I. PURPOSE: I. PURPOSE:
The purpose of the procedu The purpose of the procedu and related quality paramet and related quality paramet II. SCOPE:
II. SCOPE:
This procedure is applicabl This procedure is applicabl quality parameters. quality parameters. III. RESPONSIBILITY: III. RESPONSIBILITY: It is the responsibility of th It is the responsibility of th ensure that the operations a ensure that the operations a IV.
IV. DOCUMENT DOCUMENT REFRENCE:REFRENCE: Finished Goods Product Re Finished Goods Product Re Finished Goods Worksheet Finished Goods Worksheet V. PROCEDURE:
V. PROCEDURE:
Wear all the personal protec Wear all the personal protec
1.
1. Physical Physical Appearance:Appearance: Take 20 ml of sample i Take 20 ml of sample i present or not, compar present or not, compar 2.
2. 10% 10% solution solution in in ToluenToluen Weigh about 10.0 gm o Weigh about 10.0 gm o with toluene (LR grade) with toluene (LR grade) or not.
or not. 3.
3. Procedure Procedure for for AssayAssay a)
a) Internal Internal Standard:Standard: Di-Octylphthlate of p Di-Octylphthlate of p b)
b) Reference Reference StandarStandar Cypermethrin Techn Cypermethrin Techn c)
c) Preparation Preparation of of InteInte Weigh about 8 gm Weigh about 8 gm completely by using completely by using dissolve the materi dissolve the materi solution carefully or solution carefully or room temperature. room temperature.
re is to define the analysis method of Cyperme re is to define the analysis method of Cyperme rs.
rs.
for analysis method of Cypermethrin Technic for analysis method of Cypermethrin Technic
e
e officer / Junior officer to execute the operatiofficer / Junior officer to execute the operati re carried out as per the procedure.
re carried out as per the procedure.
ister – Technical (FOR/QC/42) ister – Technical (FOR/QC/42)
Cypermethrin Technical (FOR/QC/17). Cypermethrin Technical (FOR/QC/17).
tive equipments tive equipments
a test tube, physically check the colour and an a test tube, physically check the colour and an with standard colour grade sample and fix the c with standard colour grade sample and fix the c e Test:
e Test:
f sample in a 100 ml cone measuring cylinder f sample in a 100 ml cone measuring cylinder and dissolve well. Physically check the clarity an and dissolve well. Physically check the clarity an
nalysis: nalysis:
urity (Min-98.00%) urity (Min-98.00%)
::
ical of purity (Min – 95.00%) ical of purity (Min – 95.00%)
nal stock solution: nal stock solution:
of Di-Octylphthalate in a 150ml glass beake of Di-Octylphthalate in a 150ml glass beake Chloroform (LR grade) and transfer into 2 lits Chloroform (LR grade) and transfer into 2 lits l by using chloroform (LR grade) and make upt l by using chloroform (LR grade) and make upt sonicate for 10minutes. Then allow the soluti sonicate for 10minutes. Then allow the soluti
hrin Technical for Assay hrin Technical for Assay
al for Assay and related al for Assay and related
on and the Sr.Officer to on and the Sr.Officer to
y visible foreign particles y visible foreign particles olour grade.
olour grade.
