Method for rapidly detecting bisphenol A and bisphenol AF in food

Abstract

The invention relates to a method for detecting bisphenol A and bisphenol AF in food, belonging to technical field of analytical chemistry determination method. With ionic liquid (1-butyl-3-methylimidazole hexafluorophosphate) as an extractant and TritonX-100 or acetone as an dispersant, ultrasonic oscillation is carried out to form emulsion; after centrifugal separation, extraction drops at the lower layer are directly subjected to HPLC (high performance liquid chromatography) quantitative analysis. The method disclosed by the invention has the advantages of simpleness in detection steps, easiness in operation, low detection limit and high enrichment multiple, greatly reduced detection cost. The method disclosed by the invention is a rapid, efficient and environmentally friendly pre-treatment technology and has a wider application prospect in the field of food analysis.

Description

technical field

[0001] The invention relates to a rapid detection method for bisphenol A and bisphenol AF in food, which belongs to the technical field of analytical chemistry, and more specifically uses liquid-liquid dispersion micro-extraction-high performance liquid chromatography to detect bisphenol A and bisphenol AF in plastic packaged food. Bisphenol AF was determined. Background technique

[0002] Bisphenol A, (Bisphenol A, referred to as BPA) is a chemical raw material that can greatly enhance the transparency and durability of polymer materials such as epoxy resin, polycarbonate and unsaturated polyester resin. It is widely used in the production of packaging materials, rubber anti-aging materials, pesticides and baby products, and it flows into the environment in large quantities during production and use. Bisphenol A has the effect of estrogen, which can interfere with the production, release, transportation and metabolism of normal hormones in the body, can cau...

Examples

Embodiment 1

[0028] Example 1 : the rapid detection method of bisphenol A and bisphenol AF in edible acetic acid, concrete steps are as follows:

[0029] (1) Take 10.0 g of edible acid vinegar and centrifuge at 2500 rpm for 5 min, take the supernatant to adjust the pH to 6.0, at this time a small amount of suspended matter appears in the sample, centrifuge at 1500 rpm for 3 min, and inject the supernatant into the extraction device in, spare;

[0030] (2) Mix 20 μL 1-butyl-3-methylimidazolium hexafluorophosphate and 500 μL Triton X-100, quickly inject into the pretreated sample solution, shake well, put in a 75°C water bath for 5 min, and ultrasonicate at 75°C for 3 min (ultrasonic frequency is 60 KHz), cooled to room temperature, centrifuged at 4000 rpm for 5 min, and the lower layer of the extract was removed. Carry out secondary extraction according to the above extraction method, combine the lower layer droplets obtained from the two extractions, and inject them into HPLC for separat...

Embodiment 2

[0033] Example 2: the rapid detection method of bisphenol A and bisphenol AF in edible oil, concrete steps are as follows:

[0034] (1) Take 10.0 g of edible oil and centrifuge at 3000 rpm for 7 minutes. After centrifugation, take the supernatant to adjust the pH to 7.0, then centrifuge at 1600 rpm for 4 minutes, and set aside;

[0035] (2) Mix 15 μL extractant (1-butyl-3-methylimidazolium hexafluorophosphate) and 500 μL dispersion liquid acetone, quickly inject it into the edible oil sample liquid, shake well, put in 75 ℃ water bath for 5 min, and 75 ℃ Sonicate for 5 min (ultrasonic frequency is 70 KHz), cool down to room temperature, centrifuge at 4000 rpm for 5 min, and remove the extract droplet from the lower layer. Carry out secondary extraction according to the above extraction method, combine the lower layer droplets obtained from the two extractions, and inject them into HPLC for separation and analysis. The mobile phase is acetonitrile and water (40:60, V / V), and t...

