Gas Chromatographic Determination of Residual Aldicarb Sulfone in Peanut

Samples of residual content in peanuts were extracted with acetone / water, oxidized with peracetic acid, purified by Florisil column chromatography, and determined by gas chromatography (FPD). 1. Main instruments and equipment Gas chromatograph: with flame photometric detector (FPD) tissue masher magnetic stirrer rotary evaporator oscillator glass chromatography column: 30cm (length) × 1.3cm (inner diameter) 2. The main reagent acetone : Analytically pure dichloromethane: analytically pure, redistilled toluene: analytically pure, redistilled ether: analytically pure, redistilled oxidant: glacial acetic acid / 30% hydrogen peroxide (1: 1, V / V), add 1 before mixing % Concentrated sulfuric acid in hydrogen peroxide. Store away from light, and reconstitute Florisil after 7 days: 60 ~ 100 mesh aldicarb: purity 99.4% aldicarb sulfoxide: purity 99.9% aldicarb sulfone: 99.8% 3. Detection step 3.1 Extraction 3.1.1 Peanut kernels: Weigh 50g of mashed sample, add 200ml of acetone / water (3: 1, V / V), mash and extract for 3min. After suction filtration, the residue is crushed and extracted again with 150ml of extractant, suction filtered and combined Extract and concentrate to about 120ml, add 5ml of oxidant, after stirring for 20 minutes, add 50ml of 10% aqueous sodium bicarbonate solution, continue to stir for 20 minutes, extract with 3 x 100ml of dichloromethane, collect the extract and pass anhydrous sodium sulfate Dry and concentrate to about 20ml. 3.1.2 Peanut plants: Weigh 25g of crushed sample, add 200ml of acetone / water (3: 1, V / V) to soak overnight, then shake and extract for 30min. After suction filtration, the residue is shaken and extracted once again with 150ml of extractant. Concentrated and oxidized, extracted with dichloromethane, and concentrated (the specific operation steps are the same as peanut kernels). 3.2 Column chromatography Purification: Add 2cm thick anhydrous sodium sulfate to the upper and lower ends of the chromatography column, and add 8g of Flory silica in the middle. Pre-leached with 25 ml of toluene / dichloromethane (1: 1, V / V), then transferred the extraction concentrate to the column, and discarded the eluate. First rinse with 50ml of ether / acetone (98: 2, V / V), then rinse with 50ml of ether / acetone (1: 1, V / V), collect the eluate and concentrate to near dryness, then dilute to volume with acetone To be tested. 3.3 Gas Chromatography Detector Detector: Flame Photometric Detector (FPD) Column: 2m (Length) × 3mm (Inner Diameter) Stainless Steel Column Support: ChromosorbWAW, 80 ~ 100 mesh fixed liquid: 15% FFAP Detection Temperature: Column 226 , Detector 227 ℃, inlet 300 ℃ Carrier gas: nitrogen (99.99%), 100ml / min Combustion gas: hydrogen 35ml / min, air 76ml / min retention time: aldicarb sulfone 3min30s
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