This standard specifies the determination method of atrazine residues in food. This standard is applicable to the determination of atrazine residues in sugarcane and corn that have been treated with this herbicide. The detection limit of this method is 0.03mg/kg; the linear range is 0.40ng～2.00ng. GB/T 5009.132-2003 Determination of atrazine residues in food GB/T5009.132-2003 Standard download decompression password: www.bzxz.net

CN 67.040
National Standard of the People's Republic of China
GB/T 5009,132--2003
Replaces GR163381956
Determination of atrazine residues in food
Detcrmination of atrazine residues Jn foods2003-08-11issued
People's Republic of China and Guowei Huadu
National Standard Promotion and Management CommitteeWww.bzxZ.net
2004-01-01implemented
CB/T 5009.1322003
This standard replaces GB/T16336
1396 Determination of residues of attrition in foods by two-step method 3. Compared with B/T16336-1995, the main changes in this standard are as follows: The Chinese name of the standard is changed to "Determination of residues of attrition in foods" in accordance with GB/T 30M1t.4-2014. Part 4: Chemical analysis methods 3. The structure of the original standard is modified.
This standard is proposed and managed by the Ministry of Economic Affairs of the People's Republic of China. The drafting units of this standard are School of Public Health of West China University of Medical Sciences, Sichuan Provincial Health Station and Sichuan Occupational Disease Prevention and Control Institute.
The main drafters of this standard are: Shi Chuan, Xue Wencha, Sun Chengjun, Xie Junyi and Zhang Lijiao. The original standard was released in 1996, and this is the first time. 154
1 Scope
Determination of herbicide residues in food
This standard specifies the determination method for herbicide residues in food. This standard is applicable to the determination of herbicide residues in sugarcane that has been used as the source of the herbicide. The detection limit of this method is 0.03mg/kg and the range of detection is 0.40ng~2.00ng2. Principle
GB/T 5009.132—2003
Select the mixture of alcohol and water (1 + 1). After filtration, the filter is extracted with a mixed solvent of dichloromethane-petroleum aldehyde, partitioned with petroleum ether-ethyl acetate, purified with silica gel, eluted with ethyl acetate-petroleum ether, and the eluent is concentrated and then determined with n-hexane. The product was then determined by gas chromatography electron acquisition detector (ECT) for qualitative analysis using retention time and quantitative analysis using comparison with the peak height of a standard series. 3 Test carving
3. 1 Medium alcohol: re-distill.
3.2 Methyl chloride: re-distill in a tank
3.3 Shibo fresh: boil at .50, reheat
rain wine, mix with each other:
reheat.
3.6 Add 20mJ petroleum aldehyde to 100mL7. lipid, shake for 1min, let it stand and separate into layers, remove the lower layer of acetaldehyde and set aside.
3.7 n-Hexane: Re-distill chrysanthemum.
3.8 acetaldehyde ether.
3.9 No plastic pliers
3.10 Gun and molybdenum chloride solution.
3.11 Group magnesium adsorbent, 10U day ~ 20U day, calcine at 650 51 effect and store in the following container, take 100g of magnesium adsorbent and 10mL of water for deactivation before use, half balance overnight, mix and set aside. Store for more than 1 day, heat activate at -30 °C for 5h before use, then add water in the above proportion for deactivation before use.
3.12 Caution: Accurately weigh arazine standard substance and prepare it into a standard stock concentration of 1mk/minT with acetone. Store it in a low-pressure box (1T). When used, dilute it with hexachloride to obtain a standard concentration of 10 g/tL. 4 Instruments and equipment
4.1 Gas chromatograph with electron capture detector. 4.2 Electric stripper, high-speed weaving crusher 4.4 Constant-temperature water bath: 4.5 Small powder machine 4.6 Enterprise-efficient steam reduction device or combined steam generator 155 GB/T5009.132-2003 5 Analysis steps 5.1 Sample pretreatment 5.1.1 Extraction
5 meters, the sample is sieved through a powder sieve and passed through a 20-day sieve, about 50% of the sample is weighed, the bridge is adjusted to 0.001g and placed in a 250mL sieve bottle, add 120mL formaldehyde water (1-1>) and shake it on an electric or detector for 30 minutes to obtain a qualitative filter paper for extraction, the filtrate is transferred to a 250mL recording bottle, and the residue is added with methanol water (1+1) and shaken for 30 minutes to extract, and the combined energy is fixed with neutral alcohol water (1-1 to 25
Sugarcane: According to the sampling hardness, select the representative The H-fumigate sample was cut into fine pieces and weighed to an accuracy of 9.001 μg. The mixture was added to a high-speed crusher and 100 mL of alcohol water (1:1) was used to slurry 0.1 μg. The mixture was filtered through a Buchner filter covered with a 205-day nylon mesh and washed 3 to 4 times with 100 mL of water (1:1), and the residue was removed. The filtrate was then filtered quickly and transferred to a 252-well filter. The pellets were washed with a small amount of alcohol water (1:1) to wash the slide and the extraction bottle, and the filtrate and washing liquid were combined and the penetration rate was determined with water. 250ml..
