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GB/T 5009.162-2008 (GB/T5009.162-2008)

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GB/T 5009.162-2008: PDF in English (GBT 5009.162-2008)

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 1 mL. Prepare for GC-MS analysis.
5.4 Determination
5.4.1 Reference conditions for gas chromatography
5.4.1.1 Column: CP-sil 8 capillary column or equivalent column. The column
length is 30 m. The film thickness is 0.25 µm. The inner diameter is 0.25 mm.
5.4.1.2 Temperature at sample inlet: 230 °C.
5.4.1.3 Column temperature program: The initial temperature is 50 °C. Keep
Where:
X - The content of each pesticide component in the specimen, in micrograms
per kilogram (µg/kg);
A - The mass of the target compound corresponding to the area ratio of the
chromatographic peak of the specimen to the internal standard’s
chromatographic peak, in nanograms (ng);
f - The dilution factor of the sample solution;
m - The size of the sample, in grams (g).
For the calculation results, it retains three significant figures.
7 Precision
The absolute difference between two independent determinations obtained
under repetitive conditions shall not exceed 20% of the arithmetic mean. The
method uncertainty is as shown in Appendix C.
Method-2 -- Gas chromatography-electron capture
detector method (GC-ECD)
8 Principle
The sample is extracted, purified, concentrated, constant-volume, separated by
capillary column gas chromatography, detected by electron capture detector,
qualitative-determined by the retention time, quantified by external standard
method. Peak order: α-HCH, β-HCH, γ-HCH, pentachloronitrobenzene, δ-HCH,
heptachlor, aldrin, fenson, heptachlor epoxide, ovex, dieldrin, p, p’-DDE, p, p’-
DDD, o,p’-DDT, p,p’-DDT, tetramethrin, permethrin, cypermethrin, α-fenralerate,
deltamethrin.
9 Reagents
9.1 Acetone: Re-steamed.
9.2 Dichloromethane: Re-steamed.
9.3 Ethyl acetate: Re-steamed.
10 Instruments
10.1 Gas Chromatograph: It is equipped with electron capture detector,
capillary column.
10.2 Rotary evaporator.
10.3 Gel purification column: The glass chromatographic column with piston
which has a length of 30 cm and an inner diameter of 2.5 cm. Fill a little glass
wool at the bottom of the column. Use the wet method to put the gel which had
been immersed in the eluent ethyl acetate-cyclohexane (1 + 1) in the column.
The height of column is about 26 cm. Make the gel always be maintained in the
eluent.
11 Analytical procedures
11.1 Preparation of specimen
Remove the shell of egg. Make it into a homogenate. Remove the tendon from
meat. Cut it into small pieces. Make it into meat paste. Mix the milk products
uniformly to prepare for use.
11.2 Extraction and distribution
11.2.1 Weigh 20 g of specimen (accurate to 0.01 g). Place it in a 100 mL
stoppered conical flask. Add 5 mL of water (add water depending on the
moisture content of the specimen, to make the total moisture content be about
20 g. Fresh egg generally contains about 75% water, so it needs adding 5 mL
of water). Add 40 mL of acetone. Shake it for 30 min. Add 6 g of sodium chloride.
Shake it uniformly. Then add 30 mL of petroleum ether. Shake it for 30 min.
Take 35 mL of supernatant. Use anhydrous sodium sulfate to filter it into a rotary
evaporation flask. Concentrate it to about 1 mL. Add 2 mL of ethyl acetate-
cyclohexane (1 + 1) for re-concentration. Repeat this for 3 times. Concentrate
it to about 1 mL.
11.2.2 Weigh 20 g of specimen (accurate to 0.01 g). Add 6 mL of water (add
water depending on the moisture content of the specimen, to make the total
moisture content be about 20 g. Fresh meat generally contains about 70% water,
so it needs adding 6 mL of water). The rest of the operation is the same as the
operation in 11.2.1 in terms of the procedures of extraction and distribution of
egg samples.
11.2.3 Weigh 20 g of specimen (accurate to 0.01 g. Fresh milk does not need
to add water, which is extracted by adding acetone directly). The rest of the
operation is the same as the operation in 11.2.1 in terms of the procedures of
......
 
Source: Above contents are excerpted from the PDF -- translated/reviewed by: www.chinesestandard.net / Wayne Zheng et al.