nd make upto the mark nd make upto the mark d foreign particle present d foreign particle present
r. Dissolve the material r. Dissolve the material volumetric flasks. Then volumetric flasks. Then o the mark. Dissolve the o the mark. Dissolve the n to retain and bring to n to retain and bring to
d)
d) Standard Standard PreparatiPreparati Weigh about 0.26g Weigh about 0.26g volumetric flask. Th volumetric flask. Th make upto the mark make upto the mark to retain and bring to to retain and bring to e)
e) Sample Sample PreparatioPreparatio Weigh about 0.26g Weigh about 0.26g flask. Then dissolve flask. Then dissolve Dissolve the solutio Dissolve the solutio room temperature. P room temperature. P f)
f) Injection Injection sequencesequence Blank, Standard-1, Blank, Standard-1, g)
g) Instrument Instrument ConditiConditi Instrument Instrument Detector Detector Column Column Temperatures: Temperatures: Oven Temp Oven Temp Injector Temp Injector Temp Detector Temp Detector Temp Gas Flow Rates Gas Flow Rates:: Nitrogen Flow Nitrogen Flow Hydrogen flow Hydrogen flow Zero Air flow Zero Air flow Run Time Run Time Retention Time: Retention Time: Internal Standard Internal Standard Cypermethrin Cypermethrin Calculation Method Calculation Method Calculation: Calculation: o on:n:
of homogenized Cypermethrin reference stan of homogenized Cypermethrin reference stan en dissolve the reference standard by using int en dissolve the reference standard by using int . Dissolve the solution or sonicate for 10minutes . Dissolve the solution or sonicate for 10minutes room temperature. Perform a duplicate standar room temperature. Perform a duplicate standar ::
of homogenized Cypermethrin sample in a s of homogenized Cypermethrin sample in a s the sample by using internal stock solution a the sample by using internal stock solution a or sonicate for 10minutes. Then allow the solut or sonicate for 10minutes. Then allow the solut erform a duplicate sample solution.
erform a duplicate sample solution. ::
ample-1, Sample-2, Standard-2, Sample-1, Sam ample-1, Sample-2, Standard-2, Sample-1, Sam
n: n:
: Gas Liquid Chromatography : Gas Liquid Chromatography : FID : FID : : 5% Dexil 5% Dexil 300 ss 300 ss 2 mtrs.2 mtrs. : 260 : 260°°CC : 270 : 270°°CC : 280 : 280°°CC : 30 ml/min : 30 ml/min : 30 ml/min : 30 ml/min : 300 ml/min : 300 ml/min : 10 min : 10 min : 2 - 3 min : 2 - 3 min : 4 - 5 min : 4 - 5 min
: Internal Standard Method : Internal Standard Method
dard in a separate 50ml dard in a separate 50ml ernal stock solution and ernal stock solution and . Then allow the solution . Then allow the solution
solution. solution.
eparate 50ml volumetric eparate 50ml volumetric nd make upto the mark. nd make upto the mark. ion to retain and bring to ion to retain and bring to
ple-2. ple-2.
Relative response f Relative response f A = Area of Cyperm A = Area of Cyperm B = Weight of Di-Oc B = Weight of Di-Oc C= Purity of Di-Octyl C= Purity of Di-Octyl D = Area of Di-Octyl D = Area of Di-Octyl E = Weight of Cyper E = Weight of Cyper G = Purity of the Cy G = Purity of the Cy Total Cypermethrin Total Cypermethrin Where, Where, H = Area of Cyperm H = Area of Cyperm I
I = Area = Area of the of the Di-ODi-O B = Weight of Di-Oc B = Weight of Di-Oc J = Weight of sampl J = Weight of sampl C = Purity of Di-Oct C = Purity of Di-Oct F = Relative respon F = Relative respon 4.
4. Procedure Procedure for for Cis-TraCis-Tra a)
a) Standard Standard PreparatiPreparati Weigh about 100m Weigh about 100m volumetric flask and volumetric flask and sonicate for 10minut sonicate for 10minut b)
b) Sample Sample PreparatioPreparatio Weigh about 100mg Weigh about 100mg Mobile Phase. Diss Mobile Phase. Diss and bring to room te and bring to room te
A x B x C A x B x C ctor (F) ctor (F) == D x E x G D x E x G
thrin peak from the standard solution. thrin peak from the standard solution. ylphthalate (IS) stock solution
ylphthalate (IS) stock solution lphthalate.
lphthalate.
phthalate peak of the standard solution. phthalate peak of the standard solution. methrin in standard solution.
methrin in standard solution. ermethrin reference standard. ermethrin reference standard. H x B x C H x B x C ontent (% w/w) ontent (% w/w) = ___________ = ___________ I x J x F I x J x F e
ethrin peak in the sample solution.thrin peak in the sample solution.
ctylphthalate peak in the sample solution ctylphthalate peak in the sample solution
ylphthalate (IS) stock solution. ylphthalate (IS) stock solution.
