β- Hexachlorocyclohexane detection

2.3 Instruments and equipment 2.3.1 Gas chromatograph: equipped with an electron capture detector (ECD). 2.3.2 Electric oscillator. 2.3.3 Organize the crusher 2.3.4 Rotary evaporator. 2.3.5 Filter equipment: Buchner funnel (diameter 80 mm), suction bottle (20 mL). 2.3.6 Stoppered triangular flask: 100mL. 2.3.7 Separation funnel: 250 mL. 2.3.8 chromatography column. 2.4 Sample Preparation: Take a grain sample, crush it with a grain crusher, and pass it through a 20 mesh sieve to make a grain sample. Take a vegetable sample and wipe it clean. Remove the non edible parts and set aside. 2.5 Analysis steps 2.5.1 Extraction 2.5.1.1 Grain sample: Weigh 10g of grain sample, place it in a 100mL stoppered triangular flask, add 20 mI of petroleum ether, and shake it on an oscillator for 0.5 h. 2.5.1.2 Vegetable sample: Weigh 20g of vegetable sample. Place in a tissue mashing cup, add 30 ml. of acetone and 30 mL of petroleum ether, and mash for 2 minutes on a masher. The mashing solution is filtered and transferred to a 250mL separation funnel. Add 100mL2% sodium sulfate aqueous solution, shake well, let stand for layering, transfer the lower solution to another 250 mI. separation funnel, extract with 2X20 ml. of petroleum ether, merge the three extracted petroleum ether layers, pass through an anhydrous sodium sulfate layer, and concentrate on a rotary evaporator to 10ml. 2.5.2 Purification 2.5.2 1. Preparation of chromatography column: First, 1 cm of anhydrous sodium sulfate is added to the glass chromatography column, followed by 5 g of 5% water to deactivate Florisilica. Finally, 1 cm of anhydrous sodium sulfate is added, lightly compacted, and the purification column is rinsed with 20mI of petroleum ether. Discard the eluent, leaving a small amount of liquid on the column surface. 2.5.2.2 Purification and concentration: Accurately extract 2mL of the sample extraction solution, add it to a washed purification column, elute with 100mL of petroleum ether ethyl acetate (95+5), collect the eluent in a distillation flask, concentrate it on a rotary evaporator to nearly dry, dissolve the residue multiple times with a small amount of petroleum ether in a graduated centrifuge tube, and finally dilute to 1.0 mL for gas chromatography analysis

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