CN103293237A

CN103293237A - Detection method for phthalate compound in plastics

Info

Publication number: CN103293237A
Application number: CN2013101138160A
Authority: CN
Inventors: 张爱雷
Original assignee: Individual
Current assignee: Individual
Priority date: 2013-04-03
Filing date: 2013-04-03
Publication date: 2013-09-11

Abstract

The invention discloses a detection method for a phthalate compound in plastics. The detection method comprises the following steps: processing a plastic sample to obtain fragments with a length of 0.2 to 0.3 cm, adding an organic solvent, standing for 30 to 40 h at a temperature of 25 to 30 DEG C, carrying out ultrasonic extraction for 30 to 45 min, subjecting an extract to filtration with a 0.4-mu m organic phase filter membrane and allowing the volume of the extract to be constant; and carrying out sampling on the sample with a constant volume, carrying out analyzing by using high performance liquid chromatography and carrying out determination to obtain the content of a phthalate plasticizer in the sample. The detection method has the advantages of a fast speed, high sensitivity and a detection limit reaching a ppb grade and is capable of effectively and rapidly detecting whether the content of a plasticizer in a variety of plastic products contacting with food is qualified and fulfills safety standards.

Description

The detection method of phthalate compound in a kind of plastics

Technical field

The present invention relates to the detection method of phthalate compound in a kind of plastics, be specifically related to a kind of convenient, fast, accurate detection method at the plasticizer phthalic acid ester compounds that adds in the food pack.

Background technology

Food-safety problem more and more is subjected to the general common people's care now, food security is the field of a wide range, it not only refers to food itself, also relate to all many-side relevant with food, pollute aspects such as control, food placement and storage, packaging for foodstuff material therefor as the used starting material of food, food processing technology process.

Phthalate compound is plastifier commonly used in the plastics, for plastics performance is increased, phthalic acid is the ester class and is widely used, but it is a class environmental hormone, directly jeopardize health, China is listed repefral, dibutyl phthalate and dioctyl phthalate in the environment priority pollutant blacklist in.

Summary of the invention

Technical matters to be solved by this invention is: the detection method that phthalate compound in a kind of highly sensitive plastics is provided.

For solving the problems of the technologies described above, technical scheme of the present invention is: the detection method of phthalate compound in a kind of plastics the steps include:

Plastic sample is treated to the fragment of 0.2～0.3cm, adds organic solvent, place 30～40h for 25～30 ℃, ultrasonic extraction 30～45min, extract is with 0.4 μ m organic phase membrane filtration, constant volume; Take a sample the sample behind constant volume, utilize high performance liquid chromatography analysis, measure the content that obtains phthalic ester plasticizer in the sample.

Described organic solvent is selected in one or more in the following substances: methyl alcohol, ethanol, acetonitrile, methylene chloride.

Described organic solvent is that volume ratio is the ethanol of 1:1～1:1.2 and the mixed liquor of methylene chloride.

Adopt gradient in the efficient liquid phase chromatographic analysis process, eluant, eluent methyl alcohol-water; Gradient program: 0～4min methyl alcohol 75%, pure water 25%; 4～9min methyl alcohol is gradually varied to 100% by 75%; Pure water is gradually varied to 0 by 25%; 9～13min methyl alcohol 100%.

Measure wavelength 226nm～227nm in the efficient liquid phase chromatographic analysis process.

Beneficial effect of the present invention: this detection method speed is fast, highly sensitive, and detection limit reaches the ppb level; Can realize whether plasticizer loading is qualified in the various plastic products of effective fast detecting and Food Contact, reaches safety standard.

Description of drawings

Fig. 1 is the standard colors spectrogram of phthalic acid ester type compound.

Embodiment

As can be seen, the retention time of each material is as follows in the standard colors spectrogram of phthalic acid ester type compound from accompanying drawing 1:

1 repefral (RT=1.9lmin);

2 diethyl phthalates (RT=2.55rain);

3 dibutyl phthalates (RT=7.55min);

4 phthalic acids two (2-ethyl) own esters (RT=11.92min);

5 dioctyl phthalates (RT=12.20min).

Embodiment 1

Mineral water bottle is cut into the fragment that the length of side is 0.2～0.3cm, take by weighing sample 0.5g (being accurate to mg), with the mixed liquor 80mL that adds ethanol and the methylene chloride of 1:1 approximately, place 40h for 25～30 ℃, ultrasonic extraction 45min, extract with 0.4 μ m organic phase membrane filtration, be settled to 100mL; Take a sample the sample behind constant volume, utilize high performance liquid chromatography analysis, measure the content that obtains phthalic ester plasticizer in the sample.

Measure wavelength 226nm in the efficient liquid phase chromatographic analysis process.

After testing, wherein retention time is that absorption peak appears in the 7.56min place, compares with standard model, is defined as: dibutyl phthalate.

Embodiment 2

Plastic packaging bag is cut into the fragment that the length of side is 0.2～0.3cm, take by weighing sample 0.4g (being accurate to mg), with the mixed liquor 80mL that adds ethanol and the methylene chloride of 1:3 approximately, place 36h for 25～30 ℃, ultrasonic extraction 40min, extract with 0.4 μ m organic phase membrane filtration, be settled to 100mL; Take a sample the sample behind constant volume, utilize high performance liquid chromatography analysis, measure the content that obtains phthalic ester plasticizer in the sample.

Measure wavelength 227nm in the efficient liquid phase chromatographic analysis process.

After testing, wherein retention time is that absorption peak appears in the 1.92min place, compares with standard model, is defined as: repefral; Retention time is that absorption peak appears in the 12.20min place, compares with standard model, is defined as: dioctyl phthalate.

Claims

1. the detection method of a phthalic ester plasticizer the steps include:

Plastic sample is treated to the fragment of 0.2～0.3cm, adds organic solvent, place 30～40h for 25～30 ℃, ultrasonic extraction 30～45min, extract is with 0.4 μ m organic phase membrane filtration, constant volume;

Take a sample the sample behind constant volume, utilize high performance liquid chromatography analysis, measure the content that obtains phthalic ester plasticizer in the sample.

2. the detection method of a kind of phthalic ester plasticizer according to claim 1, it is characterized in that: described organic solvent is selected in one or more in the following substances: methyl alcohol, ethanol, acetonitrile, methylene chloride.

3. the detection method of a kind of phthalic ester plasticizer according to claim 2, it is characterized in that: described organic solvent is that volume ratio is the ethanol of 1:1～1:1.2 and the mixed liquor of methylene chloride.

4. the detection method of a kind of phthalic ester plasticizer according to claim 1 is characterized in that: adopt gradient in the efficient liquid phase chromatographic analysis process, eluant, eluent methyl alcohol-water; Gradient program: 0～4min methyl alcohol 75%, pure water 25%; 4～9min methyl alcohol is gradually varied to 100% by 75%; Pure water is gradually varied to 0 by 25%; 9～13min methyl alcohol 100%.

5. the detection method of a kind of phthalic ester plasticizer according to claim 1 is characterized in that: measure wavelength 226nm～227nm in the efficient liquid phase chromatographic analysis process.