Pre-treatment method for phthalate ester plasticizers in edible oil
A phthalic acid and ester plasticizer technology, applied in the field of food quality and safety testing, can solve the problems of undetectable PAEs, high detection limit of PAEs, and great interference by impurities, and achieves short testing process and good application. Prospect, good repeatability
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Embodiment 1
[0023] 1. Extraction
[0024] Accurately weigh 1g of first-grade soybean oil (accurate to 0.001g) into a 10mL glass centrifuge tube, add 5mL of acetonitrile, vortex and mix for 2min, 4000rpm, centrifuge for 3min, take out the acetonitrile layer by layer, repeat the above operation 3 times, and combine 3 times Extract.
[0025] In this embodiment, a liquid-liquid extraction method is used to extract PAEs in edible oil, and the extraction solvent is acetonitrile. Mix a certain amount of edible oil with acetonitrile, vortex and centrifuge, the acetonitrile layer is in the upper layer, and the fat is in the lower layer.
[0026] Too much or too little extraction times will have a certain impact on the determination results. If the number of extractions is too small, the recovery rate of the target substance will be too low to meet the analysis requirements; if the number of extractions is too high and more impurities will be extracted, it will interfere with the subsequent analy...
Embodiment 2
[0037] Embodiment 2 is tested with peanut oil as sample
[0038] Accurately weigh 1g of peanut oil (accurate to 0.001g) into a 10mL glass centrifuge tube, and extract with 10mL (divided into 2 extractions), 15mL (divided into 3 extractions), and 20mL (divided into 4 extractions) of n-hexane. After the extract was placed at -20°C for 3 hours, it was quickly transferred to another clean test tube. At 45°C, nitrogen flow was blown until nearly dry, then 2mL of n-hexane was added, mixed evenly to be purified.
[0039] Purify the liquid to be purified through a solid-phase extraction cartridge filled with ethylenediamine-N-propylsilane, collect the effluent, first elute with 5mL of n-hexane, and then wash with 5mL of 8% acetone-n-hexane (V:V) The collected eluate was blown dry with nitrogen at 40°C, and the volume was adjusted to 2 mL with n-hexane for GC-MS analysis.
Embodiment 3
[0041] Embodiment 3 is tested with olive oil as sample
[0042] Accurately weigh 1g of olive oil (accurate to 0.001g) into a 10mL glass centrifuge tube, and extract with 10mL (divided into 2 extractions), 15mL (divided into 3 extractions), and 20mL (divided into 4 extractions) of acetonitrile. After the extract was placed at -20°C for 3 hours, it was quickly transferred to another clean test tube. At 45°C, nitrogen flow was blown until nearly dry, then 2mL of n-hexane was added, mixed evenly to be purified.
[0043] Purify the liquid to be purified through a solid-phase extraction cartridge filled with ethylenediamine-N-propylsilane, collect the effluent, first elute with 5mL of n-hexane, and then wash with 5mL of 8% acetone-n-hexane (V:V) The collected eluate was blown dry at 42°C with nitrogen, and the volume was adjusted to 2 mL with n-hexane for GC-MS analysis.
[0044] The examples prove that after the above pretreatment method, GC-MS can accurately analyze the situatio...
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