Embodiment 3

[0038] Example 3 : The rapid detection method of bisphenol A and bisphenol AF in yellow rice wine, concrete operation is as follows:

[0039] (1) Centrifuge 15.0 g rice wine [ethanol content less than 6% (V / V)] for 8 min (3000 rpm), remove the suspended matter in the sample, take the supernatant to adjust the pH to 6.0, centrifuge for 3 min (2000 rpm), To remove the suspended solids produced by adding acid, take the supernatant and inject it into the extraction device for later use;

[0040] (2) Mix 10 μL extractant (1-butyl-3-methylimidazolium hexafluorophosphate) and 500 μL dispersion solution (acetone) and quickly inject it into the pretreated sample, shake well, bathe in 70°C water for 5 min, 70 Sonicate at ℃ for 8 min (ultrasonic frequency is 70 KHz), cool to room temperature, centrifuge at 1500 rpm for 10 min, take out the extract droplet in the lower layer, perform secondary extraction according to the above extraction method, combine the two extract drops, inject HPL...

technical field

[0001] The invention relates to a rapid detection method for bisphenol A and bisphenol AF in food, which belongs to the technical field of analytical chemistry, and more specifically uses liquid-liquid dispersion micro-extraction-high performance liquid chromatography to detect bisphenol A and bisphenol AF in plastic packaged food. Bisphenol AF was determined. Background technique

[0002] Bisphenol A, (Bisphenol A, referred to as BPA) is a chemical raw material that can greatly enhance the transparency and durability of polymer materials such as epoxy resin, polycarbonate and unsaturated polyester resin. It is widely used in the production of packaging materials, rubber anti-aging materials, pesticides and baby products, and it flows into the environment in large quantities during production and use. Bisphenol A has the effect of estrogen, which can interfere with the production, release, transportation and metabolism of normal hormones in the body, can cau...

Examples

Embodiment 1

[0028] Example 1 : the rapid detection method of bisphenol A and bisphenol AF in edible acetic acid, concrete steps are as follows:

[0029] (1) Take 10.0 g of edible acid vinegar and centrifuge at 2500 rpm for 5 min, take the supernatant to adjust the pH to 6.0, at this time a small amount of suspended matter appears in the sample, centrifuge at 1500 rpm for 3 min, and inject the supernatant into the extraction device in, spare;

[0030] (2) Mix 20 μL 1-butyl-3-methylimidazolium hexafluorophosphate and 500 μL Triton X-100, quickly inject into the pretreated sample solution, shake well, put in a 75°C water bath for 5 min, and ultrasonicate at 75°C for 3 min (ultrasonic frequency is 60 KHz), cooled to room temperature, centrifuged at 4000 rpm for 5 min, and the lower layer of the extract was removed. Carry out secondary extraction according to the above extraction method, combine the lower layer droplets obtained from the two extractions, and inject them into HPLC for separat...

Embodiment 2

[0033] Example 2: the rapid detection method of bisphenol A and bisphenol AF in edible oil, concrete steps are as follows:

[0034] (1) Take 10.0 g of edible oil and centrifuge at 3000 rpm for 7 minutes. After centrifugation, take the supernatant to adjust the pH to 7.0, then centrifuge at 1600 rpm for 4 minutes, and set aside;

[0035] (2) Mix 15 μL extractant (1-butyl-3-methylimidazolium hexafluorophosphate) and 500 μL dispersion liquid acetone, quickly inject it into the edible oil sample liquid, shake well, put in 75 ℃ water bath for 5 min, and 75 ℃ Sonicate for 5 min (ultrasonic frequency is 70 KHz), cool down to room temperature, centrifuge at 4000 rpm for 5 min, and remove the extract droplet from the lower layer. Carry out secondary extraction according to the above extraction method, combine the lower layer droplets obtained from the two extractions, and inject them into HPLC for separation and analysis. The mobile phase is acetonitrile and water (40:60, V / V), and t...

Embodiment 3

[0038] Example 3 : The rapid detection method of bisphenol A and bisphenol AF in yellow rice wine, concrete operation is as follows:

[0039] (1) Centrifuge 15.0 g rice wine [ethanol content less than 6% (V / V)] for 8 min (3000 rpm), remove the suspended matter in the sample, take the supernatant to adjust the pH to 6.0, centrifuge for 3 min (2000 rpm), To remove the suspended solids produced by adding acid, take the supernatant and inject it into the extraction device for later use;

[0040] (2) Mix 10 μL extractant (1-butyl-3-methylimidazolium hexafluorophosphate) and 500 μL dispersion solution (acetone) and quickly inject it into the pretreated sample, shake well, bathe in 70°C water for 5 min, 70 Sonicate at ℃ for 8 min (ultrasonic frequency is 70 KHz), cool to room temperature, centrifuge at 1500 rpm for 10 min, take out the extract droplet in the lower layer, perform secondary extraction according to the above extraction method, combine the two extract drops, inject HPL...

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