Take 50.0ml. method solution (equivalent to 1ug sample) in a 250mL separating funnel, for the main test, add 2m. sodium chloride and 30mL distilled water. For the ganfei sample, add 5ml. sodium chloride and 50mL distilled water, mix with dichloromethane and ethanol (3.5 + 6.5), and test and report the absorption 3 times. Each time, mix 20nul of the reagent. Vibrate for 1min, combine the above dichloromethane and ethanol extracts, if there is an emulsion layer, add 21m 1. Shake the whole body of the steel pipette and let it stand for stratification: discard the sodium sulfate residue below. The extract was poured into a 100ml flask with 10% anhydrous sodium sulfate. The funnel and its contents were washed with a small amount of dichloromethane several times and the washings were added to the filtrate. Most of the solvent was evaporated under reduced pressure in a constant temperature water bath at 1°C. The solvent was dried with hydrogen (N2) or purified air. 5.1.2 Purification of ethanol: Wash the flask containing the extract several times with 5% petroleum aldehyde and transfer it to 125 10mL separating funnel, and then wash the surface of the flask with 20mL of ethanol and 20mL of sodium carbonate solution for 2-3 times, then transfer to the separating funnel, extract for 1min, and separate the layers. Transfer the lower layer of ethanol to another 10luL flask, and extract again for 20mL of ethanol saturated with petroleum aldehyde for 1-30 minutes. Collect the ether layer 1 time. Combine the ether layers, add 0.1% water to the top and evaporate most of it under reduced pressure, blow with hydrogen (N2) or purified air. Dissolve the retentate with 10mL of ethanol for column chromatography. Purification by column chromatography: Add 2 mL of anhydrous sodium hydroxide to the chromatography column (1~2mL), add 10g-15g of silica-magnesium adsorption spheres. Use 30mL of industrial petroleum dehumidification method to pack the column, and spread 1mL of anhydrous sodium hydroxide on the top of the column. The test sample is transferred onto the needle column. When the liquid level in the column drops to the surface of the test sample, elute it with 80 mT of ether-oil (1 + 2) several times on the ball filled with the test sample and then transfer it to the layered column. The elution rate is n, 5 ml./min1 mL./mir. Collect and remove the liquid, dry it at 60℃ + 17℃ water tank and heat it under high pressure to remove most of the shrinkage agent, purify the injected gas with chlorine (N2), accurately add 2mL of normal hexane to break up the solution and provide for analysis by 5.2 instrument. Gas chromatograph conditions: use X% mn copper chromatograph, filled with 3% (V-17 Chromo3orbWA WDMCS (3u-1UV day), production temperature: 33℃, detection chamber temperature is 230, gas flow rate is 30mL/min, or use 2m31 glass fiber hanging, filled with 3.5% 0V-17 GasChromQ (80days--130days), sample temperature 2CC, injection and detection chamber temperature is 2/0, gas trace is c0 nL/min. 5.3 Drawing of standard curve
Use the standard working solution of lorrazine to prepare 0.0, 0, 20, 0, 40, 0.50, 0.90, 1.00g/mL standard concentration. Under the above gas chromatograph test conditions, inject 2.0% standard solution into the gas chromatograph, measure 3 times at each point, take the density of the standard solution as the coordinate, take the half mean of the color height as the vertical axis, and observe the curve 5.4 Determination of the sample after 2.0% purification
Put the sample into the gas chromatograph, re-determine 3 times, and measure the sample The average value of the peak quotient. The retention time is used for qualitative analysis and the standard curve is used for quantitative analysis.
5.5 Analysis results
When the injection volume of the new standard melt is the same, the content of dezin in the sample is calculated according to the following formula. X-ExV
Wu:
X——the concentration of dezin in the sample, the unit is milligram per gram (mng/kg); GB/T5009.132——2003
——the concentration of dezin in the sample solution obtained by the standard curve is microgram per liter (\g/liter V--the final concentration of the test solution,The unit is milliliter (mI), and the unit of sample mass equivalent to the extraction with 10 microliters of alcohol water is gram (). The calculation result is rounded to two significant figures.
6 Precision
The absolute difference between the two standard determination results obtained under the repeatability condition shall not exceed 10 of the arithmetic mean. 157
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