GB/T 5009.174-2003 Determination of metolachlor in peanuts and soybeans

This standard specifies the determination method of metolachlor residues in peanuts and soybeans. This standard is applicable to the determination of metolachlor residues in peanuts and soybeans. The detection limit of this method is 0.016ng; the linear range is 0.05ng～5.0ng. GB/T 5009.174-2003 Determination of metolachlor in peanuts and soybeans GB/T5009.174-2003 Standard download decompression password: www.bzxz.net

FC% 67.040
National Standard of the People's Republic of China
GB/T5009.174—2003
Determination of metolachlor residues in peanut and soybean
Published on August 1, 2003
Ministry of Health of the People's Republic of China
China National Green Promotion and Management Committee
Implemented on January 1, 2004
tB/T 5009.174—2003
Metolachlor (1-hydroxyethyl) oxalic acid (mctolachlor), also known as metolachlor. Trade name: dole(1), is a growth control agent for crops with high toxicity and low toxicity. This drug has been registered in peanut and soybean crops in China, and the maximum residue standard has been formulated, stipulating 0.5mg/kg for peanut and ug/k for soybean. This standard specifies the method for detecting the residual amount of isopropylamine in peanuts and soybeans. This standard specifies the method for the determination of isopropylamine in peanuts and soybeans. This standard is applicable to the determination of isopropylamine in peanuts and soybeans. The detection limit of this method is 0.06 ng~5.0 g. 2 Principle GBF 5009,174--2003 The isopropylamine in the sample is extracted with natural organic materials and then determined by gas chromatograph with electron capture detector. The qualitative results are obtained by the first retention time and the quantitative results are compared with the standard system. 3 Reagents 3.1 Hexane, redistribution rate. 3.3 Medium! 80--20 3.4 ECC e-chlorinated residues.
3.5 Filter with anhydrous 65°C for 4h. Store in a cool container. 3.6 Pretreatment: PT-100 plasticizer, silica gel column, 4mL n-hexane, 4\T hexane-acetaldehyde (2+1), 2ml hexane,
3.7 Standard preparation of renal acetylcholine (m1z20.schoT, purity>37%), 0.1c99, 0.1%, 1mL, 0.1% pure, ...1mL pure. 3.8 Differential weighing standard solution: take (3.7) 5.0mL positive film, set volume 300mL, concentrate 50g/L 4.1 Chromatographic equipment: with electron capture detector. 4.2 Ultrasonic cleaner, 4.3 Single action high speed centrifuge: 3twu r mi 4K [concentrator press installation 4.5 [50 mE, island etc. 4.6125 mt. Separation funnel.
5 Analysis steps
5.1 Sample preparation
Weigh 50ml of hot water (5.00 accurate to 0.21) and add 29ml of alcohol + water (807) into the ultrasonic cleaning device and add 20%in. Centrifuge for 10min (3000T, min) on the centrifuge. Add 125mL of the sample into two liters of water. Add 10mL of alcohol + water (80+20) into the residual water and place them in a 20mm mixing device at 135°C. 50C/. boil water in a reactor, add 1Cml hexane, move the gas to the boiler, vent, and separate the layers. The lower layer is transferred to another filter at a distance of 4 meters. Add 100% n-hexane, extract, and remove sodium sulfide from the water. After that, the volume is fixed to 21.
5.2 Purification of samples
5.1 The extract should be pre-treated in a small amount, 10m of acetaldehyde has been eluted, 5. The eluted liquid is washed with 2+1 acetaldehyde, and the volume is fixed to 1.mEEL, and the kettle is combined. 531
5009174--9303
5. 3 Gas Chromatography Reference Conditions
5.3.1 Chromatographic properties: SL20 cross-linked capillary tube at 25m×0.53mmx0.25m. 5.3.2 Vaporization density: 23%.
5.3.3 Detection sensitivity: 260%.
5.3.4 Incubator temperature: 175℃.
5.3.5 Gas, flow rate ratio: 1: 50mL/m5.4 Test
Standard value liquid is prepared into series of 3.05.0.10, C.5C.1.C.2.C0.4.C3.5.C3g/mL respectively. Take 1pL of each for gas chromatography analysis and record the area (peak height). (5.2) 1. Perform chemical analysis on the sample and record the peak height (6). Calculate the result by the following formula:
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Calculate the content of alachlor in food in grams per kilogram:
The concentration of alachlor in the tablet is calculated in micrograms per liter (/m3);
The volume of liquid for treatment is in liters (mL);
The volume of the sample after treatment is in milliliters (mL); The quality of the sample is in grams ().
Calculate the conclusion using two valid values:
The results of two independent determinations obtained under repeatability conditions shall not be less than the arithmetic mean. Gas chromatographic chain parts: chromatograph: SE-30 cross-section capillary 25×G.33um×0.25m, gasification chamber: 2, detector resistance 20, column box: 175. Standard gas (N) filling rate: flow ratio 55#1 tail blowing 5nml./min Figure 1 Isopropylamine chromatogram Figure 2 Peanut spiked sample chromatogram Figure 3 Peanut blank sample chromatogram
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