr. C. V. Rao
(Technical Manager)
Dr. Abhay Ekbote
(Director PM & Quality Manager)
Page No. 3/3
FC-PF-254215
PESTICIDE FORMULATION & RESIDUE ANALYTICAL CENTRE, PMD, NIPHM, HYDERABAD
Buprofezin content, % by mass =
A3 x A ‘IS’1 x M2
--------------------- XP
A’IS’2 x A4 x M3
Where,
A3
=
A’IS’2 =
A’IS’1 =
A4
=
M2
=
M3
=
P
=
Peak area of Buprofezin in the sample solution
Peak area of internal standard in the sample solution
Peak area of internal standard in the standard solution
Peak area of Buprofezin in the standard solution
Mass in ‘g’ of Buprofezin in the standard solution
Mass in ‘g’ of sample taken for test
Percentage purity of Buprofezin standard
Result:
SI. No.
Name of test
1.
Active ingredient
Name of the A.I
Result
1) Deltamethrin
2) Buprofezin
Unit
Method of Analysis
%
HPLC Method
Remark / Reference :
Analyzed by
Checked by
Name
Dated signature
Name
Dated signature
Name of the Laboratory : Pesticide Formulation & Residue Analytical Centre, PMD, NIPHM, Hyderabad
Flow Chart for Analysis of Deltamethrin and
Document No.
: FC-PF-254
Document Name
:
Buprofezin, % by mass
Revision No.
: 02
Issue Date
:
04/08/2013
Revised Date
: 26/03/2014
Next Revision Date
:
26/03/2016
Prepared By
Checked By
Approved & Issued By
Mrs. C. Vijaya Lakshmi
(Assistant Plant Protection Officer)
Mr. C. V. Rao
(Technical Manager)
Dr. Abhay Ekbote
(Director PM & Quality Manager)