Method for detecting bisphenol A substance by combining supermolecule solvent extraction and magnetic solid phase extraction

A supramolecular and extraction technology, applied in the field of analytical chemistry, can solve the problem that supramolecular solvent has only separation effect and no interference purification effect, and achieves the effects of high sensitivity, low detection limit and simple operation.

Active Publication Date: 2016-12-14
KUNMING UNIV OF SCI & TECH
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  • Application Information

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Problems solved by technology

Our research team has applied for the invention patent "A rapid detection method for bisphenol A (BPA) in polycarbonate (PC) material of food packaging material" (CN 103808815 A), which discloses the extraction of bisphenol A (BPA) in the sample liquid by supramolecular solvent BPA, but there is also the operation of centrifugal phase separation, and the supramolecular solvent only has the separation effect, and has no purification effect on the interfering substances in the sample matrix

Method used

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  • Method for detecting bisphenol A substance by combining supermolecule solvent extraction and magnetic solid phase extraction
  • Method for detecting bisphenol A substance by combining supermolecule solvent extraction and magnetic solid phase extraction

Examples

Experimental program
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Embodiment 1

[0023] Embodiment 1: Determination of bisphenol A substances in the infusion cap

[0024] (1) Magnetic material Fe 3 o 4 @SiO 2 Synthesis of @Mg–Al LDH

[0025] Fe 3 o 4 Synthesis of magnetic nanoparticles: Weigh 2.05 g of ferrous ammonium sulfate and 1.41 g of ferric chloride and dissolve them in 50 mL of deionized water, transfer the mixture to a 250 mL three-necked flask, mechanically stir and heat in a water bath under nitrogen protection, when the reaction When the solution was heated to 80°C, 5 mL of ammonia water (28%, w / v) was added, and the color of the solution changed from brownish yellow to black immediately. After continuous reaction for 30 min, it was naturally cooled to room temperature, and the product was separated by an external magnet. Wash with an appropriate amount of ethanol and distilled water for 3 to 5 times, and finally the prepared Fe 3 o 4 Vacuum-dried at 50°C for 12 hours and set aside;

[0026] SiO 2 wrapped Fe 3 o 4 Synthesis of M...

Embodiment 2

[0030] Embodiment 2: Determination of bisphenol A substances in feeding bottles

[0031] (1) Magnetic material Fe 3 o 4 @SiO 2 The synthetic method of @Mg-Al LDH is the same as Example 1;

[0032] (2) Sample preparation: Weigh 0.5g (accurate to 0.001g) of the sample to be tested, add 10mL of dichloromethane, ultrasonic (power 120W, frequency 40kHz) to dissolve or swell the sample, add 15mL of methanol, shake well , to precipitate the polymer compound, filter, evaporate the filtrate to dryness in a water bath at 40°C, dissolve the residue with methanol, transfer it to a 10mL measuring bottle, and dilute to the mark with deionized water to obtain a sample solution;

[0033] (3) Sample determination: Add 105 μL heptanol and 350 μL tetrahydrofuran to the sample solution in step (2), and vortex for 5 minutes; finally, add 5 mg of magnetic material Fe 3 o 4 @SiO 2 @Mg–Al LDH, vortex for 4min, equilibrate for 5min, collect the solid phase with a magnet and discard the water pha...

Embodiment 3

[0034] Embodiment 3: Determination of bisphenol A substances in waste water

[0035] (1) Magnetic material Fe 3 o 4 @SiO 2 The synthetic method of @Mg-Al LDH is the same as Example 1;

[0036] (2) Sample determination: Add 100 μL of nonanol and 500 μL of tetrahydrofuran to 10 mL of wastewater sample, vortex for 3 minutes; finally, add 10 mg of magnetic material Fe 3 o 4 @SiO 2 @Mg–Al, vortex for 5min, equilibrate for 10min, collect the solid phase with a magnet and discard the water phase, use 1mL methanol as the eluent to elute the solid phase twice, and pass the collected eluate through a 0.45 μm organic phase filter membrane After filtering, it was analyzed by HPLC, and the bisphenol A content was 0.31 μg / L, and the tetrabromobisphenol A content was 0.17 μg / L.

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Abstract

The invention discloses a method for detecting a bisphenol A substance by combining supermolecule solvent extraction and magnetic solid phase extraction. According to the method, a supermolecule solvent prepared from tetrahydrofuran and fatty alcohol and a magnetic aluminum and magnesium di-hydroxyl compound metal oxide are used for extracting the bisphenol A substance, and a high performance liquid chromatography is combined to measure the content of the bisphenol A substance. The dispersity of the magnetic aluminum and magnesium di-hydroxyl compound metal oxide magnetic material in the supermolecule solvent is good and adsorbs the bisphenol A substance well, and meanwhile, an applied magnetic field is used for quick separation. Compared with other traditional sample pretreatment methods, the pretreatment method has the advantages that the detection sensitivity is high, the cost is low, operation is easy, the separation speed is high, the magnetic nanometer material is recycled and environmentally friendly, and the pretreatment method has wide application prospects.

Description

technical field [0001] The invention belongs to the field of analytical chemistry, and in particular relates to a method for detecting bisphenol A substances by supramolecular solvent extraction combined with magnetic solid-phase extraction. Background technique [0002] The scientific name of bisphenol A is 2,2-bis(4-hydroxyphenyl)propane, also known as BPA, which is an exogenous endocrine disruptor and an additive for synthetic plastic packaging products. Bisphenol A can migrate into food or beverages through food packaging and plastic films, be absorbed by the human body, and gradually endanger human health. It can cause abnormalities in the endocrine system, immune system, and nervous system of humans and wild animals, and seriously interfere with human and The genetic function of reproduction in animals. Studies have reported that bisphenol A has the characteristics of estrogen and has certain damage to liver, kidney and breast; at the same time, bisphenol A is also re...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/06
CPCG01N30/06G01N2030/062
Inventor 杨亚玲杨德志焦扬
Owner KUNMING UNIV OF SCI & TECH
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