GB/T 5009.19-2008 PDF English
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Standard ID | Contents [version] | USD | STEP2 | [PDF] delivery | Name of Chinese Standard | Status |
GB/T 5009.19-2008 | English | 85 |
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Determination of organochlorine pesticide multiresidues in foods
| Valid |
GB/T 5009.19-2003 | English | 239 |
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2 days
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Determination of HCH and DDT residues in foods
| Obsolete |
GB/T 5009.19-1996 | English | 199 |
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2 days
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Method for determination of BHC and DDT residues in foods
| Obsolete |
GB 5009.19-1985 | English | 199 |
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2 days
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Method for determination of BHC and DDT residues in foods
| Obsolete |
Excerpted PDFs (Download full copy in 9 seconds upon purchase)PDF Preview: GB/T 5009.19-2008
GB/T 5009.19-2008: Determination of organochlorine pesticide multiresidues in foods---This is an excerpt. Full copy of true-PDF in English version (including equations, symbols, images, flow-chart, tables, and figures etc.), auto-downloaded/delivered in 9 seconds, can be purchased online: https://www.ChineseStandard.net/PDF.aspx/GBT5009.19-2008
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 67.040
C 53
Replacing GB/T 5009.19-2003
Determination of organochlorine pesticide
multiresidues in foods
Issued on. DECEMBER 03, 2008
Implemented on. MARCH 01, 2009
Issued by. Ministry of Health of the People’s Republic of China;
Standardization Administration of China.
Table of Contents
Foreword... 3
1 Scope... 5
Method One -- Gas chromatography - Electron capture detector method... 5
2 Principle... 5
3 Reagents... 6
4 Apparatus... 6
5 Analysis steps... 7
6 Result calculation... 9
7 Precision... 10
Method Two -- Packed column gas chromatography - Electron capture detector
method... 10
8 Principle... 10
9 Reagents... 10
10 Apparatus... 11
11 Analysis steps... 11
12 Result calculation... 12
13 Precision... 13
Annex A (informative) Detection limit of different matrix specimens... 14
Annex B (informative) Chromatogram of organochlorine pesticide mixed
standard solution... 15
Annex C (informative) Method uncertainty... 16
1 Scope
Method One of this Standard specifies the determination of
hexachlorocyclohexane (HCH), dichloro-diphenyl-dichloroethane (DDD),
hexachlorobenzene, mirex, heptachlor, chlordane, aldrin, dieldrin, endrin,
endosulfan, pentachloronitrobenzene in foods. Method Two specified the
determination of residues of hexachlorocyclohexane, dichloro-diphenyl-
trichloroethane (DDT) in foods.
Method One of this Standard is applicable to the analysis on α-HCH,
hexachlorobenzene, β-HCH, γ-HCH, pentachloronitrobenzene, δ-HCH,
pentachloroaniline, heptachlor, pentachlorophenyl sulfide, aldrin,
oxychlorohydrin, epoxy heptachlor, trans-chlordane, α-endosulfan, cis-
chlordane, p, p'- DDE, dieldrin, endrin, beta-endosulfan, p,p'-DDD, o, p'-DDT,
endrin aldehyde, endosulfan sulfate, p, p'-DDT, endrin ketone, mirex in meat,
eggs, dairy foods and plants (including fats). Method Two is applicable to the
determination of HCH, DDT residues in various foods.
The detection limit determined by Method One varies with the specimen matrix,
see Annex A. Detection limit of Method Two. when the sampling amount is 2g,
the final volume is 5mL, and the injection volume is 10μL, the detection limits
for α-HCH, β-HCH, γ-HCH, and δ-HCH are sequentially as 0.038 μg/kg, 0.16
μg/kg, 0.047 μg/kg, and 0.070 μg/kg; the detection limits for p,p'-DDE, o,p'-DDT,
p,p'-DDD, p,p'-DDT are sequentially as 0.23 μg/kg, 0.50 μg/kg, 1.8 μg/kg, 2.1
μg/kg.
Method One -- Gas chromatography - Electron capture
detector method
2 Principle
The organochlorine pesticide component in the specimen is extracted by
organic solvent and purified by gel chromatography. Separate by capillary
column gas chromatography. Detect by electron capture detector. Determine
the chemical composition by retention time. Quantify by external standard
method.
