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Method for detecting phthalic acid esters in food

A phthalate and food technology, applied in the field of analytical chemistry, to achieve the effects of high sensitivity, low detection limit, and low dosage

Inactive Publication Date: 2014-04-30
云南健牛环境监测有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

These methods have more or less their own shortcomings in the extraction of PAEs

Method used

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  • Method for detecting phthalic acid esters in food

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specific Embodiment 1

[0030] The detection method of PAEs in milk includes the following steps: (1) Drawing of working curve: standard stock solutions of 100 μg / mL of DBEP, DMEP, BBP, DBP, DNOP and DCHP are diluted with methanol to 0.1 μg / mL and 0.5 μg / mL respectively. μg / mL, 1.0μg / mL, 5.0μg / mL, 10.0μg / mL, 20.0μg / mL, 40.0μg / mL, and then injected under the following chromatographic conditions: C18 column (150 mm×4.6 mm, i.d. 5 μm); injection volume: 20 μL; mobile phase: acetonitrile: water (0-10min: 55%-80 acetonitrile; 10min-12min: 80%-100% acetonitrile; 12min-20min: 100% acetonitrile; v / v) ; Flow rate 1.0 mL / min; Detection wavelength: 225 nm. The regression equation, correlation coefficient, relative standard deviation, recovery rate, etc. are shown in Table 1;

[0031] (2) Sample treatment: Take 5mL milk sample in a 10mL centrifuge tube, add 0.1g sodium acetate, centrifuge at 6000r / minl for 6min to precipitate protein, transfer the supernatant solution to another centrifuge tube, repeat the ...

specific Embodiment 2

[0034] A method for detecting the content of PAEs in biscuits, comprising the following steps:

[0035] (1) Drawing of the working curve: Draw part according to the above working curve; (2) Sample treatment: Weigh 2.00g biscuit sample, crush it and put it in a clean Erlenmeyer flask, add 3mL absolute ethanol, 2mL Acetone, after shaking for 10 minutes, filter the extract with a common funnel, transfer the filtrate to a volumetric flask and dilute to 25mL with distilled water to obtain a sample extract; The pH of the buffer was adjusted to 8, and 0.5 mL of nonanoic acid was added to the centrifuge tube, vortexed for 2 min, and then centrifuged at 3500 r / min for 8 min, the lower layer solution was removed with a pipette, and 0.3 mL of the upper organic phase was dissolved in methanol to 1.0 mL. Take 20 μL of the obtained methanol solution, and use the same chromatographic conditions as the determination of the working curve to obtain the corresponding peak area, which is subs...

specific Embodiment 3

[0036] The detection method of the content of PAEs in edible oil comprises the following steps:

[0037](1) Drawing of the working curve: Draw the part according to the above working curve; (2) Sample treatment: Weigh 10mL of edible oil sample into a clean separatory funnel, add 2mL of anhydrous methanol and 2mL of acetonitrile into the separatory funnel, shake 8min, stand for stratification, take out the supernatant, extract twice, combine the supernatant, and then transfer to a 25mL volumetric flask to constant volume to obtain the sample extract; (3) Take 5mL of the edible oil sample extract, and use pH =8.0 phosphate buffer solution to adjust the pH to 8, then add 0.5 mL of n-octanol, vortex for 3 min, then centrifuge at 4500 r / min for 6 min, remove the lower layer solution with a pipette, take 0.5 mL of the upper organic phase and dissolve it in methanol to 1.5 mL. Take 20 μL of the resulting methanol solution, and use the same chromatographic conditions as the deter...

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Abstract

The invention relates to a method for detecting phthalic acid esters (PAEs) in food. The method is characterized by comprising the steps that (1) an appropriate amount of organic solvent serves as an extraction agent of the PAEs in a food sample; (2) an extracting solution of the food sample is extracted by a liquid-liquid microextraction technique; and (3) measurement is performed by an HPLC (high performance liquid chromatography), and the content of the PAEs is judged by comparison with a working curve of the PAEs. Compared with the existing detection technique, the method has the advantages that the method is simple to operate, green, environment-friendly, low in cost, high in accuracy, good in reproducibility and short in detection time, is suitable for safety detection of the food, and has a wide application potential and a broad market prospect.

Description

technical field [0001] The invention belongs to the field of analytical chemistry, and more specifically relates to a detection method for phthalates in food. Background technique [0002] Plasticizers, also known as plasticizers, are phthalate esters (PAEs) compounds, which are widely used in daily life because of increasing the plasticity and flexibility of products. They are used in lubricants, insect repellents, cosmetics, detox It is used in the production of foaming agents, food packaging materials, medical appliances, and artificial leather. It has many types and is difficult to degrade. It is highly toxic to the human body, organisms, and plants. Immunosuppressive, becoming one of the most common pollutants in the world. In plastic products, since phthalates and polyolefin plastic molecules are compatible, there is no strict chemical bond between the two, so phthalates are easily removed from the plastic during use. migrating to the external environment, causi...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06
Inventor 杨亚玲廉源沛杨超
Owner 云南健牛环境监测有限公司
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