.. lphthalate. lphthalate. e factor. e factor. s Isomer Analysis: s Isomer Analysis: on: on:
of Cypermethrin standard (known cis + trans of Cypermethrin standard (known cis + trans make upto the mark by using Mobile Phase. make upto the mark by using Mobile Phase. es. Then allow the solution to retain and bring to es. Then allow the solution to retain and bring to
::
of sample in a 10ml volumetric flask and mak of sample in a 10ml volumetric flask and mak lve the solution or sonicate for 10minutes. The lve the solution or sonicate for 10minutes. The mperature.
mperature.
isomer ratio) in a 10ml isomer ratio) in a 10ml Dissolve the solution or Dissolve the solution or room temperature.
room temperature.
upto the mark by using upto the mark by using n allow solution to retain n allow solution to retain
c)
c) Instrument Instrument conditiconditi Instrument Instrument Column Column Mobile Phase Mobile Phase Ratio Ratio Flow Flow Detector Detector Injection size Injection size Retention time Retention time Calculation: Calculation: A A Cis Isomer = Cis Isomer = ---A + B A + B Trans Isomer = 100 Trans Isomer = 100 First peak (A)
First peak (A) Second peak (B) Second peak (B) Third peak (C) Third peak (C) Fourth peak (D) Fourth peak (D) Procedure for Moisture Co Procedure for Moisture Co Procedure:
Procedure:
Take about 5 ml of sample Take about 5 ml of sample reweight the beaker again reweight the beaker again (Titrate Value). Conduct the (Titrate Value). Conduct the Calculation:
Calculation:
T.V T.V Moisture
Moisture content content = = ___ ___ 10 10 n: n: : HPLC : HPLC
: Hypersil Silica 5micron (NP), 250mm x 4.6 : Hypersil Silica 5micron (NP), 250mm x 4.6 : Hexane: Di-Ethyl ether
: Hexane: Di-Ethyl ether : 98 :02 : 98 :02 : 1.50 ml / min : 1.50 ml / min : UV 280 nm : UV 280 nm : 20 : 20µµll
:: 7.0 – 12.0 min (CIS + Trans Isomers)7.0 – 12.0 min (CIS + Trans Isomers)
+ B + B --- x 100 --- x 100 + + C + DC + D - Cis Isomer - Cis Isomer
: First peak of Cis Isomer. : First peak of Cis Isomer. : Second peak of Cis Isomer. : Second peak of Cis Isomer. : First peak of Trans Isomer. : First peak of Trans Isomer. : Second peak of Trans Isomer : Second peak of Trans Isomer ntent:
ntent:
in a glass beaker (W
in a glass beaker (W11). Then transfer the sam). Then transfer the sam
(W
(W22). Then titrate against KFR solution. Note). Then titrate against KFR solution. Note
duplicate test to get concordance value. duplicate test to get concordance value.
x water equivalent x water equivalent ________________ ________________ x x (W(W11- W- W22)) mm ID. mm ID.
ple into KFR vessel and ple into KFR vessel and own the volume as T.V own the volume as T.V
Procedure for Acidity: Procedure for Acidity: Reagents Required: Reagents Required:
0.02N Sodium Hydroxide So 0.02N Sodium Hydroxide So Methyl red indicator
Methyl red indicator Procedure:
Procedure:
Weigh accurately 10 gm of Weigh accurately 10 gm of water and few drops of met water and few drops of met color change. Note down th color change. Note down th
Calculation: Calculation:
Acidity (as H2SO4) Acidity (as H2SO4)
lution lution
s
sample in a conical flask. Then add 25ml of acetample in a conical flask. Then add 25ml of acet hyl red indicator and titrate against 0.02N NaO hyl red indicator and titrate against 0.02N NaO
burette volume as T.V burette volume as T.V T.V x Normality of 0.02N NaOH x 49 T.V x Normality of 0.02N NaOH x 49 = ______________________________ = ______________________________ 10 x Wt. of sample 10 x Wt. of sample
one and 75ml of distilled one and 75ml of distilled up to orange to yellow up to orange to yellow
