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

Active Publication Date: 2013-10-02
JIANGNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among them, phthalates (diethyl phthalate (DEP), dibutyl phthalate (DBP), butyl phthalate (BBP), bis(2) phthalate -Ethylhexyl) ester (DEHP), di-n-octyl phthalate (DnOP)), because PAEs are not connected to plastic polymers through chemical bonds and are fat-soluble substances, it is easy to contaminate edible oil
Due to the complexity of the edible oil matrix and the low content of PAEs, the detection limits of PAEs reported in many literatures are relatively high and are greatly interfered by impurities, making detection difficult, especially for low-concentration PAEs.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

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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PUM

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Abstract

The invention discloses a pre-treatment method for phthalate ester plasticizers in edible oil. The pre-treatment method comprises: carrying out extraction on a certain mass of edible oil by using an organic solvent; carrying out a freezing degreasing treatment on the extraction liquid, and extracting the liquid; carrying out solid phase extraction small column purification on the obtained extraction liquid; and carrying out an elution blow drying volume metering treatment on the purified purification solution. Compare with the pre-treatment method in the national standard, the pre-treatment method of the present invention has the following characteristics that: the inspection process is short, operations are convenient, extraction efficiency is high, repeatability is good, solvent consumption is less, a measurement cost is low, sensitivity is high, contents of five common phthalate esters in edible oil can be concurrently detected, and good application prospects are provided.

Description

technical field [0001] The invention relates to the technical field of food quality and safety detection, and provides a method for pretreatment of several common phthalate plasticizers in edible oil. Background technique [0002] Plasticizer, or plasticizer, is an additive that can increase the softness and elasticity of materials, and is widely used in various fields of national industry. Plasticizers mainly refer to phthalates (PAEs). Studies have shown that although the acute toxicity of PAEs is not obvious, it can cause poisoning of multiple tissue systems such as liver, kidney, lung, heart, and reproduction, among which the damage to the male reproductive system is the most obvious. The European Food Safety Authority, the United States, Japan, and China have successively included phthalates in the blacklist of priority pollutants, which shows that the harm of PAEs to human health has attracted widespread attention in the world. [0003] Based on the above reasons, PA...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N1/34
Inventor 金青哲曹九超刘睿杰常明黄健花王兴国
Owner JIANGNAN UNIV
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