GB/T 5009.162-2008 English PDF (GBT5009.162-2008)

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GB/T 5009.162-2008: Determination of organochlorine pesticide and pyrethroid pesticide multiresidues in animal original foods
GB/T 5009.162-2008
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 67.040
C 53
Replacing GB/T 5009.162-2003
Determination of organochlorine pesticide and
pyrethroid pesticide multiresidues
in animal original foods
ISSUED ON: DECEMBER 03, 2008
IMPLEMENTED ON: MARCH 01, 2009
Issued by: Ministry of Health of PRC; Standardization Administration of
PRC
Table of Contents
Foreword ... 3 
1 Scope ... 4 
Method-1 -- Gas chromatography-mass spectrometry ... 5 
2 Principles ... 5 
3 Reagents ... 5 
4 Instruments ... 7 
5 Analytical procedures ... 8 
6 Calculation of results ... 10 
7 Precision ... 11 
Method-2 -- Gas chromatography-electron capture detector method (GC-ECD)
... 11 
8 Principle ... 11 
9 Reagents ... 11 
10 Instruments ... 13 
11 Analytical procedures ... 13 
12 Calculation of results ... 15 
13 Precision ... 16 
Appendix A (Informative) Time window and quantitative ion of each target
compound in method-1 (GC-MS) ... 17 
Appendix B (Informative) Chromatogram ... 20 
Appendix C (Informative) Method uncertainty ... 25 
Determination of organochlorine pesticide and
pyrethroid pesticide multiresidues
in animal original foods
1 Scope
The method-1 of this standard specifies the determination method for the
chromatography-mass spectrometry (GC-MS) of benzenehexachloride, DDT,
hexachlorobenzene, heptachlor, heptachlor epoxide, chlordane, aldrin, dieldrin,
endrin, mirex, pentachloronitrobenzene, endosulfan, fenson, allethrin,
dichlorophenyl benzensulfonate, tetramethrin, fenpropathrin, permethrin,
cypermethrin, fenralerate, deltamenthrin.
The method-2 of this standard spcifies the determination method of gas
chromatography-electron capture device (GC-ECD) for the
benzenethexzchloride, DDT, pentachloronitrobenzene, heptachlor, heptachlor
epoxide, aldrin, dieldrin, fenson, ovex, tetramethrin, permethrin, cypermethrin,
α-fenralerate, deltamethrin.
The method-1 of this standard applies to the confirmation analysis of α-
benzenehexachloride, hexachlorobenzene, β-benzenehexachloride, γ-
benzenehexachloride, pentachloronitrobenzene, δ-benzenehexachloride,
pentachloraniline, heptachlor, pentachlorophenyl sulfide, aldrin, oxychlordane,
heptachlor epoxide, trans-chlordane, α-endosulfan, cis-chlordane, p,p’-DDE,
dieldrin, endrin, β-endosulfan, p,p’-DDD, o,p’-DDT, endrin aldehyde,
endosulfan sulfate, p,p’-DDT, endrin ketone, mirex, fenson, allethrin, 2,4-
dichlorophenyl benzensulfonate, ovex, tetramethrin, fenpropathrin, permethrin,
cypermethrin, fenralerate, deltamenthrin in meat, egg, milk food, fat (including
vegetable oil).
The method-2 of this standard applies to the analysis of 20 commonly-used
organochlorine pesticides and pyrethroid pesticide residues such as α-
benzenehexachloride, β-benzenehexachloride, γ-benzenehexachloride, δ-
benzenehexachloride, pentachloronitrobenzene, heptachlor, heptachlor
epoxide, aldrin, dieldrin, fenson, ovex, p,p’-DDE, p,p’-DDD, o,p’-DDT, p,p’-DDT,
tetramethrin, permethrin, cypermethrin, α-fenralerate, deltamenthrin.
The detection limits (µg/kg) of various pesticides in method-1 of this standard
are: α-benzenehexachloride 0.20; hexachlorobenzene 0.20; β-
benzenehexachloride 0.20; γ-benzenehexachloride 0.20;
pentachloronitrobenzene 0.50; δ-benzenehexachloride 0.20; pentachloraniline
0.50; heptachlor 0.50; pentachlorophenyl sulfide 0.50; aldrin 0.50;
oxychlordane 0.20; heptachlor epoxide 0.50; trans-chlordane 0.20; α-
endosulfan 0.50; cis-chlordane 0.20; p,p’-DDE 0.20; dieldrin 0.20; endrin 0.50;
β-endosulfan 0.50; p,p’-DDD 0.20; o,p’-DDT 0.20; endrin aldehyde 0.50;
endosulfan sulfate 0.50; p,p’-DDT 0.20; endrin ketone 0.50; mirex 0.20; fenson
0.50; allethrin 0.50; 2,4-dichlorophenyl benzensulfonate 0.50; ovex 0.50;
tetramethrin 1.00; fenpropathrin 1.00; permethrin 1.00; cypermethrin 2.00;
fenralerate 2.00; deltamenthrin 2.00.