3 Reagents
3.1 Acetone (CH3COCH3). analytically pure, re-distilled.
3.2 Petroleum ether. boiling range of 30°C~60°C, analytically pure, re-distilled.
3.3 Ethyl acetate (CH3COOC2H5). analytically pure, re-distilled.
3.4 Cyclohexane (C6H12). analytically pure, re-distilled.
3.9 Pesticide standard products. α-HCH, HCB, β-HCH, γ-HCH, PCNB, δ-HCH,
PCA, Heptachlor, PCPs, Aldrin, Oxychlordane, Heptachlorepoxide, trans-
chlordane, α-endosulfan, cis-chlordane, p,p’-DDE, Dieldrin, Endrin, β-
endosulfan, p,p’-DDD, o,p’-DDT, Endrinaldehyde, Endosulfansulfate, p,p’-DDT,
Endrinketone, Mirex, with a purity not less than 98%.
3.10 Preparation of standard solution. Accurately weigh or measure the
appropriate amount of the above pesticide standard products. Dissolve with a
small amount.
4 Apparatus
4.1 Gas chromatograph (GC). equipped with electronic capture detector (ECD).
4.3 Automatic gel chromatography system. with a fixed wavelength (254nm) UV
detector for optional use.
4.4 Rotary evaporator.
4.5 Tissue homogenizer.
4.6 Oscillator.
4.7 Nitrogen concentrator.
5 Analysis steps
5.1 Specimen preparation
For egg product, shell-remove and homogenize into egg wash. For meat
products, after removing the tendons, cut into small pieces and make into mince.
For dairy products, mix well for use.
5.2 Extraction and distribution
5.2.2 Meat products. weigh 20g of specimen (to the nearest of 0.01g). Add
15mL of water (the amount of water added shall be based on the water content
of specimen; make the total amount of water 20g). Add 40mL of acetone.
Oscillate 30min. The followings shall be processed according to the extraction,
distribution steps in 5.2.1 for egg product specimen.
5.2.3 Milk products. weigh 20g of specimen (to the nearest of 0.01g). Fresh milk
does not require water. Directly add acetone to extract. The followings shall be
processed according to the extraction, distribution steps in 5.2.1 for egg product
specimen.
5.3 Purification
Choose either manual or fully automated purification methods.
5.3.1 Manual gel column purification. Elute the specimen concentrate through
a gel column with ethyl acetate-cyclohexane (1+1) solution. Discard 0mL~35mL
of fractions. Collect 35mL~70mL of fractions. Concentrate it to approximately
1mL by rotary evaporation. Purify and collect 35mL~70mL of fractions by gel
column. Evaporate and concentrate. Blow off the solvent with nitrogen. Set the
volume to 1mL with hexane for GC analysis.
5.4 Determination
5.4.1 Gas chromatographic reference conditions
5.4.1.1 Chromatographic column. DM-5 quartz elastic capillary column, with a
length of 30m, an inner diameter of 0.32mm, a film thickness of 0.25μm; or
equivalent column.
5.4.1.2 Column temperature. programmed temperature
5.4.1.3 Inlet temperature. 280°C; splitless injection, injection volume of 1μL.
5.4.2 Spectrum analysis
Pipette 1 μL of mixed standard solution and specimen purification solution into
the gas chromatograph. Record chromatogram. Determine the chemical
composition with retention time. Quantify with specimen or comparison
between standard peak height or peak area.
6 Result calculation
The content of each pesticide in the specimen is calculated according to formula
(1).
7 Precision
The absolute difference between two independent determinations obtained
under repeatability conditions shall not exceed 20% of the arithmetic mean. See
Annex C for the method to determine the uncertainty.
8 Principle
After HCH, DDT in the specimen are extracted and purified, use gas
chromatography to determine. Compare with the standard and quantify.
Electron capture detector is extremely sensitive to compounds with strong
negative electrodes.
9 Reagents
9.1 Acetone (CH3COCH3). analytically pure, re-distilled.
9.2 N-hexane (n-C6H14). analytically pure, re-distilled.
9.3 Petroleum ether. boiling range of 30°C~60°C, analytically pure, re-distilled.
9.6 Anhydrous sodium sulfate (Na2SO4). analytically pure.
9.7 Sodium sulfate solution (20 g/L).
9.8 Pesticide standard product. HCH (α-HCH, γ-HCH, β-HCH, δ-HCH)
purity >99%; DDT (p,p’-DDE, o,p’-DDT, p,p’-DDD, p,p’-DDT) purity >99%.
9.10 Pesticide mixing standard working solution. Measure the above standard
stock solutions in the same volumetric flask separately. Dilute to scale with n-
hexane.
10 Apparatus
10.1 Gas chromatograph. with electron capture detector.
10.2 Rotary evaporator.
10.6 Centrifuge.
10.7 Plant sample crusher.
...... Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al.
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