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GB/T 5009.19-2008 PDF English

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GB/T 5009.19-2008: Determination of organochlorine pesticide multiresidues in foods
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GB/T 5009.19: Evolution and historical versions

Standard IDContents [version]USDSTEP2[PDF] deliveryName of Chinese StandardStatus
GB/T 5009.19-2008English85 Add to Cart 0-9 seconds. Auto-delivery Determination of organochlorine pesticide multiresidues in foods Valid
GB/T 5009.19-2003English239 Add to Cart 2 days Determination of HCH and DDT residues in foods Obsolete
GB/T 5009.19-1996English199 Add to Cart 2 days Method for determination of BHC and DDT residues in foods Obsolete
GB 5009.19-1985English199 Add to Cart 2 days Method for determination of BHC and DDT residues in foods Obsolete

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GB/T 5009.19-2008: Determination of organochlorine pesticide multiresidues in foods

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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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