2,4-D detection

This standard specifies the method for determining 2.4-drop residues in grains and vegetables. This standard is applicable to the determination of 2.4-drop residues in grains and vegetables. The detection limit of this method is 0.008 mg/kg for vegetable samples; Raw grain sample, 0.013 mg/kg; Linear range; From 0.01 ng to 10 ng. 2 principle samples, 2.4+drops were extracted with organic solvents, and 2.4- drops were derivatized with boron trifluoride butanol solution to generate 2,4- drops of butyl ester. Liquid liquid extraction and column chromatography were used to remove interfering substances, and gas chromatography electron capture detector was used for determination. Qualitative analysis based on the retention time of chromatographic peaks. Quantitative analysis of peak area using external standard method. 3 Reagents 3.1 Methanol. 3.2 Ether. 3.3 Petroleum ether; Boiling range: 30C~60C, heavy Yanrun. 3.4 Isooctane. 3.5 Acetone. 3.6 pH 2 acidic aqueous solution: prepared with dilute sulfuric acid. 3.7 50 g/L sodium chloride solution 3.8 Anhydrous sodium sulfate. Burn at 650 ° C for 4 hours and store in a dryer. 3.9 Eluent: petroleum ether+acetone (95+5). 3.10 Hygienic agent: 14% boron trifluoride butanol solution. 3.11 2.4 drops of standard solution; Prepare 2.4 drops (2.4-D, purity 99.9%) with methanol to form 1 00 mg/mL solution. 4 Instrument and equipment. 4.1 Gas chromatograph: equipped with electron capture detector. 4.2 Organize the crusher. 4.3 G3 sand core funnel. 4.4 Purification column: PT silicon magnesium adsorbent color harmonic pre-treatment small column, filled with 0.4g 60 mesh to 80 mesh silicon magnesium adsorbent. Pre rinse with 5mL acetone and petroleum ether before use. 4.5 20mL glass bottle for headspace analysis, equipped with aluminum cap and sealing gasket

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