The detection limits (µg/kg) of various pesticides in method-2 of this standard
are: α-benzenehexachloride 0.25; β-benzenehexachloride 0.50; γ-
benzenehexachloride 0.25; δ-benzenehexachloride 0.25;
pentachloronitrobenzene 0.25; heptachlor 0.50; heptachlor epoxide 0.50; aldrin
0.25; dieldrin 0.50; fenson 1.25; ovex 1.25; p,p’-DDT 0.50; o,p’-DDT 0.50; p,p’-
DDE 0.60; p,p’-DDD 0.75, tetramethrin 12.50; permethrin 7.50; cypermethrin
2.00; α-fenralerate 2.50; deltamenthrin 2.50.
Method-1 -- Gas chromatography-mass spectrometry
2 Principles
In the homogeneous sample solution, quantitatively add the stable isotope
internal standard of 13C-hexachlorobenzene and 13C-mirex. It is oscillated and
extracted by organic solvent, purified by gel chromatography. It is determined
by the gas chromatography-mass spectrometry (GC-MS) with selective ion
monitoring, quantified by internal standard method.
3 Reagents
3.1 Acetone (CH3COCH3): Analytically pure, re-steamed.
3.2 Petroleum ether: Boiling range 30 °C ~ 60 °C, analytical pure, re-steamed.
3.3 Ethyl acetate (CH3COOC2H5): Analytically pure, re-steamed.
3.4 Cyclohexane (C6H12): Analytically pure, re-steamed.
3.5 n-hexane (n-C6H14): Analytically pure, re-steamed.
3.6 Sodium chloride (NaCl): Analytically pure.
3.7 Anhydrous sodium sulfate (Na2SO4): Analytically pure. Place the anhydrous
13C6-hexachlorobenzene (6 mg/L) and 5 mL of 13C10-mirex (6 mg/L). Add 40 mL
of acetone. Shake it for 30 min. The rest of the operation is the same as the
operation of eggs in 5.2.1 starting from “Add 6 g of sodium chloride”.
5.2.4 Fat: Weigh 1 g (accurate to 0.01 g). Add 5 µL of 13C6-hexachlorobenzene
(6 mg/L) and 5 mL of 13C10-mirex (6 mg/L). Add 30 mL of petroleum ether. Shake
it for 30 min. Transfer all the organic phase into a rotary evaporation flask.
Concentrate it to about 1 mL. Add 2 mL of ethyl acetate-cyclohexane (1 + 1)
solution for re-concentration. Repeat this operation for 3 times to concentrate it
to about 1 mL, to prepare for use by gel chromatographic purification. Or
otherwise transfer the concentrated solution into the sample-injection test-tube
of the fully-automatic gel permeation chromatography system. Use ethyl
acetate - cyclohexane (1 + 1) solution to rinse the rotary evaporation flask for
several times. Combine the rinsing solution into the test-tube. Make its volume
reach to 10 mL.
5.3 Purification
Choose either manual or fully-automatic purification methods.
5.3.1 Purification by manual gel column: Make the sample concentrate pass
through the gel column. Use ethyl acetate-cyclohexane (1 + 1) solution to elute
it. Discard the 0 mL ~ 35 mL fraction. Collect the 35 mL ~ 70 mL fraction. Make
it subject to rotatory evaporation and concentration to about 1 mL. Repeat the
above procedures. Collect the 35 mL ~ 70 mL fraction. Make it subject to
evaporation-concentration. Use nitrogen to purge the solvent. Then use n-
hexane to make its volume reach to 1 mL. Prepare for GC-MS analysis.
5.3.2 Purification by fully-automatic gel permeation chromatography system
(GPC): Inject the specimen through a 5 mL sample ring into the GPC column.
The pump’s flow rate is 0.5 mL/min. Use ethyl acetate-cyclohexane (1 + 1)
solution to elute it. The time program is: Discard the 0 min ~ 7.5 min fraction,
collect the 7.5 min ~ 15 min fraction, rinse the GPC column at 15 min ~ 20 min.
Make the collected fractions subject to rotatory evaporation and concentration
to about 1 mL. Use nitrogen to blow it almost dry. Use n-hexane to make its
volume reach to...